Manual ASpect CS EN 2011-09

ASpect CS
Software for HR-CS AAS
User's manual
Service: Analytik Jena AG
Customer Services
Konrad-Zuse-Str. 1
07745 Jena
Germany
Phone: Hotline: + 49 (0) 3641 / 77-7407

Fax: + 49 (0) 3641 / 77-7449
Email: [email protected]
General information about Analytik Jena AG

on the internet: http://www.analytik-jena.de
Copyrights and Trademarks
contrAA is a registered trademark of Analytik Jena AG in Germany.

Microsoft, Windows XP/VISTA/7, MS Excel are registered trademarks of Microsoft Corp
The identification with ® or TM is omitted in this manual.
Publication No.: 160:004.23
Edition – Septembre 2011

Technical documentation made by:
Analytik Jena AG
This documentation describes the state of this product at the time of publishing. It need not
necessarily agree with future versions of the product.
Subject to change!
© Copyright 2011 Analytik Jena AG

Contents
Contents
1 ASpect CS Software .................................. 5 4.1.7.1 Entry of concentrations for manually
prepared standards ..................................... 45
1.1 User manual conventions .............................. 5
4.1.7.2 Entry of concentrations for standards
1.2 Starting and exiting ASpect CS ..................... 6
prepared with autosampler .......................... 46
1.3 General information on operation .................. 7
4.1.8 Statistics tab – Defining statistical analysis . 48
1.3.1 The workspace .............................................. 7
4.1.9 QCS tab – Quality Control Samples ............ 50
1.3.2 The Help function .......................................... 7
4.1.10 QCC tab – Quality control during the
1.3.3 The menu bar ................................................ 7 analytical process ....................................... 54
1.3.4 Frequently used control elements ................. 8 4.1.11 Output tab – screen view, printout and
saving options ............................................. 56
1.3.5 Function keys ................................................ 9
4.2 Saving and opening methods ...................... 57
1.3.6 Choosing a printer ....................................... 10
1.4 General measurement procedure ................ 10 5 Sequences ................................................ 58
5.1 Creating a sequence ................................... 58
2 Preparatory settings - Choosing the
analytical task .......................................... 11 5.1.1 Specific dialog functions in Sequence
window ........................................................ 58
3 Customizing ASpect CS .......................... 14
5.1.2 Specifying sequences of samples and
3.1 General settings .......................................... 14 actions......................................................... 60
3.1.1 View options ................................................ 14 5.2 Saving and opening sequences .................. 62
3.1.2 Save paths .................................................. 15
6 Sample information files ......................... 63
3.1.3 Export options ............................................. 16
6.1 Create information data for samples and
3.1.4 Options for continuous ASCII export ........... 16 QC samples ................................................ 63
3.1.5 Options for analysis sequence .................... 17 6.1.1 Elements in Sample ID window ................... 63
3.2 Specifying units, QC and stock standards ... 19 6.1.2 Editing sample ID ........................................ 65
3.2.1 Specifying units of measurements ............... 19 6.1.3 Edit QC sample IDs..................................... 65
3.2.2 Specifying stock standards and 6.2 Saving, opening and importing sample
QC samples ................................................. 20 information .................................................. 65
4 Methods .................................................... 21 7 Starting an analysis / Calculating
4.1 Creating method parameters ....................... 21 results ....................................................... 67
4.1.1 Lines tab – Choosing element lines ............. 22 7.1 Starting the analysis process ...................... 67
4.1.2 Flame tab – Flame parameters ................... 24 7.2 Interrupting, stopping, continuing the
analysis process ......................................... 69
4.1.3 Furnace tab – Parameters for graphite
tube furnace ................................................ 26 7.3 Repeating an individual measurement ........ 70
4.1.4 Hydride tab – Specifying the hydride 7.4 Specifics for solid sample analysis with
system ......................................................... 27 SSA 600 ...................................................... 70
4.1.5 Set auto sampler - Sample transport tab ..... 32 7.4.1 Preparing samples for automated analysis . 73
4.1.5.1 Auto sampler for flame and Hydride/ 7.4.2 Re-analyze samples for solid analysis ........ 74
HydrEA technique........................................ 32 7.5 Rinsing the system ...................................... 75
4.1.5.2 Autosampler for graphite tube technique 7.6 Reprocessing analysis results ..................... 75
(solution analytics) ....................................... 35
7.7 Evaluating measurements parallel to
4.1.5.3 Autosampler for graphite tube technique running analyses ......................................... 76
(solid analysis) ............................................. 37
7.8 Displaying results and analysis progress .... 77
4.1.6 Evaluation tab – Spectral range and
7.8.1 Sequence/Results tab ................................. 77
background corrections ............................... 40
7.8.2 Sequence tab .............................................. 77
4.1.7 Calib. tab – Calibration parameters ............. 42
ASpect CS Issue 09/2011 1

Contents
7.8.3 Results tab .................................................. 78 8.4.1 Control of hydride system functions ........... 125
7.8.4 Overview tab ............................................... 80 8.4.2 Testing the hydride system for errors ........ 127
7.8.5 Solid tab ...................................................... 81 8.5 Autosampler .............................................. 129
7.9 Opening, closing and printing 8.5.1 Autosampler AS 51/52s ............................. 129
analysis results............................................ 81
8.5.1.1 Specify autosampler AS 51/52s ................. 129
7.10 Sample details and spectra ......................... 82
8.5.1.2 Technical parameters of the autosampler
7.10.1 Displaying details of single values AS 51/52s .................................................. 131
of samples ................................................... 83
8.5.1.3 Setting insertion depth and dosing speed
7.10.2 Displaying spectra ....................................... 85 for AS 51/52s ............................................. 132
7.10.2.1 Showing single spectra and varying 8.5.1.4 Functional test of the autosampler
background correction ................................. 85 AS 51/52s .................................................. 133
7.10.2.2 3D presentation of the spectra of single 8.5.1.5 Adjust autosampler AS 51/52s .................. 135
values .......................................................... 89
8.5.1.6 Position overview in the autosampler
7.10.2.3 Line identification ........................................ 90 AS 51/52s .................................................. 136
7.11 Calibration ................................................... 91 8.5.1.7 Supply of reagents for sample ................... 136
7.11.1 Graphic presentation of calibration curve .... 92 8.5.2 Micro pipetter unit MPE 60 ........................ 137
7.11.2 Displaying calibration results ....................... 92 8.5.2.1 Specify autosampler MPE 60 .................... 138
7.11.3 Modifying the calibration curve .................... 94 8.5.2.2 Technical parameters of the autosampler
MPE 60 ...................................................... 139
7.12 Quality control ............................................. 95
8.5.2.3 Set insertion depth and dosing speed of
7.12.1 Parameters of QC charts ............................ 95
the MPE 60 ................................................ 141
7.12.2 Displaying QC charts .................................. 97
8.5.2.4 Automatic depth correction for MPE 60 ..... 141
8 Controlling and monitoring 8.5.2.5 Aligning MPE 60 to graphite tube furnace . 143
spectrometer and accessories ............... 99
8.5.2.6 Function test of autosampler ..................... 144
8.1 Spectrometer............................................... 99
8.5.2.7 Adjusting the MPE 60 ................................ 146
8.1.1 Device function test on contrAA .................. 99
8.5.2.8 Position overview of the MPE 60 ............... 147
8.1.2 Measuring a spectral peak at a selected
wavelength ................................................ 101 8.5.3 Solid autosampler SSA 600 ....................... 148
8.1.3 Starting continuous measurements ........... 101 8.5.3.1 Function test of solid sampler .................... 149
8.1.4 Correcting peak offsets ............................. 103 8.5.3.2 Alignment of solid sampler ......................... 150
8.2 Flame ........................................................ 105 9 Data management and report

printout ....................................................152
8.2.1 Testing flame functions ............................. 105
9.1 Creating and printing result reports............ 152
8.2.2 Optimizing the flame ................................. 108
9.1.1 Selecting output target and report options . 153
8.2.2.1 Manual flame optimization ........................ 108
9.2 Further print functions ................................ 156
8.2.2.2 Automatic flame optimization .................... 110
9.3 Data management for methods,
8.2.3 Extinguishing the flame ............................. 111
sequences and result data ......................... 157
8.3 Furnace ..................................................... 112
9.3.1 The database window ................................ 157
8.3.1 Editing a furnace program ......................... 112
9.3.2 Managing methods and sequences ........... 158
8.3.2 Matrix modifiers, selections for
9.3.3 Managing results files ................................ 160
enrichment and pretreatment .................... 115
9.3.4 Copying lines/wavelengths files ................. 161
8.3.3 Optimizing atomization temperature.......... 118
9.4 Copying to the clipboard ............................ 161
8.3.4 Graphical representation of furnace
program / graphite tube coating ................ 120 9.4.1 Copying results to the clipboard ................ 161
8.3.5 Further furnace functions .......................... 122 9.4.2 Copying graphics as screenshots .............. 161
8.4 Hydride system ......................................... 125 9.5 Saving results in ASCII/CSV format........... 162
2 Issue 09/2011 ASpect CS

Contents
10 User Management .................................. 163 11.2.1 General ..................................................... 177

10.1 Hierarchy and access to functions ............. 163 11.2.2 Background correction “without
reference”.................................................. 178
10.2 User Management setups ......................... 164
11.2.3 Background correction "with reference" .... 178
10.2.1 Configuring user management .................. 166
11.2.4 Background correction "IBC" ..................... 179
10.2.2 Creating a new user account ..................... 169
11.2.5 Spectrum subtraction (correction of
10.2.3 Modifying a previously created user
permanent structures) ............................... 179
account ...................................................... 171
11.3 Working with Correction Spectra in
10.3 Viewing and exporting Audit Trail .............. 171
ASpectCS Software .................................. 180
10.4 Changing a password ................................ 173
11.3.1 Initial Situation ........................................... 180
10.5 Electronic signatures ................................. 174
11.3.2 Determining Correction Spectra ................ 181
10.5.1 Signing measured results .......................... 174
11.3.3 Compiling a Correction Model ................... 182
10.5.1.1 Displaying signatures ................................ 175
11.3.4 Integration of a Correction Model into a
11 Supplement ............................................ 177 Method ...................................................... 184
11.1 Overview of markings used in the display 12 Index ........................................................ 185

of values .................................................... 177
11.2 Description of the algorithms used for
spectral background correction ................. 177

Contents

ASpect CS Software
1 ASpect CS Software
ASpect CS is the control and data analysis software for the High Resolution Con-
tinuum Source Atomic Absorption Spectrometer
• contrAA 300 for flame technique and hydride/Hg-cold vapour technique
• contrAA 600 for graphite tube technique and hydride/Hg cold vapour tech-
nique and HydrEA technique
• contrAA 700 – a multi-function system for flame technique, graphite tube
technique, HydrEA technique and hydride/Hg cold vapour technique
The following accessories from Analytik Jena are supported by this software:
• AAS Autosamplers AS 51s and AS 52s
• SSA 600 solid autosampler
• MPE 60 micro pipetting unit for graphite tube technique
• Hydride system HS60 / HS60A, HS55 / HS55A and hydride injector HS50
(hydride/Hg cold vapor technique)
• SFS 6 Injection Switch (flame technique)
The software supports the unique features of HR-CS AAS, such as simultaneous
background correction by acquiring spectral information in the vicinity of the analy-
sis line, fast element/line change and the fast sequential multielement measure-
ment at continuous sample flow in flame mode. The method parameters for the
measurement procedures can be optimized to the specific demands of the sample
to be analyzed.
The obtained data can be recalculated, exported to various file formats and printed
out.
Described software version

This manual help is based on the version ASpect CS 1.5.
Intended use
ASpect CS software exclusively serves to control the above mentioned high resolu-
tion continuum source atomic absorption spectrometer and to analyze the data
obtained with this device.
The manufacturer does not assume any liability for problems or damage caused by
the non-intended use of ASpect CS.
ASpect CS and the devices to be controlled by it may only be operated by appro-
priately qualified and instructed personnel. The use must be familiar with the infor-
mation given herein and in the user’s manual of the device.
1.1 User manual conventions

Carefully read the instructions given in this manual to make full use of the possibili-
ties provided by Aspect CS.
The following symbols and conventions are used to facilitate orientation in the
manual:

ASpect CS Software
This is a note to be followed to avoid operating errors and obtain

correct results.
 Denotes a step of operation.
 Denotes a step of operation that can be used as an alternative to
that described above.
Text format- In the description of operating procedures, menu commands, dialog
ting boxes, buttons, options, etc. are highlighted in bold letters.
Menu commands of a command sequence are separated by slashes
( / ), e.g. File / Open.
Buttons are additionally written in square brackets, e.g. [Save].
Some dialog boxes are subdivided in tabs. The name of the tab is
appended to the name of the dialog box by a dash, e.g. Options -
View.
1.2 Starting and exiting ASpect CS

Starting ASpect CS
 To start ASpect CS, click on the [Start] button on the Windows desktop. Open
the Programs folder and look for the ASpect CS folder. In this folder, click on
ASpect CS.
 Alternatively, you may click on the ASpect CS icon on the Windows desktop.
ASpect CS is being started.

If the User Management has been installed, you will be prompted to enter user
name and password. The ASpect CS workspace will become accessible only, if the
entry of these data was successful.
If the application is already running, another program instance of this application
will be opened in offline mode . In this mode, there is no communication with the
device. However, all other functions, such as the development of methods or the
loading of results can be used parallel to the running measurement mode of the
first program instance.
After you started the application, the Main Settings window is opened.
Exiting ASpect CS
 To exit the application, activate menu command File / Exit.
 Alternatively, you may close the program in the Main Settings window by a
click on the [Exit program] button.
 If, at this time, method, sequence or sample information data files are open
that have not been saved yet, you will be informed accordingly. If you want to
save these files, click on [Yes].
 A request for a software controlled system cleaning is displayed when working
with a hydride system.
 If the xenon lamp is still on, a request for the switch-off of the lamp will appear.
After you have switched off the lamp, keep a wait time of 30 s before switching
off the contrAA. The countdown of the wait time is graphically displayed on the
screen. Afterwards, you can switch off the contrAA by hardware.

ASpect CS Software
1.3 General information on operation

1.3.1 The workspace
After the start of ASpect CS software, first the Main Settings window is opened. In
this window, you must select the technique and the task to be performed. After the
confirmation of your choice by [OK], the application workspace becomes accessi-
ble. The workspace contains the typical elements of Windows applications, such
as:
• Title bar with the standard buttons for resizing the window and closing the
program
• Menu bar
• Toolbar and icon bar with buttons for fast access to important program
functions
• Workspace for the result list and further windows (e.g. methods)
• Status bar at the bottom edge of the window
1.3.2 The Help function

You can get help on the operation of ASpect CS via the menu command ? / Con-
tents and Index.
? / Contents and Activating ? / Search ..., you can search for specific help subjects by the entry of
Index key words.
? / Search ... While working with Aspect CS windows and dialogs, you can activate context-
sensitive help by pressing function key [F1].
The program pops up brief information (tool tips) on buttons of toolbar and icon bar
and other buttons as well as on the table headers in windows Method, Sequence
and Sample ID while you move the mouse pointer across the button.
1.3.3 The menu bar

The menu bar is arranged at the top edge of the Aspect CS workspace. It allows all
operating actions of software to be started. Menus and buttons not accessible for
the current contents of the workspace appear grayed out. Some menu items, such
as the print function, are displayed dependent on other windows being open.
Menu Description
File Creating, opening and saving method, sequence and sample
information files.
Opening results files.
Setting up a printer and printout.
Starting offline or online program instance.
Activating the Main Settings window.
Exiting the application.
Direct recall of method and sequence files opened recently.
Edit Copying and pasting the contents of textboxes and input fields.
Copying selected rows of the result list to the clipboard.
Deleting the contents of the result list.

ASpect CS Software
View Opening and closing windows showing graphs and information

during the analysis process e.g. signal curves.
Selecting the scale of the signal axis of graphs.
Method Devel- Activating windows required for method development.
opment
Routine Activating commands controlling the measurement procedure.
Extras Activating the Data Management window.
Activating the Options window.
Window Activating and arranging open document windows.
? Online Help and information on software version
1.3.4 Frequently used control elements

Various button, mouse and keyboard functions are used in Aspect CS, which al-
ways have the same or very similar meanings.
These control elements are described here in general. Specific information is giv-
en, where necessary, in the description of the respective windows.
Buttons
The function of icon buttons is indicated by means of tool tips displayed when the
mouse pointer rest on the corresponding button.
[OK] Closes the window and accepts the settings.

[Cancel] Closes the window rejecting possibly changed settings.
[Accept] Accepts the settings without closing the window.
[Close] Closes the window; settings are not saved permanently.
[Open] Opens a selection window for loading a file or data record.
[Save] Opens a selection window for saving a file or data record.
[...] Opens a selection dialog box, e.g. for file path selection.
Opens the Print window. From this window, you can print out
the contents of the active document window or export it to a
file.
Lists
In some of the windows, values are to be entered directly in a list. Dependent on
the type of entry, the list cell behaves like an input field, a selection list, or a spin
box.
 To select a row of a table, click on the corresponding row in the first table
column highlighted by a gray background. Afterwards, you can move the line
cursor with the [↑] and [↓] buttons.
 To change the width of a column move the mouse pointer to the correspond-
ing border line in the column head until it turns into a double-headed arrow.
Keeping the left mouse button depressed, you can then drag the border line to
adjust the desired width.
 In input fields, the following functions are additionally available:
• [F2] activates the edit mode. In this mode, the [←] and [→] keys are used
for editing character by character. Renewed pressing of [F2] reactivates

ASpect CS Software
the standard mode where the cursor keys are used to navigate between
the cells.
Edit / Copy • Text can be copied to the Windows clipboard via menu command Edit /
Copy or key combination [Ctrl+C] and inserted via menu command Edit /
Edit / Insert
Insert or key combination [Ctrl+V].
Buttons accessible in lists
[Append] Appends a new table line to the end of the list.

[Insert] Inserts a new table line before the selected line.
[Delete] Deletes the selected table line.
Shifts up the selected table line by one position.
Shifts down the selected table line by one position.
Transfers the value of the active cell to all following table lines (table
columns). If the Increm. check box has been activated, this value
will be incremented automatically, e.g. Sample001, Sample002 ... .
Graphs
In graphs, you can open a context menu by clicking the right mouse button. This
menu provides options for copying either the graph or the entire window to the
Windows clipboard.
In several graphic windows, additional icon buttons are accessible:
Activates the zoom mode. With the left mouse button pressed you can
select an area of the graph to be zoomed in.
Deactivates the zoom mode and resets the graph to the original scale.
Activates the text mode. Keeping the left mouse button pressed you
can draw a frame and enter text that shall be added to the graph.
A double click on the existing text opens the window for editing or de-
leting the text. With Ctrl+right mouse button you can move the text.
Activates the select mode in graphs of signal curves or spectra. Click-
ing the left mouse button adds labels to the measuring points; pressing
Shift+right mouse button deletes all labels.
1.3.5 Function keys
[F1] Activates the context-sensitive online help.

[F2] Activates the list cell edit mode.
[F5] Starts printing a hardcopy of the screen.
[F6] Measures the selected row of the sequence (Menu command Routine
/ Run selected sequence row…).
[F7] Displays additional presentation windows (signal curve, flame state).
[F8] Closes additional presentation windows (signal curve, flame state).
[F10] Activates the menu bar.
[F11] Continues a measurement stopped before (menu command Routine /
Continue…).
[F12] Starts or stops the measurement process (menu command Routine /
Start or Routine / Stop)

ASpect CS Software
1.3.6 Choosing a printer

If you have already set up a Windows standard printer, this printer will be used in
ASpect CS. To use a different printer, follow this procedure:
File / Printer Set-  Open the Windows standard dialog for printer selection via File / Printer Set-
up… up….
 If the desired printer is not included in the list of available printers, you must
add it under Windows.
Starting from the Windows taskbar, activate Start / Control Panel / Printer /
Add Printer.
1.4 General measurement procedure

The following actions are necessary for a manual or an automatic measurement
procedure:
1. Define the Method parameters (method development).
2. Setting up a Sequence. The sequence specifies samples and actions in the
intended order of execution. Some sample describing data, such as the name
of the sample and its position on the sample tray may also be entered directly.
To store such sample describing data permanently, however, they must be
saved to a sample information file.
3. Additionally, a sample information file can be created. This file contains
sample describing data such as sample name, dilution factor and sample tray
positions. These data are needed if the concentrations shall be back-
calculated to the original sample. Sample information files are text files; there-
fore, they may be created also with external applications.
4. Start measurement.
The results are instantly written to the result database during the measurement.
This central results file is accessed by the integrated data management functions
(export, print ...).
After the start of the measurement, the result data are entered in the result list.
Detailed result presentation (individual values, spectra …) is accessible by selec-
tion of the corresponding table cell. The results obtained last are always appended
to the end of the table; overwriting of results is not possible.
Further data analysis is possible by the Reprocessing function. Measured data
can be prepared for the printout of result reports or exported.

Preparatory settings - Choosing the analytical task
2 Preparatory settings - Choosing the analytical

task
The analytical task is to be chosen in the Main Settings window appearing directly
after program start.
File / Main Set- Alternatively, you may call this window via menu command File / Main Settings.
tings
The choice made in the Main Settings window determines the subsequently pos-
sible activities, entries and displays.
Fig. 1 Main Settings window
Technique
In this field, define the technique to be used for the specific task. The technique
selected here, determines various options accessible for the further program run.
Flame contrAA 300 / contrAA 700

Atomization with burner/nebulizer system
Graphite furnace contrAA 600 / contrAA 700
Electrothermal atomization
Hydride contrAA 300 / contrAA 700
Metal hydride analyses or mercury determination with or with-
out enrichment in a cell
HydrEA contrAA 600 / contrAA 700
Mercury/metal hydride analyses in graphite furnace

Sample state and tube tye

contrAA 600 / contrAA 700
Sample state
liquid Samples are available in liquid (dissolved) state.

For atomization, a furnace type must be selected in addition:
Wall Uses graphite tube without a platform (→ "contrAA
700" manual, section "Graphite tube versions"). Atom-
ization of sample matter occurs at the wall of the
graphite tube.
Platform Uses a graphite tube with platform. Atomization takes
places on the platform.
Selections for tube type will have an influence on the depth to
which the dosing tube of the micro pipetting unit will dip into the
furnace tube.
solid Samples are available in solid state (powder, etc.).
Sample matter is atomized in a special graphite tube for solid
analytics. A sample can be placed in the graphite tube furnace
using the automatic SSA600 autosampler or the manual SSA6
sampler.
Task
For measurement tasks and after a change of the technique, device and accesso-
ries must be reinitialized (see the description of the [Initialize] button further be-
low). Reinitialization of the device is not necessary if you select Data management
or Options.
Routine Automatic run of analysis methods

For methods and sequences a versioning scheme exists. Modi-
fied method or sequences are saved with a new version number.
In routine mode only the current (last) method or sequence ver-
sion can be loaded.
Method devel- Development and test of analysis methods and processes
opment
Data manage- Activates the Data Management window after a click on [OK].
ment
Options Activates the Options window after a click on [OK].
Available accessory
Before you can actually start a measurement, device and PC must be connected to
each other. Verify that the spectrometer and the accessory to be used are con-
nected and ready for operation. Clicking the [Initialize] button releases the detec-
tion and the configuration of the spectrometer and the accessory unit(s) dependent
on the technique selected.
On exiting the Main Settings window with the [OK] button, the system checks the
state of initialization and informs the operator of the necessity of initialization, if
necessary.
Detected accessory units are listed by name. If an accessory is identified as Not
initialized, its initialization was skipped because of the technique selected (e.g. the
hydride system if the flame technique has been selected); if --- is displayed, the
respective accessory was not detected.
In the Date and Time field, the current system time of the PC is displayed.

In the Laboratory field, you can type in a name of maximally 30 characters. The
name entered last is saved and printed out as information on result reports.
If you use the optionally installable user management, the Operator input field
shows the registered user. If you do not use user privilege management, you may
enter the operator’s name manually (30 characters).
For trainings and demonstration purposes, you may operate ASpect CS without an
AAS device being connected. To this end, activate the Simulation checkbox.
Then, all device functions (including data acquisition and analysis) will be run in
simulation mode.

Customizing ASpect CS
3 Customizing ASpect CS
3.1 General settings
In the Options window, you can choose the following settings, which apply to the
complete operation of ASpect CS:
• Display options
• Save paths of files
• Parameters for data export
• General measurement settings
The options selected in this window remain set after exiting and restarting ASpect
CS.
Extras / Options...  Activate the Options window with menu command Extras / Options... or by a
click on the
button.
 Alternatively, in the Main settings window, you may activate the Options op-
tion button in the Task field and click on [OK] (→ "Preparatory settings -
Choosing the analytical task" p. 11).
3.1.1 View options

In the Options - Display window, define the functions and elements that shall be
accessible on the workspace.
Display tab
Fig.2 Options – Display window

Display
Show toolbar Shows the toolbar.

Show icon bar Shows the icon bar at the selected position.
(The position of the icon bar may also be changed by drag-
ging it with the mouse. However, this setting will not be
saved).
Show start Displays the start graphic of the application.
screen The program start is slightly faster if you deactivate this
option.
Subwindows can Activates the Maximize system button (square) in subwin-

be maximized dows (MDI windows), thus allowing these windows to be
maximized to the size of the result list.
Calib. Table col- Transpose the calibration table for the standards definition
um by column so that the calibration standards are displayed column-wise
and the selected lines are displayed row-wise.
Hide results Results windows are hidden when sub-windows are open in
windows auto- order to prevent overlapping windows.
matically
Table colors
A click on the [...] button opens the color selection dialog. There, you may choose
predefined or newly defined colors as list background.
Use PrtScr key By default, the printout of the hardcopy of the screen is start-
for hardcopy ed with [F5]. In this case, the [PrtScr] key of the keyboard is
function used for the Windows clipboard function.
If this checkbox is activated, the [PrtScr] button starts the
printout of the screen hardcopy.
This function becomes active only after restarting ASpect CS.
Scientific Mode Activates spectrum presentation.
If this option has been deactivated, the functions for the
presentation and editing of spectrum data are not accessible.
With the [Default settings] button, all currently set options are reset to default set-
tings.
Signals
Button [...] opens a color selection dialog. Pre-defined or custom colors can be
selected for displaying the net signal or the background signal (graphite furnace
technique).
3.1.2 Save paths

The save paths selected for the program and the files during installation are dis-
played in the Options - Folder window.
Folder tab
Program Installation path of executable files.
Work directory Directory for user data. The work folder contains further sub-
folders.
The work directory is defined during installation or through set-
tings in User Management.

Temporary data Folder for files created temporarily by the application.

Sample infor- Default path for opening and saving sample information files.
mation You may change this path, i.e. you may choose a different path
for opening and saving sample information files.
Export/Import Default path for the export and import of method and sequence
data.
You may change this path, i.e. you may choose a different path
for export and import.
Results Folder for results files. This default folder may contain addition-
al subfolders for result storage. These folders are available for
saving results files at the start of measurements.
Application data Folder for data used internally by the ASpect CS software.
With the [Add…] button, you can create new subfolders to the Results folder for
saving results. Besides, it is possible to delete and rename empty folders here.
3.1.3 Export options

In the Options - ASCII/CSV Export window, you can define the parameters for
exporting results to ASCII files. The chosen parameters apply to both types of data
ASCII/CSV Export export: automatically continuous and manual (→ "Saving results in ASCII/CSV
tab format", p. 162).
Options
Decimal separa- Defines the separator for decimal numbers.

tor
List separator Defines the character separating the individual elements of a
list.
In the Result fields for export field, you may define which columns of the result
table shall be exported to the ASCII file. All exports all columns of the selected and
non-selected tabs of the result list, only selected fields opens a list in which you
can choose the columns to be exported.
A click on the [Default settings] button resets all options and stored window loca-
tions to default settings.
3.1.4 Options for continuous ASCII export

The Options - Continuous ASCII Export window serves to activate the export of
result data during the analysis process. The export file is updated each after the
Continuous ASCII output of a new line in the process and result window. The result data will be ap-
Export tab pended to already existing files.
Further export options may be defined in the Options - ASCII/CSV Export win-
dow.
The export function is activated by selecting the Continuous ASCII Export of re-
sults data checkbox.

File name
[Method The file name corresponds to the name of the method. The file
name].csv name extension used is ".csv".
The file is saved to the default Export/Import path (Options -
Paths).
[Results file The file name corresponds to the name of the results file. The
name].csv file name extension is ".csv".
The file is saved to the default Export/Import path (Options -
Paths).
other You may freely define file name and save path. A click on the
[...] button opens the file selection dialog for the selection of an
existing file.
Continuous ex- The spectra are exported as CSV files to the specified path.
port of spectra The filename is created automatically using "Row number-
(CSV) Sample name-Line-Replicate", e.g. 0007-Sample-Al309-
02.csv.
Export path A click on the [...] button opens the path selection dialog for the
selection of an export path.
3.1.5 Options for analysis sequence

In the Options – Analysis sequence window, you can define general options for
the analysis process.
Analysis sequence
tab
Fig.3 Options – Analysis sequence window
Stop after following errors
Offset of optical The analysis sequence is stopped if the optical system is not
system correctly adjusted.
Please check the correct function of the spectrometer (→
"Device function test on contrAA" p. 99).

Invalid calibra- If activated, the analysis sequence will be stopped if the cali-
tion function bration function could not be calculated.
Additional error checks
Monotony of If activated, the calibration points will not be tested for monoto-
calibration ny.
points The monotony test serves to determine if higher standard con-
centrations also lead to higher measured values.
Autosampler If activated, the signals from the fill level sensors of the au-
level sensors tosampler and the waste bottle will be checked.
Display windows
Signal plot If activated, a window is displayed during the analysis process

showing the curve of the measured signal (e.g. absorbance
curve) as a function of time.
Spectrum plot If activated, a window is displayed during the analysis process
showing the scanned spectral range (e.g. absorbance curve).
Bargraph Show measured absorption or emission as bargraph.
Scaling of max. Defines the maximum of the signal axis for the presentation of
signal value the signal curve and the spectrum.
Auto: Automatic scaling of signal axis.
(Alternatively, you may set this option also via menu function
View / Scale (Abs).)
Report window If activated, a window is displayed during the analysis process
showing status information on the used atomizer (flame, graph-
ite furnace, hydride system).
Sample conc. in If activated, the Sample conc. in calibration curve window is
calibration displayed with the current calibration, and if measured already,
curve the recalibration curve. After the measurement of the sample,
the calculation of the uncorrected concentration from absorb-
ance/emission data is illustrated by red auxiliary lines. If addi-
tion calibration is used, the converted calibration curve will be
displayed.
Furnace camera For graphite tube technique only.
Keeps the furnace camera’s photograph of the graphite furnace
permanently superimposed for viewing at the display screen,
until the preset furnace control temperature Temperature for
shutter to open has been reached (→ "Further furnace func-
tions" p. 122).
This allows you to directly watch as a sample droplet is depos-
ited and drying.
Other
Always save Spectral data is always saved during measurement indepen-

spectra dent of the set method parameters (Method - Output window).
Attach date/time Following a recalculation, the results are automatically export-
to the results ed (→ "Options for continuous ASCII export" p. 16).
filename
Only for graphite tube technique.
Continuous ex- Following a recalculation, the results are automatically export-

port during re- ed (→ "Options for continuous ASCII export" p. 16).
processing

Take-up compo- While the graphite tube cools down, the MPE takes up next
nents during samples. This option may be used to accelerate a measuring
cooling phase sequence.
Beep after end of A beep will sound as soon as the graphite tube has completely
cooling phase cooled down.
Stop after trans- Stops a running measurement program if active and if the
former overheat- transformer for graphite tube technique was found to be in an
ing overheated state. The program will not continue in this case.
Interrupts a running program on detecting a transformer over-
heat situation if disabled. Resumes the interrupted program
after the transformer has cooled down.
Readjust wave- If activated the wavelength is readjusted for each replcate
length before measurement. This improves precision (default is active).
each measure-
ment
Formation re- If activated a message is displayed when starting a measure-
quired after ment without tube formation after opening the furnace or
opening furnace switching on the instrument.
3.2 Specifying units, QC and stock standards

In the Data management window, the units available for the entire application as
well as frequently used stock standards and QC samples are managed.
 To activate the Data Management window, activate menu command Extras /
Data... or click on symbol button
Extras / Data
.
3.2.1 Specifying units of measurements

You can define the units of measurement available throughout the application in
the Data management – Units window. Five preferred units are available each for
Unit tab liquids and solid reference samples: mg/L, µg/L, ng/L, µg/mL and ng/mL (liquids);
mg/kg, µg/kg, ng/kg, µg/g and ng/g (solids). These units cannot be edited, you
may, however, freely define other units. For freely defined units it is necessary to
enter the conversion factor under Factor:
Unit Name of the unit (max. 10 characters)

Comment Remarks on the unit (max. 20 characters)
Factor Factor 1 corresponds to 1 µg/L or µg/kg, factor 1000 corre-
sponds to 1 ng/L or ng/kg
Type solid = unit used for a solid sample, liquid = unit used for a liquid
sample (solution)
The [Append] and [Insert] buttons serve to append user-defined units to the end
of the list or insert them above the currently selected row. With the [Delete but-
ton], you can delete user-defined units, the preferred default units, however, can-
not be deleted. To permanently save any changes on this tab, click on Save.

3.2.2 Specifying stock standards and QC samples

The composition of frequently used stock standards and QC samples is managed
under Data management – Stock std/QC samples. The composition of these
Stock std/QC frequently used multielement standards is then available throughout the applica-
samples tab tion.
Selection Check boxes to switch between the list of Stock standards

and QC samples
Name Here, enter the name of the standard (max. 20 characters).
Elements and The element concentrations are to be entered in the format
concentrations element symbol concentration; in the given example e.g. Ni
0.5; Cu 10; Fe 25; Co 0.005.
(You may also select the elements and enter their concentra-
tions via the list popping up after a click on the [Concentra-
tions…] button.)
Unit Enter the name of the standard unit here (max. 10 characters).
[Append] Appends a new row to the end of the list.
[Insert] Inserts a row in the list above the currently selected row.
[Delete] Deletes the selected row.
[Concentration] Opens the input window for the entry of the element(s) and
concentration(s) of the selected standard.
Entry of standard concentrations

 Select a row on the standard list.
 Click on the [Concentration…] button to open the Concentration entry input
window with the element list.
 Enter the concentrations of all elements contained in the standard and confirm
your entries with [OK].

Methods
4 Methods
4.1 Creating method parameters
 To create a new method, activate menu command File / New Method....
This will bring up a selection dialog with the following options:
File / New Meth- Based on de- Opens the Method window for the entry of new method
od... fault parameters parameters and with editable default settings for calibration
and statistics.
Based on cur- Opens the Method window with the currently set method
rent parameters parameters.
Based on saved Activates the Load method dialog.
method… After the selection of the method, its parameters are dis-
played in the Method window.
 Choose the desired option and confirm your choice with [OK] to open the
Method window either directly or via the Load method dialog.
 Alternatively, activate the Method window by a click on the button or

Method Develop- by menu command Method Development / Method....
ment / Method... This will bring up the Method window with the currently set method parame-
ters.
The functions of labeled and icon buttons in the Method window are described in
section "Frequently used control elements" p. 8.
 Activate the selected method parameters with the [OK] or the [Accept] button
for the following analysis.

Methods
4.1.1 Lines tab – Choosing element lines

The element lines are to be specified in the Method – Lines window. You may
choose a maximum of 200 different lines.
Lines tab
Fig.4 Method – Lines window with selected element lines
The following line parameters must be defined:
Elem. Element symbol (up to 2 characters)

* Measuring mode: Abs = Absorption mode
Measuring mode: Ems = Emission mode
Wavel. [nm] Wavelength of analysis line in nm
Int. mode Mean: Signal averaging over the integration time
Area: Measurement of the peak area over the integration
time
Height: Measurement of the peak height over the integration
time
Line Designation of analysis line
You can choose a free name, which serves to clearly identify the
analysis line (10 characters).
Read time Analysis time for a repeat measurement in seconds (max. 600 s)
Group Only flame technique

Analysis lines of the same group number are measured at con-
tinuous sample flow, i.e. while the system drives to the next
analysis line and adjusts the burner, the injection tube of the
autosampler remains immersed in the sample.
With analysis lines of different groups, the injection tube comes
up from the sample. The sample flow to the burner is stopped.

Methods
Order Order in which the analysis lines within a group are measured.
With the [Opt.] button, you can have their order optimized auto-
matically, i.e. the lines will be measured by increasing fuel gas
flows.
With graphite tube technique, Order defines the order in which
lines will be measured.
Advice on the selection of the "Int. mode"

Mean (value): To be used for applications without injection module with sufficiently
high sample volumes available (flame technique; seldom: hydride technique)
Area and Height: For the atomization of a defined sample volume (in hydride
technique or, in combination with an injection module, in flame technique).
Inserting a new element line

 In the Method – Lines window, click on [Append] to open the den Select El-
ement/Line dialog.
Fig. 5 Select Element/Lines dialog
This selection dialog contains the periodic system with the selectable elements
being displayed as blue buttons. Additionally, it shows the line table with the follow-
ing columns:
Element Element symbol

Line [nm] Wavelength in nm
Type P = Primary line, S = Secondary line
 By activating the Element or the Line option button, the line table is sorted
increasingly by either the chemical symbol or the wavelength.
 If you click on an element symbol in the periodic system (blue buttons are
selectable elements), the lines of the selected element will be displayed in the
line table.
Alternatively, you may enter the element symbol in the Select Element text
box.
To have the complete element list displayed again, delete the entry in the Se-
lect Element text box.

Methods
 To select the analysis lines to be used, successively click on the corresponding

rows in the line table.
The selected analysis lines appear under the periodic system.
 To undo the selection of a line, click on it once more in the line table.
With the [Deselect] button, you can deselect all lines previously selected.
 Confirm your choice of analysis elements/lines with [OK].
 Only flame technique:
Click on the [Display atomization parameters…] button to open a window
with recommended flame parameters. These flame parameters appear as de-
fault settings on the Flame tab.
 [User-defined lines] can be clicked to open the Edit lines dialog screen. It
allows you to enter new lines for analysis. An element symbol and a wave-
length must be specified for each user-defined analytical line. On selection of
[Add], the related data will be transferred to the lines table. User-defined ana-
lytical lines are marked with "*" in the lines table of the Select Element/Line
window.
The selected elements/lines will appear on the table in the Method - Lines win-
dow.
Note
You may also choose several lines of different sensitivities of a single element.
4.1.2 Flame tab – Flame parameters

Selected technique Flame technique
Burner parameters and gas flows for flame technique are adjusted in the Method -
Flame window.
Flame tab
Fig.6 Method - Flame window with burner and gas flow settings

Methods
Line-independent settings for the burner/nebulizer system

(BNS)
First, adjust those parameters that apply to the complete method and that cannot
be varied for the analysis of individual elements/lines.
Flame
Type Selection of type of flame

C2H2/air: Acetylene/air flame (fuel flow = 40 – 120 L/h)
C2H2/N2O: Acetylene/nitrous-oxide flame (selectable only
with 50 mm burner)
(fuel flow = 120 – 315 L/h)
Scraper The scraper is activated for the automatic analysis process with
the 50-mm burner and acetylene/nitrous oxide flame. Now and
then, the burner head is automatically cleaned by the scraper.
Cleaning can be performed before each sample, before each
group,before each element or before each replicate.
Ox. control off: Operation without auxiliary oxidant
on: Operation with auxiliary oxidant
Note
When working with auxiliary oxidant, optimize the flame parameters manually (→
"Manual flame optimization", p. 108).
Burner/nebulizer
Type Selection of the used type of burner: 50 mm or 100 mm

Burner angle Angular position of the burner relative to the optical axis
[deg]: The burner angle must be set manually on the burner (normally
it is set to 0°). The entry of the value is optional. It only serves
to complete analysis method and report data.
Adjustment range: 0 – 90°
Nebulizer rate Aspiration rate of the nebulizer
[mL/min] The aspiration rate is a nebulizer-specific value. The entry of
the value is optional. It only serves to complete analysis method
and record data.
Adjustment range: 1.0 – 9.9 ml/min
Line-dependent parameters for gas flow and burner height

In the table, you may directly enter the fuel gas flows and the burner height set-
tings, if these data are known for the selected elements.
The corresponding values may however also be determined manually or automati-
cally in the program for flame optimization and transferred to the table of line-
dependent flame parameters in the Method – Flame window (→ "Optimizing the
flame", p. 108).

Methods
4.1.3 Furnace tab – Parameters for graphite tube furnace

Selected technique Graphite tube technique
Method Furnace is the window that provides a survey of essential parameter set-
tings for furnace programs to atomize the various elements being analyzed.
Furnace tab
Fig. 7 Method – Furnace window with furnace parameter settings
To serve as default settings for atomization of the various elements using EA tech-
nique, the respective furnace program data from the cookbook are preset. Regard-
less of that, a furnace program can be edited for any analytical line in the Furnace
window and a currently selected method can be transferred (→ "Editing a furnace
program" p. 112).
The related list includes the following furnace program parameter items:
Line Name of element line

Tot. Total number of furnace program steps
Dry. Number of drying steps in a furnace program
Pyrol. Temp. Pyrolysis temperature in °C
Atomize Detailed display of temperature data during atomization phase
Temp. End temperature of atomization phase
Ramp Temperature variance during atomization phase in
°C/s
Gas Feeds inert gas
Inj. No mark Sample is injected before start of furnace program
"*" Sample is injected at some later point in time
Pretr.. Thermal preparation
Sample and modifiers will be thermally prepared if this item was
marked.
Enr. Enriches the sample if marked
Modifier Additionally involved modifiers. For each measurement, a max-
imum of five additional modifiers can be selected.

Methods
Control buttons
[Edit furnace Opens the Furnace – Furnace program window that provides
program] a full display of the furnace program. Furnace parameter set-
tings can be adapted for any element line subject to analysis
(→ "Editing a furnace program" p. 112).
[Accept furnace Validates the parameter settings of a marked analytical line for
program] all subsequent lines in the list.
[Modif.+Extras] Opens the Furnace – Modif.+Extras window with setting op-
tions for additional modifiers, enrichment and thermal pre-
treatment of element lines (→ "Matrix modifiers, selections for
enrichment and pretreatment" p. 115).
"Clean furnace" as an additional sequence action

The furnace will be cleaned by baking out on completion of a furnace program for a
given element line in all cases. In addition, a further cleaning step can be defined
for a particular sequence by selecting Clean furnace. Required settings for this
action can be made in the Action clean furnace subarea.
Temp.[°C] Specified end temperature for baking (cleaning) process.

Ramp [°C/s] Rate of temperature change
Hold [s] Holding time at end temperature
(→ "Specifying sequences of samples and actions" p. 60)
4.1.4 Hydride tab – Specifying the hydride system

The hydride system parameters are to be adjusted in the Method – Hydride win-
dow. The hydride system connected is detected during device initialization.
Hydride tab
The parameters for the hydride injector HS50 are defined using flame technique in
the Method – Sample transport window (→ "Auto sampler for flame and Hy-
dride/HydrEA technique" p. 32).
Note
The commands for additional washing or loading of the hydride system are re-
leased from the Hydride System window (→ "Hydride system", p. 125).

Methods
Fig.8 Method - Hydride window
Mode
You can choose among different modes depending on the equipment of the hy-
dride system.
Hydride (contin- Operation with autosampler or manual.

uous) The reaction takes place in the reactor under continuous condi-
tions.
Hydride (batch) Manual mode.
The sample is pipetted into the reaction beaker (max. 20 mL).
The beaker is to be clamped gas-tightly to the head of the
batch module. With the first channel of the 4-channel peristaltic
pump, the reductant is pumped into the reaction beaker. The
fast and partly vigorous reaction liberates metal hydride or
atomic Hg vapor.
FBR mode Not intended for HydrEA technique
(Fast Baseline Return, FBR) (accessible only in continuous
mode)
After the maximum absorption has been reached, the direct
argon gas flow purges the cell free during Wash Time 2 thus
causing a fast return of the signal to baseline level.
Cell temperature / Pump speed level
Cell temp.[°C] Not intended for HydrEA technique

For the hydride formers As, Se, Sn, Sb, Te and Bi, the cell tem-
perature is selectable in the range between 600 °C and 960 °C.
For Hg analyses, you may choose between RT (room tempera-
ture < 60 °C) or 150 °C.
The cell is heated to the selected cell temperature at the
start of the analysis process, or you may start it in the Hy-
dride System window.

Methods
Pump speed Four speed levels (1 - 4) are available for the transport of the
level sample (in continuous mode) and the components.
In continuous mode, the supplied sample volume is determined
on the basis of the pump speed level selected and the reaction
time.
System cleaning
System cleaning may be selected optionally after every sample measurement.
Between sam- System cleaning after each sample measurement

ples off System is not cleaned.
Cleaning with acid System is rinsed after every sample
with diluted acid.
The corresponding time is to be defined under Wash
time acid. When half of the wash time is over, the
sample path is switched to the reactor.
Cleaning with reductant + acid This cleaning method
is the method of choice if the system is heavily con-
taminated (samples with high element contents).
First, the system is rinsed with reductant for the se-
lected Wash time reductant. This process is fol-
lowed by a wait time (soak time) to allow the re-
ductant to take effect onto the deposits on the tube
walls. Finally, the system is rinsed with diluted acid
for the Wash time acid.
at action The system cleaning can be set as an programmable special
action (→ "Specifying sequences of samples and actions" p 60).
This additional cleaning step can be inserted after samples with
high analyte content.
Cleaning with acid see option Between Samples.
Cleaning with reductant + acid see option Between
Samples
Pos. reductant Position of reductant on the sample tray.
[Wash times...] A window is opened for the defintiion of three wash times:
Wash time reductant, Soak time, Wach time acid.
Please set these values according to the selected cleaning op-
tions.
Operation times
The operation times are to be adjusted dependent on the selected operating mode.
All operation times are entered in seconds.
Load time Time in which the sample pump loads the sample tube up to
the two-valve assembly with sample. This time is needed only
for the first measurement of a new sample.
Prewash time Time for purging the beaker with argon before the reaction
(for the analysis of hydride formers).
The prewash time is used to purge off air in order to prevent
an oxy-hydrogen reaction in the following reaction.
Reaction time Time in which the sample pump pumps sample into the reac-
tor. This is the crucial parameter for the supplied sample vol-
ume and the measuring sensitivity.
Pump time Time in which reductant is pumped into the beaker in order to
start a reaction.

Methods
AZ wait time Time directly preceding the baseline (auto zero) adjustment.
Wash times 1 … 3 Times used to convey the reaction gas by means of the argon
flow. The transport paths are different in the individual phases
for the various operating modes.
The transport paths can be presented graphically.
Heat. Time collec- Time in which the collector heating is on in order to release
tor the enriched Hg.
Cool. Time collec- Time in which the collector is ventilated in order to cool it
tor down for a new enrichment cycle.
Gas flows Defines the argon flow flowing in the phases displayed left of
it. The adjusted gas flow applies until a new gas flow can be
entered. The gas flow can be switched over differently often
for the different operating modes. The gas paths for the indi-
vidual phases are illustrated in the graphic of the analysis
process on the hydride system (→ "Hydride system – Graph
of analysis process", p. 30). The gas flows are adjustable in
three steps from 5 to 15 Liters/hour.
Batch Parameters
Sample volumes Here, enter the volumes of the sample being in the beaker.
Enrichment cycles To be defined for the batch mode with Hg enrichment on the
collector.
Define the number of beakers the contents of which is en-
riched.
[Plot] button
By a click on the [Plot] button, you can open the graphic presentation of the gas
paths for the individual phases of the analysis process.
Hydride system – Graph of analysis process
Hydride tab Click on the [Plot] button in the Method - Hydride window to open the Plot win-
dow. This window shows a graphic presentation of the programmed analysis pro-
cess.

Methods
Fig. 9 Plot window: Graphic representation of analysis process with hydride system
The individual phases of the analysis process are shown in colors in the process
chart. By clicking on a particular phase shown by a colored field, the corresponding
parameters appear in the Parameters field, and the adjusted gas flow is illustrated
in the Gas paths and flows field. The process is determined by the operating
mode selected on the Hydride tab.
Graphic for If sample statistics has been activated, the different processes
can be displayed for the first, the next and the last measure-
ment.
Gas paths and This flow diagram shows the gas paths of the hydride system.
flows The modules of the system are shown with their connection
tubes (for argon and reaction gas). The modules include React.
(Reactor), GLS (Gas-Liquid-Separator), Coll. (gold collector),
Batch (Batch module) and Cell or furnace.
In the process graph, click on the phase the gas flow of which
you want to get displayed. The gas path is marked in red and
the argon flow displayed numerically in L/h.
Parameters This field serves to display and edit the operation times, meas-
uring times and the corresponding gas flows of a selected
phase of the process.
Click on the phase of interest. The name and the numerical
value of the operation or measuring time /gas flow will be dis-
played and can be changed. The process graph will be updated
accordingly when you change a parameter.
Line Select displayed line data.

Methods
4.1.5 Set auto sampler - Sample transport tab

4.1.5.1 Auto sampler for flame and Hydride/HydrEA technique
In the flame technique the auto samplers AS 52s have a dilution function and AS
51s do not. The samples can also be fed manually to the burner-nebulizer-system
Sample transport is preferred. As an option it is possible to use the injection switch for both automat-
tab ic and manual mode. The hydride injector HS 50 is also set on the tab Sample
transport.
Fig. 10 Method – Sample transport window with activated autosampler for flame
techniques
The Method – Sample Transport window allows you to specify parameters for the
autosamplers:
• turning a sampler on
• Wash modes
• automatic dilution steps as part of an analysis
• using Flame technique:
Involvement of SFS 6 injection switch or HS 50 hydride injector
Accessories
Autosampler Use the connected and initialized autosampler.

If deactivated the sample is supplied manually without au-
tosampler.

Methods
Injection switch The SFS 6 Injection switch can be used in combination with an
SFS autosampler or in manual mode. On the one hand, it allows for
permanent intake of wash or carrier solution and for the burner
to be held at a constant temperature by the aerosol, on the oth-
er hand it allows for reproducible measurements of small sam-
ple volumes.
The injection module can also be used for processing time con-
stant signals (mean integration).
Injection time: The time the valve of the SFS 6 opens the
sample path to nebulize the sample and convey the
aerosol to the burner. The time depends on the
highest concentration to be expected. Typical val-
ues: 0,5 ... 2.0 s.
Load time: The time needed to fill the sample aspiration
path between sample cup and injection module with
new sample.
Hydride injector The hydride injector HS 50 is a purely pneumatic batch system
HS50 for manual operation. It consists of batch installation and cell
holder with quartz cell. The reductionagent solution is trans-
ported pneumatically from the supply bottle into the reaction
tank. The quartz cell is heated by the flame. The operation
times of HS50 are controlled by the AAS software in a simple
way.
Peak area mode as well as peak height mode is possible.
The measurement procedure is divided in following parts: Pre-
wash – Autozero – Reaction/Integration.
Reaction time Set reaction time.
During the reaction phase reaction agent is trans-
ferred to the reaction beaker. The measurement
signal acquisition starts simultaneously. The integra-
tion time has to be set in a way to acquire the total
signal.
Prewash time Set prewash time.
During the prewash time the reaction beaker is
flushed free from air. The prewash phase is omitted
for the determination of Hg because the argon flow
is necessary in order to transport the Hg out of the
sample.
Sample volume Define sample volume.
Delay time Time which is needed to transport the sample to the atomiza-
tion unit (e.g flame or reaction chamber in the hydride system).
The time is essentially determined by the length of the sample
tubes. This time is needed to convey the sample to the flame.
Use autosampler for automatic dilution

In connection with the AS 52s an automatic sample dilution can be carried out.
Individualized dilution factors can be set for each sample in the Sample-ID window
(→ "Create information data for samples and QC samples" pg. 63).
In the method set the general parameters for the dilution (Dilution mode and Fill
level in the mixing cup).
In addition you can activate an automatic Dilution if concentration exceeded. If
the value for concentration is found to exceed the measuring range as determined
by the respective calibration graph by more than 10 %, the sample will be diluted.

Methods
With AS 52s, dilution is performed in the mixing cup. Required volumes are math-
ematically determined as part of a program sequence, depending on the extinction
value for undiluted solution state. Once calculated, the analyte volume is intro-
duced into the mixing cup and the mixing cup is then filled with diluent solution to
the predefined fill level. The amount of diluent solution is drawn from the storage
bottle for diluent solution.
Dilution mode in mixing cup

Dilution if conc. Dilutes sample solution as described above if active and having
exceed detected on exceeding concentration level.
Mixing cup level The fill level to which the mixing cup will be filled up with diluent
[mL] solution.
Specify washing steps

While a measurement sequence is running, you can specify washing steps to clean
the various sample paths inside the system and its accessory units.
Wash mode off Wash mode switched off. No rinsing performed au-
tomatically.
after sample Washes after each sample, but not within a sta-
tistical series.
Wash time Time in which the rinsing agent is aspirated in the wash cup.
Includes washing of tube path and burner-nebulizer system.
Mixing cup cy- Number of wash cycles for mixing cup.
cles Fills mixing cup with wash liquid/diluent solution and drains it
again in one cycle.
Controlled cleaning
Where analyzed samples are of a kind that result in exceeding the calibration
graph working range by more than 10 %, the graphite tube, the burner-nebulizer
system (flame technique) or the hydride system may be washed as may be appro-
priate for the currently selected technique, in order to remove contamination from a
preceding measurement. During the wash, the absorbance/emission is measured
in order to check the cleaning results.
Automatic controlled cleaning should be performed following measurement of high-
ly concentrated samples, notably, with Dilution on conc. exceeding mode active.
Controlled Will automatically trigger controlled cleaning on exceeding

cleaning specified concentration level if active.
Control limit The value, to which the signal level must have returned during
rinsing, before the diluted samples / samples of lower concen-
tration are analyzed.
Note
Controlled cleaning can also be defined as part of a sequence, independently of a
concentration exceeded situation.
Note on wash procedure of AS 52s and AS 51s autosampler

To perform washing of the sample aspiration path and the burner-nebulizer sys-
tem, the autosampler arm dips the needle into the wash cup of the autosampler. A
membrane pump delivers wash liquid from a storage bottle for the time the needle
is submerged. Its pump rate is greater than the aspiration rate of the nebulizer or
that of the hydride system, respectively. The complete sample path is cleaned

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(cannula, sample tube, sample injector SFS6 and the burner-nebulizer system).
Surplus amounts of washing liquid will flow off into the waste bottle.
The mixing cup of AS 52s is cleaned by filling with wash liquid/diluent solution and
draining it again in one single cycle.
Parameters for dipping depth and dosing speed

Specific parameters of the autosampler, however, such as immersion depth in the
various cups and pipetter speed levels are to be selected in the separate Au-
tosampler window (→section "Autosampler AS 51/52s" pg. 129). The Au-
tosampler window on this tab can be opened by clicking [Techn. parameters].
4.1.5.2 Autosampler for graphite tube technique (solution analytics)

The graphite tube is fed with the autosampler MPE 60 or MPE 60/2.
Sample transport
tab
Fig.11 Method – Sample transport window with settings for the MPE 60
The Method – Sample Transport window allows you to specify parameters for
these autosamplers:
• turning a sampler on
• Wash modes
• automatic dilution steps as part of an analysis
Delay time Moving the calculated time of the measurement start by the
delay time This time is needed to convey the sample to the
flame.
Use autosampler Use the connected and initialized autosampler.
This option must always be activated in the graphite tube tech-
nique.

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Use autosampler for automatic dilution

In connection with the MPE 60 an automatic sample dilution can be carried out.
Individualized dilution factors can be set for each sample in the Sample-ID window.
(→ "Create information data for samples and QC samples" pg. 63). Method is
available for general parameter settings (mode and position of the dilution agent) to
achieve dilution.
You can also define automatic dilution on exceeding a certain concentration level.
If the value for concentration is found to exceed the measuring range as deter-
mined by the respective calibration graph by more than 10%, the sample will be
diluted.
For the MPE 60 and MPE 60/2 an analyte reduction occurs directly in the graphite
tube. A dilution in the mixing cup as described for AS 52 s is only possible with the
MPE 60 (→ "Auto sampler for flame and Hydride/HydrEA technique" pg. 32).
Dilution mode in graphite tube:

The sample volume will be reduced in accordance
with the dilution factor and placed into the graphite
tube. The remaining balance against the initial sam-
ple volume will be replaced by diluent liquid.
reduced volume:
The sample volume will be reduced in accordance
with the dilution factor and placed into the graphite
tube. The remaining balance against the initial sam-
ple volume will not be replaced by diluent liquid.
in mixing cup:
Dilution takes place in the mixing cup. The volume is
always filled up to 500 μl.
Dilution if conc. Performs dilution as described above if active.
exceeded
Diluent position Selects position of diluent on the sample tray.
Specify washing steps

While a measurement sequence is running, you can specify washing steps to clean
the various sample paths inside the system and its accessory units.
Wash mode off Wash mode switched off. No rinsing performed auto-
matically.
between samples
Washes after each sample, but not within a statistical
series.
between measurements
Cleaning after each statistic run
after each component
The autosampler is washed after transfer of each
component into the graphite tube (modifier, standard,
sample, etc.).
Wash cycles Number of wash cycles per wash, 1 to 5
again in one cycle.
Controlled cleaning
If samples are analyzed which result in the calibration graph working range being
exceeded by more than 10%, the graphite tube may cleaned by baking out in order

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to remove contamination from the previous measurement. During the cleaning, the
absorbance/emission is measured in order to check the cleaning results.
Automatic controlled cleaning should be performed following measurement of high-
ly concentrated samples, notably, with Dilution on conc. exceeding mode active.
Controlled clean- Will automatically trigger controlled cleaning on exceeding

ing on conc. ex- specified concentration level if active.
ceeding
Control limit The value, to which the signal level must have returned
during cleaning, before the diluted samples / samples of
lower concentration are analyzed.
Note
Controlled cleaning can also be defined as part of a sequence, independently of a
concentration exceeded situation.
Note on wash procedure for MPE 60

Following acceptance of the samples or other liquids the dosing tube is automati-
cally cleaned with the cleaning liquid found in the storage bottle (deionized water,
slightly acidified with 0.1 N HNO3). Here the cleaning liquid is pumped from the
storage bottle through the dosing tube and into the wash cup of the autosampler.
Parameters for dipping depth and dosing speed

Specific parameters of the autosampler, however, such as immersion depth in the
various cups and pipetter speed levels are to be selected in the separate Au-
tosampler window (→ "Technical parameters of the autosampler MPE 60" pg.
139). The Autosampler window on this tab can be opened by clicking [Techn.
parameters].
4.1.5.3 Autosampler for graphite tube technique (solid analysis)

The automatic sampler SSA 600 with and without liquid dosing and the manual
sampler SSA 6(z) are available for the solid analysis.
Sample transport In the window Method-Sample Supplyspecify the following parameters:
tab
• involvement of SS 600 or SSA 6 solid sampler
• operating mode – analytical sequence
• autosampler modifications

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Fig.12 Method– Sample transport window (solid analytics)
Autosampler
SSA6/SSAZ Use manual sampler SSA 6z.

manual mode On selection of the manual SSA 6 sampler, no further sample
transportation options need to be specified. All samples must
be individually weighed and their sample mass values entered
in the main window on the Solid tab.
SSA 600 Use automatic solid autosampler SSA 600.
SSA 600 with Use automatic solid autosampler SSA 600 with integrated dos-
automatic liquid ing automatics for liquid components (standards and/or modifi-
pipetter ers).
On selection of the manual SSA 6z sampler, no further sample transportation op-

tions need to be specified. All samples must be individually weighed and their
sample mass values entered in the result window on solid tab.
For working with the SSA 600 autosampler, you will specify the sequence of sam-
ple transportation in more detail in this window.
Mode One-platform mode Analysis relies on one single platform

which is refilled again and again.
This platform is located in tray position 1.
All required operations (gauging, dosing, weighing,
liquid dosing) are performed with this platform during
an analytical process.
Batch-Operation Analysis relies on several platforms.
Analysis may run automatically, depending on your
pre-settings.
Batch (special position 42) Analysis relies on several plat-
forms. Analysis may run automatically, depending on
your pre-settings. For samples requiring no weighing
operation, for example, "Kal.Null" or liquid standards,
position 42 on the sample tray will be used. For this
reason, an empty platform must be placed in this
position as pipetting destination of sample is neces-
sary.

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Number of platforms For Batch-Operation and Batch (spe-

cial position 42) 42)
Define the number of involved platforms and, hence,
the number of available sample positions.
Installation site Allows precision level settings for the integrated micro scales
depending on the degree of interfering factors (especially exci-
tation/vibration).
If the time of weighing appears too long, it can be reduced by
changing the setting for location site. This will be at the expense
of precision. Available setting options are:
• very disturbed
• disturbed
• quiet
• very quiet
Speed The speed of SSA600 motion can be set in three stages.

Recommended stage: 2
Sampler tray Number of trays placed one on top of the other.
Getting sample Weigh Once a dosed solid substance was weighed, the
weight weighed portion value will be adopted without a pre-
liminary query for acceptance of this weight.
Weigh with confirmation
Displays the result after each weighing.
By pressing the green key (key at autosampler or
[OK] in weighing window on the monitor screen), the
user may signal his/her acceptance of the weighed
portion result.
On actuation of the orange key (key at autosampler
or [Repeat] in the weighing window on the monitor
screen), the platform will return into dosing position,
dosing will be altered and weighing will sub sequent-
ly repeat.
No weighing
This weighing mode allows no measurement of con-
centration. It is only intended for qualitative analysis
of solid samples.

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4.1.6 Evaluation tab – Spectral range and background corrections

The line-specific evaluation parameters for the determination of the measured data
from the spectrum are to be defined in the Method - Evaluation window.
Evaluation tab tab
Fig. 13 Method – Evaluation window

Spectr.range Number of pixels for spectrum measurement (max. 200).
Only the specified number of pixels of the CCD line is read and
stored. This way, the computing time can be optimized in the
evaluation.
Eval. Pixels The number of pixels used to evaluate the absorbance signal,
from which finally the measured values are generated.
The absorbance values of the evaluation pixels are summed
up. This way, analysis inaccuracies can be eliminated, which
would be caused by a peak located between two pixels. There-
fore, theoretically an absorbance value of up to 9 A might ap-
pear as measurement result.
BGC mode with reference: Background correction (BGC) requires a refer-
ence spectrum in the sequence.
without reference: Background correction (BGC) does not
need a reference spectrum.
IBC: Iterative baseline correction. Background correction (BGC)
requires a reference spectrum in the sequence.
See also → "Working with Correction Spectra in ASpectCS
Software" pg. 180.

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Perm.Struct. Elimination of permanent structures.

This technique requires the measurement of a reference spec-
trum. Permanent structures are bands that may exist in refer-
ence and sample spectrum at different intensities, which how-
ever are not caused by the element to be analyzed. In the most
cases, these structures are caused by molecular vibrations,
e.g. from the nitrous oxide flame.
off: Spectra are not corrected for permanent structures.
on: Spectra are corrected for permanent structures.
BGC fit Fitting of pixels to background correction (→ "Description of the
algorithms used for spectral background correction", p. 177).
dynam.: The pixels for background correction are found auto-
matically by software.
static: The pixels for background correction are user-defined in
the BGC pixels column.
BGC pixels In this cell, enter the position of the pixels, if you activated the
static BGC fit option.
Type in the pixel numbers for the background correction. In the
status bar appears an example entry.
Button [Spectral corrections]

Opens the window Spectral corrections where existing correction models can be
selected or new models may be created (→ "Working with Correction Spectra in
ASpectCS Software“).
Note
In the display of the line spectra, the pixels can be selected based on the graphic
presentation for the background correction and transferred to the method.

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4.1.7 Calib. tab – Calibration parameters

In the Method – Calib. window, you can select the calibration parameters (stand-
ards and their preparation) and the blank correction.
Calib. tab
You may use a maximum of 65 standards in one calibration.
Fig.14 Method– Calib. window: Selection of calibration method and line-specific pa-
rameters
General calibration parameters

Selection of calibration method
No calibration The results of sample measurement are exclusively presented

in absorbance or emission.
Calibration is not necessary for these measurements.
Standard calibra- Calibration is performed with samples of known concentration.
tion The samples of unknown concentration are measured against
these calibration standards.
Method of addi- Not for solid analytics.
tions Different quantities of a known sample are to be added to the
unknown sample and the resulting substance measured. The
concentration of the unknown sample results from the per-
formed regression.
Method of addi- Not for solid analytics.
tions cal- The calibration curve, by means of which other concentrations
ib(ration) can be determined, is set up by the method of standard addi-
tion. At the same time, the concentration of the first sample is
found by this method.
Standard preparation
manually The standard solutions are already prepared.

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prep. by sampler Only if AS52s autosampler is included.

Standards are only prepared with the autosampler.
The standard solutions are prepared in the mixing cup of the
autosampler by mixing different portions of stock solution and
diluent.
In this case, under Volumes, adjust the following parameters
for preparing the standard solutions:
Amount The total fill volume in the mixing cup (adjusting
range: 1 - 20mL)
Sample fract. (Only with addition method): The proportionate
sample volume (increments of 0.5 mL).
With the addition method, the fraction of the sample solution of
a measurement series is always the same. The proportionate
sample solution must be smaller than the total fill volume. The
difference volume is filled up with stock solution and diluent
solution. The sample volume/total volume ratio is the correction
factor for the concentration to be computed.
by variation of Only for graphite tube technique.
volume Different volumes of stock solution or reference sample quanti-
ties are subjected to atomization in order to achieve a stepping
in concentration (referred to sample volume/sample weight).
by dilution Only for graphite tube technique.
Different volumes of stock solution and the amount of diluent
solution required for achieving full sample volume are placed
into the graphite tube in one transfer operation in order to
achieve a stepping in concentration (referred to the sample
volume).
Blank correction
This function is available only for the methods of standard addition and addition
calibration.
Absorbance cor- In every standard addition procedure, the blank is measured,

rected too, and its value subtracted from all measured values before
the regression line is calculated. This method was customary
for a long time; with many real samples however, it leads to
incorrect results.
Concentration First, a separate standard addition is carried out for the blank
corrected solution using the same concentration additions as for the
sample. The found concentration will then be subtracted auto-
matically from all other concentrations determined by standard
addition.
Element-line specific calibration parameters

Calibration function (only with Standard calibration)
linear Calibration points result in linear calibration curve.

The methods of standard addition and addition calibration are
approved only for linear calibration curves.
nonlinear Calibration points result in a non-linear calibration curve.

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automatically Both types of calibration curves are computed.

The sums of the squared residuals are compared with each
other (Mandel test). If the sum for the nonlinear function is sig-
nificantly lower than that for the linear function, the nonlinear
calibration curve will be selected. Otherwise, the linear calibra-
tion curve will be used.
Note
With the methods of standard addition and addition calibration, always the linear
calibration curve will be used.
Intercept
Set zero The calibration curve exactly intercepts the measured zero
point.
calculate The zero value is included in the calculation as any other cali-
bration point.
Weighting of calibration points
none All calibration points are taken into account with the same
weighting.
1/conc Calibration points obtained with lower concentrations are to be
weighted more strongly.
1/SD Points with lower deviations within several repeat measure-
ments of a standard are taken into account with a stronger
weighting (requires: activated Sigma statistics option).
1/(SD*conc) Combination of the calculation methods 1/conc and 1/SD.
Checking the calibration curve

ASpect CS provides automatic checking of determined calibration curves by
means of a prognosis range that is calculated based on a manually selected statis-
tical certainty.
none Uses all measured and non-deleted calibration points for the
calculation of the curves. Calibration points are neither labeled
nor eliminated.
Elim. outliers If calibration points are outside the calculated prognosis range,
outliers will be eliminated by means of an F-test (a test to ascer-
tain whether the exclusion of a point results in a significant im-
provement of the residual scattering):
• An F-test is performed for the calibration point being far-
thest outside the prognosis range.
If the exclusion of this point does not lead to a significant
improvement of the residual scattering, the point will be
included and the calibration point not further optimized.
• If the exclusion of this point results in a significant im-
provement, the calibration point will be defined as outlier
(marked in the table by "!", in the graph marked by red
color) and the calibration recalculated without this point.
• Then, another F-Test is performed for the calibration
point now being farthest outside the prognosis range.
This procedure is repeated until all outliers have been
eliminated.

Methods
• All calibration points lying outside the new prognosis

range, that have not been eliminated as outliers are
marked by "?" in the table and brown color in the graph.
Concentration unit
Enter the concentration units for the element to be analyzed in the Unit column.
Note
With the contrAA it is possible to choose several analysis lines of different sensitivi-
ties for one element and thus extend the working range. For every analysis line, a
separate calibration curve is determined. In the calibration table, the calibrations for
different lines of an element are distinguished by an index following the element
symbol. The index number corresponds to the sequence in the element table, e.g.
Cu1, Cu2.
4.1.7.1 Entry of concentrations for manually prepared standards
Calibration tabel for flame technique Caibration table für graphit furnace technique
Fig.15 Calibration table for standard methods with manually prepared standards
 Use [Concentration] on the Calib tab to open the Calibration table window.
 Define the number of standards in the various list fields above the table, as
required for your selected calibration method.
Maximum number of standards: 65.
Calibration Standard types

method
Standard Cali- Cal.-Zero.x (You may make several Cal. Zero entries, e.g.
bration if the elements to be analyzed are dissolved in
different solvents. In this case, the concentration
of the respective element line is to be set to "0",
the other columns remain blank.)
Cal.-Std.x
Standard Addi- Sample+Addx
tion:
Addition Cali- Sample+Addx
bration:

Methods
 Continue by making entries for the following table items:
Pos. When using an autosampler:

Position of the standard on the sample tray of the au-
tosampler.
Rec. Only with Standard Calibration:
Defines the corresponding standard as recalibration stand-
ard.
Element lines Concentration of the individual elements in the standard.
4.1.7.2 Entry of concentrations for standards prepared with autosampler

Automatic preparation of calibration standards is performed, using flame technique
and the AS 52s autosampler for mixing.
For graphite tube technique, a calibration series is accomplished by volume step-
ping or volume thinning inside the graphite tube.
For automatic preparation of calibration standards, the concentration settings for
stock standards must be specified at first. The concentration values of available
stock standards can be saved and retrieved, if necessary, from a data base.
Calbration table for flame technique Calibration tabel for graphite furnace technique
Fig. 16 Calibration table for standard procedures with automatically prepared stand-
ards
Entering stock standards

In the list of stock standards, several stocks with different elements and concentra-
tions may be specified.
 On the Calib. tab, click on [Stocks] to open the Stock Standards window.
 With [Append], add a new row to the stock list.
This will bring up the Insert Stock Standard dialog.
Maximum number of stock standards: 20
 To load stocks from a stock database, activate the From stock database op-
tion and choose the name of the stock from the list.
 Alternatively, you may activate the Enter manually option to enter the stock
data directly in the list:

Methods
Name Name of the standards.

Pos. Position of the standard on the autosampler.
Elements and Lists the elements and the corresponding concentrations of
concentrations the standards. With [Concentrations...], you can open a list
for the entry of the concentrations.
Alternatively, you may type in the values in the following
input format directly into the row: Element symbol-space-
concentration. For nickel e.g. with a concentration of 0.5
mg/L type in: Ni 0.5
Further elements and their concentrations are simply added
each separated by a semicolon. An example of the input
format is given under the stock list.
Unit Concentration unit of the elements contained in the stand-
ard.
After having defined the stock standard, fill in the calibration table.
Completing calibration table

 Use [Concentration] on the Method - Calib tab to open the Calibration table
window.
 Use the various list fields above the table to set the number of standards as
required for a selected calibration method.
Maximal number of standards: 65.
Calibration Standard types

method
Standard Cali- Cal.-Zero.x (You may make several Cal. Zero entries, e.g.
bration if the elements to be analyzed are dissolved in
different solvents. In this case, the concentration
of the respective element line is to be set to "0",
the other columns remain blank.)
Cal.-Std.x
With Standard Sample+Addx
Addition
Addition Calibra- Sample+Addx
tion
 Make further table entries as follows:
Pos. Position of the standard or zero value on the sample tray

of the autosampler.
Preparation % with APN 52s
Vol. % of the stock portion in the solution
Vol with MPE 60
Stock volume to be injected in µL.
Stock The number of the stock. It is automatically en-
tered according to the position on the au-
tosampler.
Rec. Only with Standard Calibration:
Defines the corresponding standard as recalibration
standard.
Element lines Display of element concentration in the standard according
to the above set volume percent.

Methods
Deactivating standards for selected lines

If you do not want to use standards for specific lines, deactivate them as follows:
 Keeping the Ctrl key depressed, click on the Line cell in the row specifying the
standard.
 Alternatively, you may click on the respective Line cell and then press the
space key.
The cell background turns gray.
 In the same way, you can reactivate the standards for the calibration of the
element.
The deactivation of standards gives you the possibility to have the calibration
standards automatically mixed also for the simultaneous analysis of several lines of
different sensitivities of one element.
4.1.8 Statistics tab – Defining statistical analysis

On the Statistics tab, choose the statistical methods to be applied to calibration
and sample measurements. The settings selected here are independent of the
Statistics tab chosen calibration method and remain set at every method change.
Fig .17 Method – Statistics window
Statistics type
Sigma statistics Calculates mean value and standard deviation.

Error statistics based on the arithmetic mean:
The sample is measured repeatedly after the blank cycles.
Based on the measurement results, the arithmetic mean, the
standard deviation and the relative standard deviation are calcu-
lated.

Methods
Median statis- Calculates median and range (R).

tics Error statistics according to the median method:
The sample is measured repeatedly after the blank cycles. The
measured values are sorted by size. The displayed median is:
· The value in the middle of the sorted list, if the number of meas-
urement cycles is odd.
· The mean value of the two measured values in the middle of the
sorted list.
As the smallest and largest individual measured values do not
influence the measurement result, the median statistics is suita-
ble for the elimination of outliers.
Number of replicate measurements
Samples Number of repeat measurements per sample

Calib. std. Number of repeat measurements per calibration standard
QC samples Number of repeat measurements per QC sample
Pre-runs Number of pseudo measurements.
Number of sample measurements preceding the statistics
measurement, but disregarded for the calculation of the meas-
urement result.
Grubbs outlier test

This function is provided for sigma statistics with at least three repeat measure-
ments per sample.
Deactivated Includes all values of the statistics series for the determination
of the mean value.
Activated Eliminates outliers by excluding them from the calculation of
statistical quantities. The thus found mean values in the result
table are marked by "!".
Confidence interval calculation

The calculation of the confidence interval is based on the chosen statistical certain-
ty (see below). In the calculation of the confidence interval, the errors in sample
measurement and particularly the calibration errors are included, so that a value
will be presented even if the statistics function has been deactivated.
off Confidence interval is not calculated.

absolute Displays the confidence level in absolute values (in concentra-
tion units)
relative Displays the confidence interval in relative values (in percent of
the concentration value)
Confidence level The confidence level (selectable between 68.3 ... 99.9%) is
used for the calculation of the confidence interval of the sam-
ples and the prognosis ranges of the calibration curves.

Methods
4.1.9 QCS tab – Quality Control Samples

Quality Control (QC) is of particular interest for serial measurements. You may
insert quality control measurements in the sample measurement process, which
shall deliver known results, i.e. either the absolute value (absorb-
ance/concentration) or the concentration difference relative to preceding sample is
known.
The results of the quality control measurements are automatically recorded on so-
called QC charts (also called quality rule charts or control charts).
QCS tab
You may define various quality control samples (QC samples). The concentration
and tolerance data for these samples are to be defined in the Method – QCS win-
dow.
Fig. 18 Method – QCS window
Elements of the QCS tab

Type QC sample the parameters of which (error limits and proce-
dure selected) are displayed in the list of lines.
You can select a QC sample from the list for viewing and
editing.
Name Name of the displayed QC sample
Reaction Procedure to be taken if the results of the QC sample exceed
the defined error limits.
[New/Modify…] To be activated for defining a new or modifying an existing
QC sample.
[Delete] Deletes the displayed QC sample.
Blank correction Not accessible for QC standard and QC blank
Takes blank correction into account, if activated.
Unit List box for selecting the corresponding concentration unit.
[QC samples Opens a list with the line-specific parameters of all QC sam-
overview] ples.
Table In the table, the parameters of the QC sample selected in the
Type list box are displayed.

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Entering parameters of QC samples

 To create a new parameter set for a QC sample or edit the currently displayed
one, click on [New/Modify...].
This will bring up the Add/modify QC sample type window.
 From the Type list, choose the sample type and, if you intend to define several
QC samples of the same type, assign a number (e.g. QC-Std.2). The following
sample types are selectable:
QC Sample Defines a sample as QC sample.

The concentrations of the QC sample may either be loaded
from the database or typed in directly.
To recall a stored data record for the QC sample from the
database, activate the from database option and choose
the corresponding QC sample from the opposite list box
(→ "Specifying stock standards and QC samples", p. 20).
Alternatively, you may type in the concentrations of the QC
sample directly in the table on the QCS tab. In this case,
activate the Enter manually option.
Max. number of QC samples: 50
QC Std. Defines a standard as QC sample.
You may use every standard as QC standard that has
been defined in the calibration table (Calib. tab). If the cal-
ibration standard was defined as being mixed by the au-
tosampler, the QC standard will be mixed by the au-
tosampler as well. The autosampler positions will be
adopted from the Calibration Table.
The assigned number at the same time defines the used
calibration standard. Example: QC-Std.2 – the second cal-
ibration standard is to be used as QC sample.
Possible number of QC standards = number of standards
in the calibration table (max. 65)
QC Blank Defines the blank as QC sample.
QC Stock Defines a stock sample as QC sample.
In recovery/addition, the measurement results of a defined
concentration addition to one or several samples are
checked. To this end, a QC stock sample is to be defined
after any sample in the sample table (QC-Stock sample =
sample + addition with a solution of known concentration).
After the measurement of sample and QC stock sample,
the concentration difference of both is compared with the
“Exp(ected) conc(entration growth)” and the recovery rate
calculated. When using the flame technique, the solution
with added stock solution must have been pre-mixed.
If no certified quality control samples are available, quality control may also be
carried out by means of double determinations:
QC-Trend The measured concentration value is stored when the

quality control sample appears for the first time in the ana-
lytical procedure. When the QC sample appears the next
time, the concentration difference is formed and evaluat-
ed. It is advisable to measure these QC samples at the
beginning and at the end of a sample measurement se-
ries.

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QC-Matrix A sample to be analyzed is split before preparing the

sample. Both portions are separately subjected to all steps
of sample preparation. They are placed separately on the
autosampler tray as QC Trend and QC Matrix. The differ-
ence between the determined concentrations is evaluated.
 From the Reaction list box, choose the further procedure to be run if the error
limit is exceeded:
With QC Sample, QC Std. and QC Stock selected as QC sample type:
flag The measured value is flagged in the sample table; the

measurement program continues measuring the next sam-
ple.
recal. + con- A recalibration is run. Afterwards, the QC sample is re-
tinue measured. If the QC sample is now within the permissible
range, the measurement is continued with the next sample;
otherwise, the measurement program will be stopped or con-
tinued with the next method.
cal. + continue A new calibration is run. Afterwards, the QC sample is re-
measured. If the QC sample is now within the permissible
range, the measurement is continued with the next sample;
otherwise, the measurement program will be stopped or con-
tinued with the next method.
recal. + rerun A recalibration is run. Afterwards, the QC sample is re-
measured. If the QC sample is outside the permissible range,
the measurement program will be stopped. If it is within the
range, all samples measured after the last QC sample or the
last (re)calibration, will be re-measured. If the QC sample is
again outside the permissible error limits, the measurement
program will be stopped or continued with the next method.
cal. + rerun A new calibration is run. Afterwards, the QC-sample is re-
measured. If the QC sample is outside the error limits, the
measurement program will be stopped or continued with the
next method. If it is within the range, all samples measured
after the last QC sample or the last (re)calibration, will be re-
measured. If the QC sample is again outside the permissible
error limits, the measurement program will be stopped or
continued with the next method.
next method The current measurement program will be stopped and the
measurement program of the next method started.
Stop The current measurement program will be stopped.
If you selected QC-Blank as QC sample type, you may only choose among the
flag, next method and Stop reaction options described above.
For the QC Trend and QC Matrix QC sample types, no reaction is provided.
 In the list of QC samples, define the line-specific parameters for every element
line dependent on the QC sample type selected:

Exp. conc. For QC Sample und QC Std.
Expected concentration in QC sample.

Methods
Exp. conc. in- For QC Stock.

crease Expected concentration increase from sample to sample +
addition.
Enter the value according to the added volume and the
concentration of the spiking solution.
Exp. absorb- For QC Blank.
ance Absorbance expected in QC Blank.
Low. range [%] Lower range of error limit in percent.
Up. range [%] Upper range of error limit in percent.
QC-Chart If marked by "+"sign, the result of the quality control for this
line will be presented on the QC chart of the result list.
React.! If the error range limits are exceeded, the procedure select-
ed from the Reaction list box shall be applied.
If several lines have been marked by "+", it will do that the
error limits are exceeded for one of these lines to start the
selected reaction (OR logic).
Unit Unit of the expected concentration (only with selected QC
Std. option)

Methods
4.1.10 QCC tab – Quality control during the analytical process

On the QCC tab of the Method window, you can define the parameters for the
quality control:
• Relative standard deviation (sigma statistics) or relative range (median sta-
tistics),
QCC tab
• Calibration check
• Recalibration check
• Procedure to be run if error limits are exceeded
You may choose various control options with different reactions simultaneously.
Fig. 19 Method–QCC window
Types of quality checks
RSD/RR% check Check of relative standard deviation or relative range (→

"Statistics tab – Defining statistical analysis", p. 48)
Calib. check Check of calibration
Recal. check Check of recalibration factor
Reactions if error limits are exceeded
none The corresponding check is not performed.

flag Marks the corresponding sample, calibration or recalibration in
the sample table, if the error limits are exceeded.
repeat + contin- Accessible only for RSD/RR% check option.
ue Repeats the measurement of the respective sample, if the serial
precision limit was exceeded, before the next sample is meas-
ured.
cal. + continue Accessible only for Calib. check and Recal. Check options.
Runs a new calibration if the error limits for the calibration or the
recalibration factor were exceeded. Afterwards, measurement is
continued with the next sample.

Methods
next method Accessible only for Kalib. check and Recal. check options.
Stops the measurement of the currently running method and
starts the next method, if the error limits were exceeded.
Stop Accessible only for Calib. check and Recal. check options.
Stops the measurement of the currently running method, if the
error limits were exceeded..
Tube control
Only for graphite tube technique.
Specifies settings for graphite tube monitoring.
Max. heating Enter maximum number of measurements to be performed with

cycles the tube.
Enter current graphite tube utilization value in adjacent field.
Reaction Select reaction type on reaching of maximum number of meas-
urements:
no react. Graphite tube utilization is not monitored.
flag Marks current measurement in sample table when
limit value is exceeded.
Stop Stops analytical procedure on excession of limit
value.
Line-specific parameters of quality checks

In the table, enter the line-specific parameters of the various quality checks. You
may define for every analysis line, whether it shall be considered for the check. If
one or several of the checked lines exceed the error limit, the reaction chosen
above will be released.
Quality Parameter Meaning

check
RSD/RR% RSD/RR%< The system will respond as selected if the relative
check standard deviations or the relative ranges are larger
than or equal to the specified value.
RSD! If the lines are marked by "+", the RSD% or
RR% will be checked.
Calib. R2(adj.)> The coefficient of determination R2(adj.) must be larger
check than or equal to the specified value. Otherwise, the sys-
tem will respond as selected.
R2! If the lines are marked by "+", R2(adjust) will
be checked.
Recal. Rec.Fact> Upper limit of recalibration factor.
check Rec.Fact< Lower limit of recalibration factor.
The selected response will be released, if the calibration
factors are outside these specified limits.
Rec.! If the lines are marked by "+", the recalibra-
tion factor will be checked.

Methods
4.1.11 Output tab – screen view, printout and saving options

On the Output tab, you can choose the scope of result saving, the number of dec-
imal places with which results are presented on the screen and on the printouts,
Output tab and the order of lines on the printout.
Fig.20 Method – Output window
 By activating the Method and/or Spectra option, the corresponding data will
be saved additionally together with the analysis results.
 In the table below, define the number of decimal places for the display and
printout of absorbance and concentration values, and the order in which the
analysis lines shall appear on the printout.
For the development of analysis methods, it is advisable to save the spectra as
well. You will get important information from them, e.g. on potential matrix or inter-
ference problems. Recalculation with modified method parameters without saved
spectra will be possible only based on the calculated absorbance values. So, for
instance, it is not possible anymore to change the data points for background cor-
rection, because the spectral information on the individual pixels is missing.
For a proven routine method, however, saving of spectra will not be necessary.
Note
If in the Options – Analysis sequence window, you activated the Always save
spectra option, the spectra will always be saved independent of the settings in the
method parameters (→ "Options for analysis sequence", p. 17).

Methods
4.2 Saving and opening methods

Methods are managed in the database window (→ "The database window", p.
157).
Saving methods
The command for saving the current method parameters can be given in different
ways.
 In the Method window, click on the [Save] button.
 Alternatively, you may activate menu command File / Save / Method....
File / Save /
Method This will bring up the Save method window.
 In the Name textbox, type the desired method name.
 In the Cat (category) textbox, you may optionally enter an additional identifier
of maximally three characters to facilitate later method search in the database.
 In the Description textbox, you can optionally enter information on the meth-
od.
 Activate the option Save calibration data, if you want to save the calibration
data with the method.
 Save the method with [OK].
On doing so, the method will be saved to the database. If you choose an existing
method name, the existing method will not be overwritten, but a new version
created in the database. To remove methods from the database, you must explic-
itly delete them!
Note
The method may also be saved to the results file of the measurement.
To save the method along with the results file, you must have activated the Save
with results - Method option in the Method - Output window. After having opened
the results file, you may also reload the method.
Opening methods
File /  Activate menu command File / Open method... or, on the toolbar, click on the
Open method folder symbol right of the Method field.
 Alternatively, you may click on the [Open] button in the Method window.
This will bring up the Load method window.
 Choose the desired method from the list.
 By the entry in the Cat textbox, you can define that only methods of the speci-
fied category are displayed.
If you want to see methods of all categories, delete the entry in the Cat field.
 Activate the Current version only check box, if with methods of the same
name you want to see the method of the highest version number only.
 Open the selected method with [OK].

Sequences
5 Sequences
A sequence is based on a loaded method, which contains the information on the
type of calibration, statistical analyses, quality control, etc.
The sequence contains the information on the samples and actions in their order of
processing. Some sample describing data such as sample name and position on
the sample tray may also be entered directly. For permanent storage, however, the
sample describing data must be saved as sample information file.
5.1 Creating a sequence

 To create a new sequence, activate menu command File / New Sequence...
to open the Sequence window.
 Alternatively, you may open the window with the currently active sequence
parameters by using menu command Method Development / Sequence... or
File / New Se- by a click on the following icon:
quence...
.
Method Develop-
ment / Sequence... The meaning of buttons and symbols contained in the Sequence window, which
are also used in other windows of this application, are described in Section
"Frequently used control elements" p. 8
5.1.1 Specific dialog functions in Sequence window
Fig. 21 Sequence window

Sequences
List of sequence of samples and actions

Type Sample type or analysis step.
Pos. Sample position on autosampler tray (if used).
Name Sample name
Entry in this cell is optional. For calibration samples and QC
samples, the name is adopted from the method, if a sample
name has been specified there.
For samples to be analyzed, the names can be transferred
from the sample information file.
Name(2) Additional designation for sample identification (optional).
Elements Elements / element lines to be analyzed from this sample.
Input format: see the tip under the corresponding column:
"all" All elements/element lines defined in the method
will be determined (default).
Element symbol
Only the specified elements will be determined, e.g.
Cu,Pb.
Element symbol + Index (for the analysis of several lines of
an element)
Only the specified element lines will be determined,
e.g. Cu1,Cu2.
"not" element symbol
The specified elements will not be determined, e.g.
not Cu,Pb.
"not" element symbol + Index
The specified element lines will not be determined,
e.g.. not Cu1,Pb2.
Specifics This field is not used so far.
Buttons
[New] Adds a new row to the end of the list and opens the Edit Se-
quence window.
[Insert] Inserts a new row at the selected place of the list.
[Delete] Deletes the selected row.
[Delete Table] Deletes the complete sequence table.
[Samples] Opens the window Sample ID.
[Sequ.<-QC- Transfers QC sample information (e.g. names and sampler
samples] positions) to window Sample ID (→ "Create information data for
samples and QC samples" p. 63).
The information from the QC sample ID table are entered in
the sequence table. The first row with the new sample ID is to
be defined in the From row textbox.
[Sequence<- Transfers information on sample name and place on the tray of
Sample] the autosampler from the Sample ID window (→ "Create infor-
mation data for samples and QC samples" p. 63).
The information from the Sample ID table is entered in the se-
quence table. The first row with the new sample ID is to be de-
fined in the From row textbox.

Sequences
5.1.2 Specifying sequences of samples and actions
Fig.22 Edit sequence window
 In Sequence window click on [New] to open the Edit sequence window.

 Successively choose the sample types and actions and transfer them to the
sequence list by a click on [Accept]:
Sample/Action Description
Samples Measures the number of samples specified under Number.
QC samples Measures a QC sample and evaluates it as specified in the
Method.
From the appearing list box, choose one of the QC sample
types specified in the Method – QCS window. The parame-
ters of the QC sample are displayed in the opposite field.
Reference Measures a reference.
Reag. Blank Measures a blank.
QC Blank DL Measures a blank for the determination of the detection and
determination limits according to the blank method.
Calibration Measures the calibration samples and runs the calibration
according to the options defined in the method.
Recalibration Measures the calibration sample provided for recalibration
and performs the recalibration.
Special action Actions which do not directly involve the measurement of
samples. These actions can occur for each line, only for
the first line or only for the last line in the method as pre-
ferred. For list of possible special actions see below.
Load method Loads a saved method, e.g. to start another element analysis
within the sequence.
Click on [...] to open the Open method window (→ "Saving
and opening methods", p. 57). Choose one of the stored
methods.
The following special actions can also be inserted in the measurement pro-
cess:

Sequences
Lamp off Switches the xenon lamp off.

Pause Stops the analysis. Afterwards, the sequence can be con-
tinued with menu command Routine / Continue… or the
button.
Standby Switches the xenon lamp into standby mode.
Idle time Waits for the time entered in the appearing textbox (min)
before continuing with the analysis.
Show cal. plots Shows the calibration curve during the running sequence.
Dark current Repeats the dark current measurement.
measurement
Clean furnace (for contrAA 600 /contrAA 700 with graphite tube tech-
nique)
Triggers extra bake-out (cleaning) sequence to decontami-
nate the graphite tube. The graphite tube is heated to a pre-
defined temperature once. Parameter settings for this bake-
out sequence can be made in the Method - Furnace win-
dow (→"Furnace tab – Parameters for graphite tube fur-
nace" p. 26).
Format tube (for contrAA 600 /contrAA 700 with graphite tube tech-
nique)
Formats the graphite tube.
Flame on/off (only flame technique)
Extinguishes/ignites the flame.
Beep Lets the PC generate a beep tone, e.g. to indicate the end
of the calibration procedure. (Requires installation of a
sound card and loudspeakers.)
Cleaning Performs controlled cleaning. (→ "Auto sampler for flame
and Hydride/HydrEA technique" p. 32 and "Autosampler for
graphite tube technique (solution analytics)" p. 35)
Clean system (only hydride technique)
Additional system cleaning. The parameters for this cleaning
step are defined in window Method/-Hydride (→ "Hydride
tab – Specifying the hydride system" p. 27).
Load system (only hydride technique)
After first installing the hydrid system or system cleaning
which should be performed daily at the end of the work the
hydride system tubing has to be loaded with reagents. For
this reason this action should be defined in the sequence
prior to the first measurement.
 After you have chosen all elements of the sequence, click on [OK] to return to
the Sequence window.
 In the list, enter the Elements to be analyzed.
 When using the autosampler:
Define the position of the samples on the autosampler. The positions of cali-
bration and QC samples are automatically transferred from the method. How-
ever, you may change the positions here.

Sequences
Note
It is advisable to enter the data of the samples to be analyzed in the Sample ID
window and transfer them afterwards to the sequence list (→ "Create information
data for samples and QC samples" p. 63).
5.2 Saving and opening sequences

Like methods, sequences are saved to a common database. When you save and
open sequences, the database window is opened (→ "The database window", p.
157).
Saving sequences
 In the Sequence window, click on [Save].
 Alternatively, you may activate menu command File / Save / Sequence.
File / Save / Se-
quence This will bring up the Save Sequence window.
 In the Name textbox, type the desired sequence name.
As default, "Sequence" and the current date are offered, e.g. "Sequence-08-
15-05".
 In the Cat (category) textbox, you may optionally enter an additional identifier
of maximally three characters to facilitate later sequence search in the data-
base.
 In the Description textbox, you can optionally enter information on the se-
quence.
 Save the sequence with [OK].
On doing so, the sequence will be saved to the database. If you choose an exist-
ing sequence name, the existing method will not be overwritten, but a new
version created in the database. To remove sequences from the database, you
must explicitly delete them!
Opening sequences
File / Open Se-  In the Sequence window, click on [Open].
quence ....
 Alternatively, you may activate menu command File / Open Sequence .... or,
on the toolbar, click on the folder symbol right of the Sequence field.
This will bring up the Open Sequence window.
 Choose the desired sequence from the list.
 By the entry in the Cat textbox, you can define that only sequences of the
specified category are displayed.
If you want to see sequences of all categories, delete the entry in the Cat field.
 Activate the Current version only check box, if with sequences of the same
name you want to see the sequence of the highest version number only.
 Open the selected sequence with [OK].

Sample information files
6 Sample information files

6.1 Create information data for samples and QC samples
 Open the Sample ID window by a click on the following symbol:
Method Develop- .
ment / Sample  Alternatively, you may open the Sample ID window using the menu commands
ID... Method Development / Sample ID... or File / New Sample Information File.
File / New Sample The meaning of buttons and symbols contained in the Sample ID window, which
Information File are also used in other windows of this application, are described in Section
"Frequently used control elements" p. 8.
6.1.1 Elements in Sample ID window
Fig. 23 Sample information – Sample ID window
The program pops up brief information (tool tips) on the table while you move the
mouse pointer across the button.
Sample information
Pos. Position of sample on autosampler
Name Sample name
The entry is optional.
Maximum number of characters: 20
Pre-DF Pre-dilution factor. Factor by which the original sample was
diluted before being placed on the autosampler or supplied to
the spectrometer, if no autosampler is used. The entry of the
factor is required for the calculation of the concentration of the
original sample (Conc.2 in the result table).

Unit Concentration unit of sample.

Wt. [g] Only for solution analytics.
Weighed portion in grams.
The weight of the original sample, which was dissolved in
sample preparation (in mL). The entry of the weight is required
for the calculation of the concentration of the original sample
(Conc.2 in the result table).
Note: For solid analytics, known weighed sample portions must
be specified in the Result window on Solid chard (→ "Specifics
for solid sample analysis with SSA 600" p. 70).
Vol. [mL] Volume of solvent used to dilute the weighed sample portion
(in mL). The entry of this value is required for the calculation of
the concentration of the original sample (Conc.2 in the result
table).
Name(2) Additional sample name.
AS-DF Dilution factor of autosampler.
Blank corr. Blank correction.
off No blank correction performed.
on For the calculation of the concentration of the origi-
nal sample, the blank measured last in the se-
quence will be subtracted.
Hum [%] Only for solid analytics.
Relative moisture of a sample
Note:
This specification is required to calculate the original sample
concentration (Conc.2).
Factor This field is not used so far.
Note!
For solid analytics, known weighed sample portions must be specified in the Re-
sult – Solid window (→ "Specifics for solid sample analysis with SSA 600" p. 70).
QC sample information
This tab contains the QC sample information.
The columns correspond to the columns of the tab Sample information. Addition-
ally information about the QC type is contained in column Type. The columns Unit
is omitted because QC sample units are defined in the method. Blank correction is
not available for QC samples.
Buttons
[New] Adds the number of rows specified in the # textbox to the end
of the list.
[Insert] Inserts the number of rows specified in the # textbox at the
selected place of the list.
[Delete] Deletes the number of rows specified in the # textbox from the
selected row of the list on.
# Input field for the entry of the number of rows to be added,
inserted, or deleted.

[Delete Table] Deletes the complete table of sample information.

[Samples -> Se- Transfers sample names and positions on autosampler to the
quence] sequence list. In the From row input field, define the first row
From row to be transferred.
[QC samples -> Transfers QC sample names and positions on autosampler to
Sequence] the sequence list. In the From row input field, define the first
From row row to be transferred.
6.1.2 Editing sample ID

 In the # field, enter the number of samples to be analyzed. Then, click on
[New] to add the corresponding number of rows to the list.
Sample infor-  In the table, enter the required information for every sample.
mation
 If the entries to be made in a column are identical, you may copy the entry of
the selected cell to all following cells of the column by click on .
If you activate the inc. check box, the value to be copied will be incremented
by one each in copying it to the next cell. In this way, you can easily assign
successive places on the tray of the autosampler.
 Texts in input fields can be copied to the Windows clipboard and pasted from
there by using menu commands Edit / Copy and Edit /Paste or shortcut keys
[Ctrl+C] and [Ctrl+V].
 When you entered all information required, specify in the From row field from
which row on you want to transfer sample information to the sequence. Then,
transfer the data by a click on [Samples->Sequence].
6.1.3 Edit QC sample IDs

Information for following QC sample types can be defined:
• QC spike
QC Sample infor-
mation • QC trend
• QC matrix
• up to 20 QC samples
 Enter the necessary data in analogy to the sample ID information (→ "Editing
sample ID" p. 65).
6.2 Saving, opening and importing sample information

Saving sample information
Sample information is saved in CSV format which can be edited with spreadsheet
software, e.g. MS Excel.
There are different ways to give the command for saving the current sample infor-
mation.

 In the Sample ID window, click on [Save].

 Alternatively, you may activate menu command File / Save / Sample Infor-
File / Save / Sam- mation....
ple Information...
This will bring up the standard Save as... dialog.
 In the File name field, enter the desired name for the sample information file.
 Save it by a click on [OK].
Opening a sample information file

 In the Sample ID window, click on [Open].
 Alternatively, you may activate menu command File / Open Sample Infor-
File / Open Sam- mation File....
ple Information
File... This will bring up the standard Open window.
 Choose the desired file from the list and open it with [OK].
Importing sample information from CSV-format

Sample information files are saved in CSV format which can be read by MS Excel
and other spreadsheet software. The other way round, however, it is also possible
to load an Excel table as sample information file. If you want to use an Excel table
as source of sample information, you may also load them in Aspect CS using menu
command File / Open Sample Information File....
The successive individual variables are separated by ";".
Type (Max. number of characters)

Pos. Integer
Name string (20)
Pre-DF Floating-point number
Unit string (10)
Wt.[g] string (12)
Vol.[mL] Floating-point number
Name(2) string (20)
AS-DF Floating-point number
Blank corr. 0=off; 1=on
Factor Floating-point number
To get an example of the input format, it is advisable to save a sample information
file and inform yourself of the used format.

Starting an analysis / Calculating results
7 Starting an analysis / Calculating results

Measurements are started via the toolbar buttons or the Routine menu.
Symbol Menu command Function

Routine / Start Starts an analysis process.
Sequence...
Routine / Run Repeats the selected rows in the sequence. Several
selected Se- rows can be marked using the mouse in combination
quence Row... with the Ctrl- and/or Shift-Key.
Routine / Stop Instantly stops the analysis process.
(rot) The stop function should be used only in the flame
technique. In hydride technique, sample residues may
be left in the system and lead to contamination, if the
analysis process is stopped that way.
Routine / Break For graphit furnace technique, HydrEA and hydride
(gelb) technique.
During the execution of a hydride procedure, a pro-
gram break can be requested with this button. When
the break request has been detected, the button is
grayed out. The procedure will be executed to the end.
Then, the analysis process will be stopped.
Routine / Con- Continues a stopped routine.
tinue...
Routine / Extin- Extinguishes the flame.
guish flame
Routine / Wash For flame technique.
The sampler tube is immersed in the wash cup for rins-
ing. If the Injection Switch has been selected as ac-
cessory unit, the switch will open. This is to ensure that
the sample path is rinsed, too. The rinse pump is con-
tinuously delivering fresh wash solution.
For hydride technique.
Rinses the hydride system with acid (also with reduct-
ant, if necessary).
The corresponding parameters are to be set in the
Method - Hydride window (→"Hydride tab – Specify-
ing the hydride system", p. 27).
Routine / Re- Causes the recalculation of the results, if the original
process data, e.g. the calibration function or the method, have
changed.
7.1 Starting the analysis process

After you have selected the method, the sequence and possibly the sample infor-
mation data, the system has all information necessary to start the analysis process.
The contrAA must have been prepared for the technique to be applied:
• Flame technique: The flame has been ignited and burning longer than the
specified warm-up time.
• Graphite furnace technique: The furnace is prepared.

• Hydride technique: The cell is pre-heated.

• Autosampler: Sample have been prepared and placed onto the tray.
• The xenon lamp is switched on.
Saving analysis results during the analysis process

The results of the analysis are saved to a database in the default folder or a user-
defined subfolder directly during the measurement. They may be saved optionally
to a new database or added to an existing database. However, it is not possible to
overwrite a result database by selection of the same name.
The target for result storage will be requested automatically at the start of a meas-
urement routine. The appearing window Start Sequence provides the following
options for results file storage:
Name Here, enter the desired name for the result database.
New file/list With this option activated, you must enter a
new file name. The program will check if the file
name already exists. Existing files cannot be over-
written.
Append to file/list New results will be appended to an
existing results file. Click on [...] to open a selection
window where you can choose an existing results
file from the displayed list.
Folder Choose the save path for the results file. The default folder for
saving of results is shown in the Options – Folder window
(click on ).
Description Here, you may enter an additional comment that is saved along
with the analysis results.
Switch off lamp When the measurement is stopped because of an error the Xe
after error stop lamp is automatically switched off..
[OK] Starts the measurement.
The file contains the results of measurement and evaluation and the sample ID
information. If selected accordingly in the method settings, method and spectrum
data are saved simultaneously with the results. In this case, method parameters
are saved to the result database, while spectra are saved to a separate file of the
same file name, but a different extension in order to save storage capacity.
The result database is saved with the extension ".tps". Spectrum files get the ex-
tension ".SPK".
Starting measurements
 Start the measurement routine using menu command Routine / Start Se-
quence or click on .
 In the Start Sequence window, choose a file name for the results file.
You may optionally save the results to a new file or append it to an existing file.
Routine / Start Overwriting of an existing file is not possible.
Sequence
After you selected the file name, the measurement routine will start according to
the settings selected in the method and the sequence.
 If you use an autosampler, the measurement runs automatically.
In the case of manual sample feed without autosampler, follow the prompts for
the provision of samples displayed on the screen.

Displays during the analysis process

While the measurement is running, the results are displayed in real time in the pro-
cess and result window.
Additionally, the following windows may be displayed on the screen: Signal plot,
Flame report (for flame technique), Furnace report (for graphit furnace technique)
and Sample conc. in calibration curve. The display of these windows is to be
selected in the Options – Analysis sequence window (→ "Options for analysis
sequence", p. 17). You may also optionally hide these windows during the meas-
urement.
View / Open Dis-  To open the display windows, use menu command View / Open Display Win-
play Windows dows or function key F7.
…/ Close Display  To close the display windows, use menu command View / Close Display
Windows Windows or function key F8.
Window / Cascade Using the standard Windows menu commands Window / Cascade, Window / Tile
horizontal and Window / Tile vertical you may arrange the windows on the
…/ Tile horizontal
screen as desired.
…/ Tile vertical
In the sequence list of the result window, the measurement progress is logged. The
rows with the successive actions are marked by the following symbols in the table
column:
- Not measured/executed yet.

Ο Just being measured.
+ Already measured/executed.
Additionally, in the symbol bar at the side up to three large buttons are displayed
during measurements:
[Activate Scrap- The scraper cleans the burner head between two measure-
er] ments within a statistics series of a sample.
[Method (read Turns the method window on. A method can only be read, it
only)] cannot be changed.
[Sequence Turns the sequence window on. A sequence may be expanded
Samples] while measurement is going on. The sequence window includes
a [Sample ID] control button that allows you to edit further
sample ID data.
[Stop Sequence] Instantly stops the analysis process.
[Display win- Opens (if closed) or closes (if open) the report and graphic win-
dows] dows during the measurement.
7.2 Interrupting, stopping, continuing the analysis process

Analysis processes can be interrupted and continued later. However, when using
the hydride technique the currently running sample measurement should be fin-
ished first and only the analysis process stopped. This procedure is to prevent
sample residues from being deposited in the system. In flame analyses, you may
stop the process at any time.

Routine / Stop
 With menu command Routine / Stop or button (red button), you can stop
… / Break the analysis process instantly (recommended for flame analyses or as emer-
… / Continue gency stop in hydride analyses).
 With menu command Routine / Break or button (yellow button), you can
request for an interruption of the analysis process. After this request was de-
tected, the button is grayed out. The currently running hydride measurement
will be finished first. Then, a stop of the analysis process is released (recom-
mende for graphite furnace technique and hydride technique).
 With menu command Routine /... or the button, you can continue a
stopped/interrupted routine.
This will bring up the Continue Sequence dialog, in which you are informed of
the status of actions before the interruption.
If you want to modify the method before continuing, activate the Continue with
modified method check box. On doing so, a new method entry is made to the
results file.
The measurement may be continued in one of the following ways:
Continue Repeat current sample, current line and current statistical

run.
First statistical Continue with current sample, current line and the first
run statistical run.
First element Continue with current sample, first line and first statistical
run.
From table row Continue with the table row displayed in the text box.
7.3 Repeating an individual measurement

The software lets you repeat individual actions within a sequence.
 In the result window on the Sequence/Result or the Sequence tab, select the
row with the action to be repeated.
 Start the measurement routine with menu command Routine / Run Selected
Sequence Row... or a click on
Routine / Run
Selected Se- .
quence Row...  In the Start Sequence window, choose a file to which the result of the repeat-
ed measurement shall be saved.
You may optionally save the result to a new file or append it to an existing file.
Overwriting of existing results by selection of the same file name is not possi-
ble.
After you selected the file, the selected action will be repeated.
7.4 Specifics for solid sample analysis with SSA 600

For solid sample analysis performed with an SSA 600 autosampler, more action
items can be specified in addition to sample and action sequences typical in solu-
tion analytics:
• Dose sample (place sample onto sample platform)

• Determine deadweight (tare) of platform

• Weigh sample
These actions may be performed partially or fully during an analytical procedure.
They require one person to replace the samples while analysis is underway.
If these actions are defined to precede an analysis, the given sequence will be au-
tomatically performed without any interruption. When using an SSA 600 with liquid
dosing unit the sampler automatically pipettes modifiers and standards.
The actions for solid sample analysis are specified in the results window, tab Solid.
The sample and standard measurements defined in the sequence are splitted into
single measurements and the samples are assigned to the platforms.
Fig. 24 Result window – solid tab
Dialog functions in the results window / solid

Table elements
Nr. Number of single measurement.

Seq. Number in sequence.
Pos. Designates the positions of sample platform on the SSA 600
tray. Positions range from 1 to 42 in single-tray mode and from
1 to 84 in double-tray mode.
Note: Positions are assigned by the ASpect CS software! Sam-
ples must be distributed according to predefined positions.
Type Type of the sample which needs to be placed, or has already
been placed onto this platform.
Name Name of sample
Line Analytical line
# Weight of sample after weighing
If this column contains a "--------" entry, the sample only consists
of liquid portions (liquid standard) and need not be weighed for
this purpose.

Weight (mg) Weight of sample

Note: This window is for defining or entering the weighed por-
tion of solid samples. Entries from the Sample-ID window will
be disregarded!
Tare (mg) Deadweight of empty platform
For samples not subject to weighing, this element will also con-
tain a "--------" entry.
Dos. Sample was dosed onto the platform, unless there is a "*"
marker.
STd./Mod. If marked with "*", this element indicates that liquid components
(standards or modifiers) are dosed onto the platform.
If known, the following settings can be directly entered at the sample table:
• Weighed portion if sample preparation occurred on external scales
• Deadweight (tare)
• Marking for completely dosed sample platform
Preparing samples
[Tare] Determines the weight of an empty platform for marked tray

positions.
This is accomplished by transferring the respective position
contents onto the scales and returning them onto their positions
after weighing. The resulting deadweight value will be entered
at the Tare column.
[Dosing] Transfers the platforms of marked positions successively into
dosing position.
A dialog window appears with details regarding the sample that
needs to be dosed. Depending on what options were selected,
more preparations can be made before or after this sample for
marked positions. If a table already contains entries, related
preparations will be skipped. Compliance with this order: Tare -
Dosing - Weighing - (Dosing) - (Weighing) - Mod./Std Pipetting
is compulsory.
with tare Weight of empty platform is determined in advance
with weighing Dosed sample is weighed after dosing
with Mod./Std. pipetting Platform is transferred to liquid
dosing after weighing.
If option Weigh with confirmation (→ "Autosampler for graph-
ite tube technique (solid analysis)" p. 37) was configured in the
autosampler window, "Dosing" and "Weigh" may be repeated
for any number of times.
If all three options were set, this sequence may be used to run a
complete sample preparation procedure. On completion of this
sequence, the tray will contain filled platforms that are com-
pletely prepared for analysis. If one of the preparatory steps
was not carried out, this step will be requested as part of the
analytical procedure.
[Weigh] Weigh loaded platform
[Load / Save] Save and reload weighing and dosing data of selected table
rows. The sample table (tab Solid) is automatically recreated
when modifying a sequence or method. The existing entries will
be lost. Using the function [Load/Save] these data can be
saved and restored.

[Std./Mod.] Successively transfers the platforms of marked positions into

the position for dosing of liquid analytical constituents (liquid
standards, modifiers).
Displays a dosing screen for liquid dosing. This screen shows
the liquids to be dosed and the volumes to be dosed.
[Burn out] Performs burning out for platforms of marked positions.
Places the platforms into the furnace, triggers and runs burn-out
program and returns the platforms to the tray as soon as the
furnace has cooled down. If option with tare was marked, the
empty platforms will be weighed after burning out and their
weights added in the tare column.
Re-analyze sample / modify weight entries
[Measure row(s)] Re-analyze an element in the sample (→ "Re-analyze

samples for solid analysis" p. 74).
[Prepare re- Re-analyze individual samples (→"Re-analyze samples
measurement] for solid analysis" p. 74).
[Re-measure
single val.]
[Delete entries] For selected table rows all entries in columns starting with
column Wt. [mg] are deleted.
7.4.1 Preparing samples for automated analysis

For automated analysis without user intervention, a sample platform with a sample
is required for each individual measurement:
Total number of sample platforms = number of analytical samples x number of ana-
lytical lines x number of sample measurements in a statistical series
The column Pos. shows the assignment of the samples to the sampler trays. The
assignment is determined by the software and cannot be changed.
 Select the table rows for which samples will be prepared in tab Solid. Hold
shift or ctrl to make multiple selections.
 Click [Tare], [Std./Mod.], [Dosing] or [Burn out] control button as appropriate
to trigger required sample preparation actions (→ "Specifics for solid sample
analysis with SSA 600" p. 70).
 Once all samples are prepared, you can trigger sequential measurement.
Action omitted or uncompleted during sample preparation, must be performed as
part of analysis. Special advisory windows will appear prompting you to perform
relevant action, for example, to dose a given sample. The analytical procedure will
stop for this time.
If the number of samples exceeds the number of platforms defined in the method
then the platforms are re-used after analysis.
When using an SSA 600 with liquid dosing unit the pipetting of modifiers and
standards is automatically performed during the sequence. Up to four standards
and three modifiers can be placed on the SSA 600. If more standards or modifiers
are needed these may be pipetted manually.

Save data of previously prepared samples

When the sequence or method is modified the sample table on tab Solid is rebuild
and the samples are reassigned to the platforms. In order to prevent loss of exist-
ing weight data these data can be saved. Two contiguous blocks can be stored.
 Mark the table rows with prepared samples. The data has to be in one contigu-
ous block.
 Use button [Load/Save] for opening the window Load/Save SSA600 table.
 Select one of the two Save buttons.
 Select [Save selected entries] and confirm the message box with [OK].
 Quit window Load/Save SSA600 table with [OK].
 Reopen the window Load/Save SSA600 table after the sample table in win-
dow Solid has been rebuild.
 Select Save.
 Enter the row number of the sample table where the data block will be inserted.
 Select [Load starting from row] and confirm with [OK].
 Quit window Load/Save SSA600 table by using [OK].
The data block is inserted into the sample table starting with the defined table
row.
 If applicable, adapt the positions of platforms on the sample tray.
7.4.2 Re-analyze samples for solid analysis

Individual samples as well as individual elements can be re-analyzed when using
solid analysis technique.
Re-analyze a sample
 Select tab Results.
 Double-click on the sample. The window Single values (→ "Sample details
and spectra" p. 82) is opened.
 Select the sample in the table.
 Select [Mark for re-measurement].
 Close window Single values.
 Repeat the procedure for all samples which shall be re-analyzed.
 Go back to tab Solid.
 Select [Prepare re-measurement].
For all marked samples additional entries for re-analysis are added to the
sample table.
 Prepare the samples for analysis according to the platform assignment.
 Start the measurement with [Re-measure single val.].
The recalculated results for the re-analyzed samples are added to the results
table in window Solid.
Re-analyze an element in a sample

 Mark all measurement of the sample element in the sample table (tab Solid).

 Select [Measure row(s)].

 Enter a new results file name in window Start Sequence or append the data
to the existing file.
 Start the measurement by using the [OK] button.
7.5 Rinsing the system

Rinse steps for the various systems are started with menu command Routine /
Wash.
Routine / Wash In addition, rinse commands are accessible in the respective technique-specific
windows such as for autosampler and hydride system.
Flame technique
The sampler tube is immersed in the wash cup for rinsing. If the Injection Switch
has been selected as accessory unit, the switch will open. This is to ensure that the
sample path is rinsed, too. The rinse pump is continuously delivering fresh wash
solution.
Hydride technique / HydrEA technique

The hydride system is rinsed with acid (or reductant, if necessary). The rinse pa-
rameters for the hydride system are to be selected in the method (→ "Hydride tab –
Specifying the hydride system", p. 27).
7.6 Reprocessing analysis results

After any change of evaluation conditions, such as a change of the calibration func-
tion, method, etc., the results must be recalculated to take these changes into ac-
count.
Likewise, it is possible to change sample information data, such as sample names
and dilution factors, and have them taken into account for the presentation of anal-
ysis results.
 Activate menu command Routine / Reprocess... or click on .

Routine / Repro- This will bring up the Reprocess results window.
cess...  In this window, make the following entries:
Name Name of original file with analysis results.

Signals The various sample readings were saved to the original
file. Recalculation is performed using signal data as input.
Spectra Spectra of individual measured values of samples were
additionally saved to the original file. Recalculation is per-
formed using spectrum data as input.
Modified sample Sample information data were changed and shall be up-
information data dated in reprocessing.
Reprocess en- Causes reprocessing of the entries in the result list cover-
tries ing the rows specified in the from and to fields.

Description Additional remark saved along with the reprocessed anal-

ysis results.
Results file
Folder Choose the save path for the results file.
Name Enter the file name for the results file.
New file/list If activated, you must enter a new file
name. The program checks if the file name ex-
ists already. Existing files cannot be overwrit-
ten.
Append to file/list New results will be appended to
the existing results file. With [...] you can open
the selection dialog. Choose an existing re-
sults file from the displayed list.
Save spectra Saves the spectra of individual measured values along
with the new analysis results.
This check box will be accessible only, if the original file
contains spectra.
 Confirm the selection of the results file with [OK] and start the reprocessing
action.
Note
Reprocessed values may be optionally saved to a new database or appended to
an existing results file. The originally obtained results are preserved unless the
original file is deleted. Thus, it is impossible to manipulate the original data.
7.7 Evaluating measurements parallel to running analyses

While measurements are running, it is impossible to evaluate results in the same
program instance. However, it is possible to start a second program instance of the
application in offline mode, while measurements are running in the first instance. In
this mode, there is no communication with the device. However, all other functions
such as developing methods or loading and analyzing results can be used parallel
to the running measurements of the first program instance.
File / Start Offline  Start ASpect CS in the second instance by menu command File / Start Of-
fline.
File / Open Re-
sults…  Open the results file of the running measurement using menu command File /
View / Update Open Results….
results list The results measured so far will be loaded in the result window.
 Further results of the running measurement can be loaded via menu command
View / Update results list or the icon button
.
You may further process the results, e.g. by loading sample details or the calibra-
tion function (→ "Displaying details of single values of samples" p. 83, "Calibration"
p. 90).
Note
In reprocessing, the recalculated results are saved to a new database. For access-
ing the original results file these must be re-opened.

7.8 Displaying results and analysis progress

Important note
Depending on the selected operating mode, the measured values are determined
in absorbance or emission. In the following, only absorbance values will be men-
tioned. The same specifications and information, however, also applies to emission
values. In numerical presentation of data, the abbreviation Abs is used for absorb-
ance values and Ems for emission values.
The measurement results and the sequence are extensively displayed in the result
window in the background of the workplace.
The presentation on different tabs in the Results window provides a good overview
of measurement results and statistical analyses.
The following tabs are selectable:
• Sequence/Results (contents of Sequence and Results tab on a single
tab)
• Sequence (displays the current sequence)
• Results (presentation of measurement results)
• Overview (summary of measurement results)
The status bar of the result window shows the file name of the current results file.
7.8.1 Sequence/Results tab

The Sequence/Results tab contains the data of the two separate tabs Sequence
and Results (→ "Sequence tab", p. 77, "Results tab" p. 78).
7.8.2 Sequence tab

On the Sequence tab, the active sequence is listed.
On this tab, you can follow the progress of the running analysis. The various sam-
ples and special functions are marked in the first column of the table as follows:
- Not measured/executed yet.

Ο Just being measured.
+ Already measured/executed.
Note
After the measurement, you can remeasure a selected sample. To this end, you
must have marked the sample row in the sequence. Then, click on on the
toolbar.

7.8.3 Results tab

The Results tab shows all measurement results and statistical analyses. The val-
ues are split up in tables for a clear presentation. The index tabs for these tables
are arranged at the bottom edge of the window.
The values are sorted by the order of sample measurement. For every sample, the
analyzed elements are listed.
Abs./Time table
The table contains the absorbance values and the statistical analyses according to
the selected method options (Method - QCC window).
No. Number in analysis sequence.

Name Sample name
Line Element line
Abs. Average of measured single absorbance values
SD Standard deviation (Sigma statistics)
RSD% Relative standard deviation (Sigma statistics)
Date/Time Date and time of measurement
Single values (Abs.) Single values of absorbance measurements
Conc.1 table
The Conc.1 table shows the analyzed concentrations of the samples as supplied
to the AAS.

Name Sample name
Line Element line
Unit Concentration unit
Conc.1 Analyzed concentration of sample
SD1 Standard deviation of Conc. 1 (Sigma statistics)
RSD% Relative standard deviation of Conc. 1 (Sigma statistics)
R Range of Conc. 1 (Median statistics)
R% Relative range of Conc. 1 (Median statistics)
Cf Confidence interval
Rem. Remarks (→ "Overview of markings used in the display of val-
ues" p. 177).
DF Dilution factor if concentration is exceeded
In the method, you can define automatic dilution by the au-
tosampler if the concentration is exceeded (→ "Auto sampler
for flame and Hydride/HydrEA technique" p. 32 and
"Autosampler for graphite tube technique (solution analytics)"
p. 35). The dilution factor of this automatic dilution procedure
by the autosampler is considered for the calculation of Conc.1.
Abs. Mean value of measured individual absorbance values
SD(Abs.) Standard deviation of absorbance values (Sigma statistics)
Single values Single values of absorbance measurements
(Abs.)

Conc.2 table
The Conc.2 table shows the concentrations of the original samples. In calculating
Conc.2, the sample information data (see Sample ID table below) are considered:
• Pre-dilution
• Weighed portion of solids
• Conversion factors for other units
Nr. Number in analysis sequence.

Name Sample name
Line Element line
Unit Concentration unit
Conc.2 Concentration of original sample taking sample information
data into account
SD2 Standard deviation of Conc. 2 (Sigma statistics)
RSD% Relative standard deviation of Conc. 2 (Sigma statistics)
CF Confidence interval of Conc. 2
Abs. Absorbance value
SD(Abs.) Standard deviation of absorbance values (Sigma statistics)
R(Abs.) Range of absorbance values (Sigma statistics)
(Abs.)
QC Res. table
The QC Res. table shows the results of QC samples: Rated and actual values of
concentration, recovery rates (not for blank) and reactions to possible deviations
(all types except blank)
No. Number in analysis sequence

Name Sample name
Line Element line
QC (for calibra- R2(adj.)
tion functions) Slope
Char. Conc. – Characteristic concentration
QC (for QC sam- Conc.1
ples, Rated value
not for QC blank) Recovery Recovery rate
With QC samples and QC Std., the recovery rate
of concentration is determined.
With QC-Stock, QC-Trend and QC-Matrix, the re-
covery rate of the concentration increase caused
by additions is determined.
QC (for blank SD Standard deviation of blank measurements
detection limit) LOD Detection limit (Limit of Detection)
LOQ Determination limit (Limit of Quantitation)
Abs. Mean value of measured individual absorbance values
For solid analytics: normalized extinction.

SD Standard deviation of absorbance values (Sigma statistics)

(Abs.)
Error table
If errors occur during the measurements, the corresponding measurements are
marked in red in all tables. In the Error table, the respective error is indicated in
writing.
Single val. table

The Single val. table contains the measured individual absorbance values.
Sample ID table
The Sample ID table contains the sample information data (→ "Create information
data for samples and QC samples" p. 63).

Name Sample name
Line Element line
Pos. Position of sample on autosampler
Pre-DF Pre-dilution factor. Factor by which the original sample was di-
luted before being placed on the autosampler or supplied to the
spectrometer, if no autosampler is used. The factor is required
for the calculation of the concentration of the original sample
(Conc.2).
Wt.[g] Only for solution analytics
Weighed portion in grams. The weight of the original sample,
which was dissolved in sample preparation (in mL). The weight
is required for the calculation of the concentration of the original
sample (Conc.2).
Vol.[ml] Volume of solvent used to dilute the weighed sample portion (in
mL). This value is required for the calculation of the concentra-
tion of the original sample (Conc.2).
Name (2) Additional sample name.
AS-DF Dilution factor of the autosampler.
Blank corr. Blank correction.
off No blank correction performed.
on For the calculation of the concentration of the original
sample, the blank measured last in the sequence will
be subtracted.
Factor This field is not used so far.
7.8.4 Overview tab

On the Overview tab, the analysis results are summarized. You may choose
among various presentation options:
• Conc.1 – Concentration 1
• Conc.2 – Concentration 2

• Abs.(RSD%/R%) – Absorbance (Relative Standard Deviation or Relative

Range)
• LOD – Limit of Detection
• LOQ – Limit of Quantitation (also known as Limit of Determination)
• Recovery (Rated value) – Recovery rate (rated value)
• R2(adj) – Correlation of calibration curve
By activation of the respective check boxes, the following sample types can be
displayed:
• Samples
• QC samples
• Cal. Std.
• Other
The print icon opens the window Print Overview from which the printout pro-
cess can be started. In addition to the printout, the data can be optionally saved as
TXT-, HTML- or PDF files (→ "Creating and printing result reports" p.152).
7.8.5 Solid tab

The Sequence tab provides a listing of the currently active sequence for solid
analysis.
It breaks the various sequence-listed samples down by individual measurements in
the same manner as the SSA-600 table does and indicates their weighed portions,
tares and dosing states (→"Specifics for solid sample analysis with SSA 600" p.
70)
7.9 Opening, closing and printing analysis results

Opening a results file
You may open a results file for reviewing the results.
If you want to have sample information data, e.g. sample names or dilution factors,
included in reprocessing, it is necessary to extract sample information when load-
ing the file. Then, sample information data are accessible in the Sample ID window
(→ "Create information data for samples and QC samples" p. 63).
To load a calibration function, the method parameters must have been saved to the
results file. The method parameters are loaded when the calibration file is opened
and can then be viewed and edited in the Method window.
Line spectra are accessible only if a file with the spectra was saved along with the
results file.
File / Open Re-  Activate menu command File / Open Results... to open the standard Open
sults... dialog.
 Choose the results file to be loaded.
This will bring up the Load results window. In this window, beside device

name and its serial number, also the used analysis technique, the software
version and the optional description are displayed.
 If, in later steps of operation, you need the sample information data, activate
the Extract sample information check box.
 Conform your choice with [OK].
The results file is being loaded and displayed in the result window.
Note
The name of the currently loaded results file appears in the status bar of ASpect
CS.
Clearing results list from the display

Edit / Clear Re-  To clear the results list from the display, use menu command Edit / Clear Re-
sults Table sults Table.
Note
Sequences transferred to the process and result window remain displayed there.
Printing result reports

The contents of result reports can be defined in the Data management - Reports
window (→ "Data management and report printout" p. 152). The compiled ele-
ments are summarized in a report file, which can be saved and reloaded.
File / Print / Re-  Start the printout of the result report by activating menu command File / Print /
port... Report....
This will bring up the Data management - Reports dialog.
 In this dialog, choose the desired options and then click on [Print].
7.10 Sample details and spectra

In the result window, the measured single values of every measurement and, if
saved along with the results, the spectra may be displayed in the separate Single
values window.
Note
Activate the spectra-saving option in the Method - Output window (→ "Output tab
– screen view, printout and saving options", p. 56).
 To open the Single values window, double-click with the left mouse button on
the desired sample row of the result table.
 Alternatively, right-click on the row of interest of the result table. In the appear-
ing context menu, click on Detail results....
View / Detail re-  Another alternative to open Single values window is to mark the respective
sults... row of the table and then activate menu command View / Detail results....

7.10.1 Displaying details of single values of samples
Fig. 25 Single values window
Sample data
Fe303 (Example) Analyzed element line
No. Number of measurement
Name Sample name
Abs. /Ems. Absorbance or emission value (averaged over all single values)
SD Standard deviation (Sigma statistics). This parameter is dis-
played independently of the statistical method chosen for the
measurement (Sigma/Median).
RSD Relative Standard Deviation (Sigma statistics). This parameter
is displayed independently of the statistical method chosen for
the measurement (Sigma/Median).
Date / Time Date and time of the measurement selected in the table
Displaying / deleting single values

The measured single values of the samples are shown in the table.
No. Number of single value within the sample measurement

Wt. [mg] For solid analytics:
Weighed portions of individual samples.
Abs Calculated absorbance of single value

Rem. None The single value is included in the calculation of

the mean value of the sample
#MAN. The value was manually excluded from the calcula-
tion of the sample value
#CORR. The value was automatically excluded from the
calculation of the sample value due to the Grubbs
outlier test.
[Exclude] / [Re- Exclude the single value from average calculation or reinclude
include] it.
[Show spectrum] Accessible only in scientific mode and if single spectra were
saved along with the measurement results.
Display of the measured wavelength-dependent line spectra,
from which the single sample value results.
Overlapped Single spectra are overlapped in the graphic. The marked
single spectrum is highlighted in bolt.
Replace with Only for calibration standards

entry numeber During reprocessing of the analysis results the actual calibra-
tion standard will be replaced by sample at the entered posi-
tion in result table.
In the graph right of the table, the signal curve of the marked single value is shown
as a function of time. The number of measuring points corresponds to the number
of measured spectra. Spectrum number and Time (read time) were specifically
defined for each element line in the Method - Lines window (→ "Lines tab –
Choosing element lines", p. 22).
If desired, you may manually exclude a single value from the calculation of the
sample average.
 To this end, mark the single value to be excluded in the table.
 Click on [Exclude] to exclude the value from the calculation of the sample av-
erage for result reprocessing.
 To reinclude the previously excluded single value in average calculation, click
on [Reinclude].
Note
By activating the Grubbs outlier test option, outliers among single values can be
detected and eliminated automatically during the analysis.
Buttons
You can select the next line or the next sample of the results list for display by us-
ing the buttons:
Previous sample
Previous line
Next line
Next sample
The spectra window is updated accordingly.

7.10.2 Displaying spectra

Accessible only in Scientific Mode and if single spectra were saved together
with the measurement.
The line spectra of a single value can be loaded from the Single values window.
 Mark the single value of interest in the table of the Single values window.
 Click on [Show spectrum] to activate the spectrum display.
This will bring up the Spectra window.
In the Spectra window, you can:
• Display the individual spectra
• Vary background correction
• Display the family of spectra in a 3D-plot
• Perform wavelength correction.
The wavelength correction provided in the Spectra – Adjust wavelength window
is described in Section "Correcting peak offsets", p. 103.
7.10.2.1 Showing single spectra and varying background correction

In the Spectra - Processing window, single sample values are shown in different
views. As a result of data acquisition by means of the CCD line, a three-
dimensional family of spectra of signal changes is generated as a function of wave-
length range and time. Sections are laid through the family of spectra to get a two-
dimensional view of the measuring curves:
• At a fixed wavelength (pixel) versus time
• At a fixed time versus the wavelength range.
Both diagrams can be shown in the graph.
Fig. 26 Spectra – Processing window: Display of single spectrum and background

correction

Graphic presentation
In the wavelength plot, the abscissa is graduated in Pixels. Three red wavelength
values indicate the upper and the lower limit of the measured spectral range and
the position of the measurement pixel (peak of element line). The data points for
background correction are marked by gray lines. The measurement pixel is set off
by a continuous red line. The range of evaluation pixels is marked in light red.
Plot selection Absorbance Absorbance spectrum

list box Reference energy
Energy of reference spectrum (average only)
Sample energy
Energy of sample spectrum
Spectrum Shows the spectral curve of a selected measurement vs. wave-
length.
Choose the number of the measurement to be displayed from
the field with spin box.
average If this check box is activated, the spectral curve av-
eraged over all measurements is displayed. The
button [...] opens a window where the range used
for averaging the spectra can be restricted. In this
case the start and the end spectrum number of the
averaging range have to be entered.
Pixels Shows the spectral curve at a selected pixel vs. time.
Choose the number of the pixel to be displayed from the field
with spin box.
Eff. If this check box is activated, the integral over the
evaluation pixels is shown.
Graphic zoom in.
Left-click this button and holding the mouse button depressed
select the spectrum section to be zoomed in.
Resets the zoom to the original coordinates.
Activates the text mode. Holding the left mouse button de-
pressed draw a frame and type in text, which can be added to
the graph.
A double click on existing text opens the window for editing or
deleting the text. Holding the Ctrl-key and the right mouse but-
ton depressed, you can shift existing text across the graph.
Select button. Activates the selection mode in signal or spectral
plots. On activation, measuring points are marked in the graph.
With the left mouse button, you can add a vertical line cursor to
the graph at the desired position.

Set or delete background correction pixels.

A green cursor is displayed when the mouse is over the spec-
trum plot. Pixels can be selected by clicking on the respective
pixel. Clicking on an already selected pixel deletes the selec-
tion. Adjacent pixels can be selected or deleted by mouse
dragging.
Clicking on the arrow opens a context menu:
Mark background correction pixels
Highlights the selected pixel on the spectrum plot
(green marker).
Delete all background correction pixels
Deletes all selected correction pixels.
Liste of background corredction pixels...
Lists the pixel numbers of the selected background
correction pixels.
Activates line identification mode. Clicking on a spectral region
or dragging with the mouse searches the line database for the
selected position. The element symbol is displayed next to the
mouse cursor (→ „
Line identification“).
Moves the vertical line cursor in 1-pixel or measured value in-
crements across the graph. The data of the currently marked
measuring point are displayed below the tool buttons.
Y-Scale Scaling of the graph
auto Auto scaling – the spectrum is displayed at optimal
ordinate expansion.
from/to Manual scaling. Specify the ordinate limits in the
fields below.
Varying background correction and evaluation pixels

The software allows you to change the support points used for background correc-
tion. The thus resulting changes in the signal curve are simultaneously displayed
on the graph. As a result, the mean value of the sample is optionally calculated
either simultaneously or, with bulk data, on activating a separate command. The
found new correction pixels may be transferred directly to the opened method. In
this way, it is possible to find the ideal background correction mode for a new
method.
BG parameters
Mode Used background correction method –

with reference, without reference or IBC (iterative baseline
correction)
No. of spectra Number of measurements the single value of the sample is
based on.
Range (pixels) Evaluated spectral range.
Maximally, the stored number of pixels can be used for the
evaluation. If the evaluation range is restricted, the pixels left
and right of the measurement pixel are distributed symmetrical-
ly.
Range [nm] Indicates the width of the spectral range used for the evalua-
tion, which depends on the selected number of pixels.
Meas. Pix. Display of the measurement pixel. The measurement pixel is
pixel # 101 in the center of the detector line.

Eval. Pixels Number of pixels used for the evaluation of the measured sig-
nal. The integral that represents the measurement result is
calculated over the measured values of these pixels.
dynam. BGC fit Automatic searching of correction pixels.
Spectral corrections
Correct perma- Automatically corrects permanent structures (only active with

nent structures methods using background correction “with reference”). Per-
manent structures are spectral structures which occur in the
reference as well as in the sample spectrum, e.g. caused by
flame absorptions. Use this setting if these structures are not
completely compensated.
Model Selection of model for spectral correction (→ „Working with
Correction Spectra in ASpectCS Software“ p. 180).
Abs. (Mean) Displays the mean value of the sample absorption (Abs
(corr.)).Using graphite tube technique displays additional the
background absorption (Abs (BG)).
[Line parame- Loads lines parameters for background correction and spectral
ters] evaluation from the method or sends them to the method.
[3D plot] Open an additional window for spectra display.
Select the next line or the next sample of the results list for dis-
play (as in window Single values).
Loading/sending line parameters

 In the Spectra window, click on the [Line parameters…] button.
This will bring up the Line parameters/Processing window.
 From the line table, choose the line whose parameters you want to send to the
method or load from the method.
 Activated the desired action.
Copy from method/line – loads the original parameters from the method
Copy to method/line – sends the modified parameters to the method.

7.10.2.2 3D presentation of the spectra of single values

The family of curves obtained from the single values of the sample is displayed in
the Spectra – Plots window.
Fig. 27 Spectra – Plots window: 3D presentation of spectra based on single value of

the sample
The left side of the Plots tab and its options are identical with those of the Pro-
cessing tab. On the right side, the plot of the family of spectra is shown three-
dimensionally at variable tilts.
The spectrum/pixels selected on the left side is/are marked by a light green on the
plot.
Redraws the plot of the family of spectra at different speeds

from very slow to fast.
Display 3D Three-dimensional presentation
By changing the settings in the Rotate and Tilt spin
boxes, the viewing angle of the plot can be varied.
2D Two-dimensional presentation of spectra dependent
on the pixels
Contour Top view onto the family of spectra.
Absorbances of the same level are connected by
contour lines.

7.10.2.3 Line identification

Spectral peaks and molecular bands in the recorded data can be identified based
on a spectra and line database.
Fig. 28 Spectra – Line identification window
The upper list displays the entries found in the line database for the current spec-
tral region. Selecting a row sets the plot cursor on the corresponding wavelength.
Clicking on a spectral region or dragging with the mouse searches element line at
the selected position in the line database. The element symbol is displayed next to
the cursor and the corresponding list entry is selected.
The lower list shows the entries found in the molecule spectra database for the
current spectral region. Selecting a line displays the corresponding molecule spec-
trum. Factor multiplies the spectrum with the entered value while Offset shifts the
spectrum. The check box Show sum spectrum activates an additional list column
for displaying the sum of selected spectra. These functions may be used for model-
ling complex background spectra.

7.11 Calibration
Calibration is carried out during sample measurement according to the options
selected in the sequence. The calibration curves and functions can be viewed and
edited after the measurement.
Note
After the opening of stored results, the calibration can be displayed only if the
method has been saved along with the results.
 Open the Calibration window using menu command Method Development /

Calibration... or the icon button
Method Develop-
ment / Calibration
The calibration window displays the calculated calibration curve (taking the curve
parameters into account).
Fig.29 Calibration window
The window contains

• Graph of the calibration curve,
• Calibration table
• Parameters
• Residuals
• Limits of detection (LOD) and limits of quantitation (LOQ).
Selection list boxes in Calibration window
Line Select the element line the calibration of which shall be dis-
played.

Calibration func- Display of the used calibration function (set in the Method -
tion Calib. window).
The calibration function is specific for every element line.
You may select a new calibration function from the list box. The
calibration will then be recalculated accordingly.
7.11.1 Graphic presentation of calibration curve

In the graph, the measuring points, the calculated calibration curve, and the resid-
uals are displayed. The numbers at the measuring points correspond to those used
Method Develop- on the Table tab.
ment / Calibration
Other markings used
Z Zero. Calibration zero
Colors of measuring points:
Black Normal measuring point

Light gray Deleted/outlier (not included in calculation)
Blue Suspected outlier (included in calculation)
Curve colors:
Black Calibration curve within the valid calibration range

Blue Calibration curve outside the valid calibration range
Green Lower and upper limit of the prognosis range within the valid calibra-
tion range
Light gray Lower and upper limit of the prognosis range outside the valid calibra-
tion range
Note on prognosis range

The position of the prognosis range depends on the selected statistical certainty. It
is a measure of the “quality” of the calibration, from which also the statistical cer-
tainty of the measurement of the analytical samples depends in the end. Besides,
the prognosis range serves to identify suspected outliers among the calibration
points. The confidence level is to be chosen in the Method - Statistics window
(→"Statistics tab – Defining statistical analysis", p. 48)
7.11.2 Displaying calibration results

Display of measured values of calibration standards – Table tab
On the Table tab, the value pairs of the standards (entered concentration / meas-
ured value) are displayed.
Method Develop- If the standards were measured repeatedly and a statistical analysis option set in
ment / Calibration the method, you may additionally activate the display of the standard deviation
(SD), the relative standard deviation (RSD%), the range (R) and the relative range
(RR%) by selecting the corresponding check boxes.

Note
The statistical analysis is to be defined in the method.
To exclude individual calibration standards from the calculation, select the standard
in the table by a mouse click and then click on [Delete Std.].
The measurement is only marked as deleted and can be reactivated at any time.
Display of calibration data – Parameters tab

This tab shows the calibration data as far as their calculation makes sense.
R² (adj.) Coefficient of determination

Slope Slope of calibration curve
Method SD Standard deviation of the method
Char. Conc. / Characteristic concentration or weight (concentration or weight
Char. Weight required to absorb 1% of the available light energy in the atom-
izer – corresponding to an absorbance value of approx. 0.0044)
Residuals tab
The graph on the Residuals tab shows the deviations of the calibration points from
the calculated calibration curve and the limits of the prognosis range.
Limits of detection and determination of the current calibration -

LOD/LOQ tab
The limits of detection and the limits of determination of the AAS can be deter-
mined based on the current calibration results.
In this area, values of the blank method and the calibration curve method will be
displayed only if the AAS has been calibrated already.
Limit of detec- The weight (concentration) of the element to be analyzed that

tion can be detected with a defined statistical certainty.
Limit of determi- The minimum weight (concentration) of the element to be ana-
nation lyzed that can be determined with a define confidence level.
SD Blank Only with blank method.
Measured standard deviation of the blank (IDL sample).
[Calculate] Starts the calculation of the limits of detection and determina-
tion, e.g. after a change of the calibration curve.
Calibration curve method

The calculation of the limits of detection and determination according to the calibra-
tion curve method necessitates a linear calibration curve. The calibration should be
carried out in the lower concentration range. Calibration parameters that are es-
sential for the result of computation include the following:
• Number and position of calibration points
• Number of repeat measurements per standard
• Quality of regression
• Slope of calibration curve
• Relative statistical certainty (probability level)
The values obtained from the calibration curve method can be considered useful
only if the calibration was run in the lower concentration range. The limits of detec-

tion and determination can be displayed and printed in the Calibration window.
They are not saved in the result protocol.
Blank method
The standard deviation of the blank is determined within the sample measurement.
For this purpose, the measurement of the blank (QC Blank DL) is included in the
sequence (→"Specifying sequences of samples and actions", p. 60).
Calculation instructions for the blank method:
The blank is to be measured 11 x. From the obtained values, the absolute standard
deviation SD of the blank is determined. The following formulas apply to the limits
of detection and determination:
Limit of Detection (LOD) LOD = 3 * SD / (slope of calibration curve)
Limit of determination (LOQ) LOQ = 10.0 * SD / (slope of calibration curve)
The limits of detection and determination according to the blank method are dis-
played in percent.
7.11.3 Modifying the calibration curve

You can modify an existing calibration curve by the
• change of the used calibration function
Method Develop-
ment / Calibration • deactivation or activation of standards.
To change the calibration function, choose a new model from the Calibration
function list box.
To exclude a standard from the calculation, mark it on the Table tab and then click
on the [Delete Std.] button. The measurement is only marked as deleted and can
be reactivated at any time.
The program recalculates the calibration curve and displays the modified curve.
Routine / Repro- The modified calibration parameters will be applied to the results, if you activate
cess
menu command Routine / Reprocess... or click on on the toolbar (→
"Reprocessing analysis results", p. 75).

7.12 Quality control

The Quality Control function serves to monitor the measurement results of a meth-
od over a longer period of time. For this purpose, specific QC samples of different
types are chosen for a method and included in the measurement series. When
evaluating the QC samples, the results are compared to those obtained with previ-
ous QC samples.
The evaluations are presented on quality control charts (QC charts) and saved
along with the method. The QC charts are available after every loading of the
method and will be updated at the next measurement start.
Select the type of QC samples and their parameters in the Method window on the
QCS tab (→ "QCS tab – Quality Control Samples", p. 50). In the Sequence win-
dow, define the integration of the QC samples within the measurement series (→
"Specifying sequences of samples and actions", p. 60).
You can view the QC charts of the loaded (active) method in the QC window.
There, you can also define the parameters and the configuration of the QC charts.
 Open the QC window using menu command Method Development / QC... or
icon button
Method Develop-
ment / QC... .
7.12.1 Parameters of QC charts
QC charts pa-
rameters tab
Fig.30 QC – QC chart parameters window
The content of the QC charts is defined in the QC window on the QC charts pa-
rameters tab and can be customized to the requirements of your laboratory re-
garding the frequency of the entries.

Entries
Number prep. The preparation period is a number of QC chart entries that are
period used for the calculation of control limits (C) and error limits (E).
The preparation period always contains the older chart entries.
If set to 0 (no prep. period), all entered QC data will be includ-
ed in the calculation of control and error limits.
Max. number of Total number of entries on a QC chart.
entries A full chart must be renewed (see below).
Enter scheme All values Enters every performed QC action.
1 value / day Enters the last QC action of the day only.
2 values / day Enters the first and the last QC action of the
day only.
Definition of "day": A "day" corresponds to one day according to the PC clock, i.e.
in the course of a day, any previous entry on the QC chart will be overwritten by a
new QC value; however, when a new day begins, a new entry will be generated.
Chart display
Specification of the type of QC evaluation to be displayed on the QC chart:
QC sample type Type of QC evaluation

QC Sample Mean values
QC Standard Mean values (normalized)
Recovery rates
QC Trend Trends
QC Matrix Ranges
Precisions
Blank No choice. The absorbance of the blank is displayed.
Updating displayed charts

Defines how to proceed with (almost) full charts:
Accept prep. Accepts the preparation period of the old chart for application
period, delete to the new chart and deletes remaining values.
remain
Last values > The values of the old chart measured last represent the prepa-
new prep. period ration period of the new chart; all other values will be deleted
from the chart. New measured values will be evaluated based
on the newly created preparation period.
Delete all, new All values will be deleted. New measured values will first fill the
prep. period preparation period.
[Process] Deletes the charts according to the option selected above.
Graphic options (Other settings)

In this field, you can choose the point size used for the graph, and if the points
shall be connected with each other by a line.
Point size The individual points are displayed as circles. Choose a higher
point size for larger circles.
Connect points Connects the points on the graph with each other by a line.

7.12.2 Displaying QC charts

The QC charts are displayed in the QC – QC charts window.
Separate charts are generated each for every QC sample type defined in the
method and for every element line specified there.
Fig. 31 QC – QC chart window
Type Here, choose the QC sample type to be displayed.

Line Here, choose the element line to be displayed.
Displayed val- Number of displayed values and the date of the first and the
ues last value displayed.
Entries Total number of entries on the current QC chart and the date of
the first and the last value.
x(max) Select the number of entries to be displayed on the graph.
Prints the QC graph inclusive of alphanumerical data and
measured values.
Marks and colors used in the QC chart graph

Yellow field Preparation period
Light gray hori- Mean value calculated from preparation period
zontal line
Red horizontal Upper and lower control limit (C) calculated from prepara-
lines tion period (3 Sigma)
Green horizontal Calculated warning limits (W; 2 Sigma).
lines
Small black cir- Measuring points
cles
If you click on a measured value on the graph, a window is opened with the follow-
ing information on this measured value.
Number Number of the measured value in the QC series

Value Measured value (converted according to the presentation type of

the QC chart)
Date / Time Date and time of measurement
User Displayed when working with User Management indicating the
user logged in at the time of measurement.

Controlling and monitoring spectrometer and accessories
8 Controlling and monitoring spectrometer and

accessories
8.1 Spectrometer
The Spectrometer window serves to test spectrometer functions and method de-
velopment. The following data can be adjusted or viewed and the following actions
Method Develop- performed:
ment / Spectrome-
• Device data
ter...
• Switching xenon lamp on/off
• Test of wavelength correction
• Display of the readout parameters of the CCD line
• Starting a measurement at a test wavelength
• Starting a continuous measurement for device optimization
• Correction of possible peak offsets.
 Activate the Spectrometer window using menu command Method Develop-
ment / Spectrometer... or icon button
8.1.1 Device function test on contrAA
Parameters tab
Fig. 32 Spectrometer – Parameters window
In the Spectrometer – Parameters window, you may check basic device functions
and start a test measurement at a selected wavelength.
Basically, all control lamps must be active and lighting green, when the contrAA
has been switched on and initialized.

Device functions are tested by a click on the corresponding buttons. If the test run
was successful, the lamp lights green.
Instrument data
Display of the connected AAS device and the installed software version.
Lamp
[Lamp off] / Switches the xenon lamp on/off.

[Lamp on]
[Shutter open] / Opens or closes the shutter.
[Shutter closed]
[Hot spot Init.] Reinitializes the system for hot spot tracking.
Standby If activated, lamp current is switched to standby mode. This
function serves to extend lamp life.
Current [A] Allows varying the current.
The factory-set lamp current has been optimized for igni-
tion behavior and lifetime!
Remaining lamp Only if option Show remaining lamp life on window Options –
life time Display is activated.
Remaining life time of the xenon lamp (0% corresponding to
2000 h). A red bar is displayed starting with 1000 h.
Wavelength
Wavelength Display of the selected wavelength.

Clicking the [...] button will bring up the Select Element/Line
window for setting the desired wavelength (→ "Lines tab –
Choosing element lines", p. 22).
By a click on [Set], the monochromator is driven to the selected
wavelength.
Corrections
Prism corr. Checks the wavelength correction on the Monochromator.

Ne correction Performs wavelength correction by means of neon lines.
Measurement
Read time [s] Entry of the total time for spectral measurement.
[Measurement] Start the measurement based on the adjusted parameters.
Emission meas- If deactivated, the absorbance spectrum will be measured.
urement If activated, the emission spectrum will be measured.
Always open If activated, the measurement in window Spectrometer are
shutter always performed with opened shutter. When checking the
system with closed shutter, e.g. for dark current measurement,
the control has to be deactivated.
Note: The setting has no effect for measurements performed
outside of the window. In all other cases the shutter is automat-
ically controlled.
Always request Performs a reference measurement before every sample
reference measurement.

8.1.2 Measuring a spectral peak at a selected wavelength

To trigger test measurement at a slected wavelength, use the Spectrometer –
Parameters window.
 In the Wavelength/Correction field, click on [...] to open the Select Ele-
ment/Line window. There, choose the desired line.
Parameters tab  Alternatively, you may enter the value directly in the Wavelength input field.
 Click on [Set] to drive the monochromator to the desired wavelength.
If the adjustment was successfully finished, the indicator lamp left of the button
will light green.
 In the Read-out parameters field, enter the values for Read time [s] and No.
of spectra.
 Activate the Always request reference check box.
 Start the measurement with the [Spectrum recording] button and follow the
prompts for the reference and the following sample measurement.
The measurement results are displayed in the Spectra window (→ "Displaying
details of single values of samples", p. 83).
8.1.3 Starting continuous measurements
Spectrum tab
Fig. 33 Spectrometer – Spectrum window
In the Spectrometer – Spectrum window, you can start a continuous measure-

ment at a defined wavelength. In servicing, the continuous measurements are used
for device optimization.

Graphic and digital evaluation
Display Options for the presentation of the spectrum:

Energy Display of energy spectrum; measuring unit: cts
(counts)
To obtain results with the noise being as low as
possible, the integration times for the CCD line are
to be chosen so that the maximum energy is at ap-
proximately 30000 cts.
Absorbance Display of absorbance spectrum
Intensity Display of the energy per time unit; unit of meas-
urement: Mcts/s (megacounts per second)
The intensity allows you to compare the absorption
of different peaks independent of the integration
time.
Meas. pix. Selection of the pixel the values of which are continuously dis-
played in the Energy field.
In the Maximum and Minimum fields, the corresponding re-
sults of the continuous measurement are displayed.
Mark meas. pix- Marks the set Measurement pixel in the graph by a vertical
els red line.
Mark points Marks every pixel in the graph by a point (circle).
Scaling of graph Scaling of the graph is possible by direct entry of the start and
end points of ordinate and abscissa in the input fields or – after
activation of the zoom mode – by selection of the area to be
zoomed in with the left mouse button depressed (→
"Frequently used control elements" p. 8).
To undo scaling, activate the auto check box or deactivate the
zoom mode.
 In the Spectrometer – Parameters window, adjust the following parameters:

wavelength, read time, no. of spectra.
 Switch to the Spectrum tab.
 Start the reference measurement by a click on [Ref. spectrum].
If a reference spectrum has been measured, the indicator right of the button
lights green.
 Start the continuous measurement with [Start].
The values are measured with the adjusted parameters. The measurements
are repeated continuously until you click on [Stop].

8.1.4 Correcting peak offsets
Fig.34 Spectra – Adjust wavelength window: wavelength adjustment for peak offsets
The contrAA is delivered pre-adjusted, i.e. frequently used analysis wavelengths

are tested and adjusted in the factory. If you intend to use a less customary analy-
sis wavelength, you can check the accuracy of this wavelength in the Spectra –
Wavelength adjustment window. Corrections of peak offsets are possible in the
subpixel range, i.e. smaller than the pixel dispersion.
The found correction factors are saved to the line/wavelength file and are valid for
every further measurement. However, it is also possible to delete entered correc-
tion factors from this file again. The device-specific line/wavelength file may be
copied and loaded for reviewing it (→ "Copying lines/wavelengths files", p. 161).
Peak pick
Arrow buttons Use these buttons to shift the peak wavelength.

Pixels Currently selected pixel
Wavelength Current analysis wavelength
Dispersion Spectral resolution in picometers per pixel
[pm/Pixel]
Stretch x-axis Expands the abscissa to facilitate peak finding.
(factor)
[Find Peak Cen- Find peak and correct offset automatically.
ter]
Update adjustment value
Current offset Displays the found offset value.

[nm]
Obs. offset [nm] Displays the previously stored offset value.
[Save adjust- Saves the adjustment value to a line/wavelength file. The val-
ment value] ues stored in this file will be used for all following measure-
ments.

[Delete adjust- Deletes the entry for the current analysis wavelength from the
ment value] line/wavelength file.
 In the Spectrometer – Parameters window, set the analysis wavelength and

start the measurement of the analysis peak (→ "Measuring a spectral peak at a
selected wavelength", p. 101).
The results of the measurement are displayed in the Spectra window.
 Switch to the Spectra – Adjust wavelength window.
 Expand the x-axis to make the peak well visible.
 If the peak is centered to the analysis pixel 101 (red vertical line coincides with
the peak), the peak has been detected correctly. In this case, no further action
is required.
 If the peak appears beside the red line, use the arrow buttons to move the
green line onto the peak
or
have the peak position found automatically using the function released with the
[Find Peak Center] button.
 Save the peak correction with the [Save adjustment value] button.
 In the Spectrometer – Parameters window, start another measurement at the
analysis wavelength.
Now, in the Spectra – Adjust wavelength window, the peak must be centered
to the analysis pixel 101.

8.2 Flame
Selected technique: Flame
In the Flame window, you can test individual functions of the burner/nebulizer sys-
tem and individually adjust the parameters for the elements.
Method Develop-  Activate the Flame window using menu command Method Development /
ment / Flame... Flame... or icon button
8.2.1 Testing flame functions

On the Control tab, you can check the current status of the burner/nebulizer sys-
tem.
Control tab
Fig.35 Flame – Control window tab
Status
Flame Status display of the flame:

off The flame is not burning.
C2H2/Luft The acetylene/air flame is burning.
C2H2/NO2 The acetylene/nitrous oxide flame is burning.
Burner Attached burner head:
100 mm 100-mm single-slot burner
50 mm 50-mm single-slot burner
Error No burner head attached

Siphon The fill level of the siphon (drain trap) below the mixing cham-
ber is monitored. The drain trap serves to drain non-nebulized
liquid.
OK The drain trap is filled with liquid up to the overflow
port.
Error The fill level of the drain trap is insufficient.
The drain trap must always be filled sufficiently to prevent
backfiring of the flame particularly that of the nitrous oxide
flame. In case of error prompt remove the burner head. Fill
distilled water in the mixing chamber till the error prompt disap-
pears.
Waste bottle Fill level of waste bottle. (If you do not use a waste bottle with
fill level sensor, plug the supplied jumper plug into the corre-
sponding connector).
OK The waste bottle is not full (correct state).
Error The waste bottle is full and needs to be emptied.
Measurements are possible; on starting a meas-
urement, however, a warning message will be dis-
played.
Pressures
Fuel Status of fuel pressure at device inlet

"-" – No fuel pressure detected
Nebulizer Operating pressure at nebulizer.
Air Status of air inlet pressure. Displayed only when air supply is
open.
N2O Status of nitrous-oxide inlet pressure. Displayed only when the
nitrous-oxide supply is open.
Actual gas flows
Fuel Fuel flow

Oxidant Oxidant flow through nebulizer
Oxidant (total) Total oxidant flow (oxidant + auxiliary oxidant). Displayed only if
auxiliary oxidant is active.
Fuel/Oxidant Fuel/oxidant flow ratio
Function tests
The test functions are accessible only if the flame is extinguished. The availability
of the test functions depends on the context.
[Test air] Opens solenoid valve in air path.

Requirement: Air and fuel are supplied (inlet pressures de-
tected)
Displayed parameters: nebulizer pressure, oxidant flow and
total oxidant, if auxiliary oxidant was activated (Method –
Flame window).
[Test N2O] Opens solenoid valve in nitrous-oxide path.
Requirement: Nitrous oxide and fuel are supplied (inlet pres-
sures detected).
Displayed parameters: Nebulizer pressure, oxidant flow and
total oxidant, if auxiliary oxidant was activated.
Active only with acetylene/nitrous oxide flame and 50-mm sin-
gle slot burner.

[Test fuel] Adjusts the rated gas flow (proportional valve).

Displayed parameters: Fuel flow for acetylene/air flame (for
[Test air] or the acetylene/nitrous-oxide flame (for [Test
N2O]).
Being activated with [Test air] and [Test N2O].
[End Test] Finishes the function test.
Flame / Scraper
[Ignite flame] Ignition of the acetylene/air flame:

Air supply is released.
Ignition arm is swiveled out; the coiled filament is glowing.
The rated acetylene flow (proportional valve) is adjusted, when
nebulizer pressure and oxidant flow have reached their rated
values.
Process is aborted, if the flame fails to ignite within 10 seconds.
If the flame is burning, the [Extinguish flame] button becomes
active.
[Ignite flame] is active, if the flame is not burning.
[Air→N2O] Switching from acetylene/air to acetylene/nitrous-oxide flame:
Oxidant valve (3/2 solenoid valve) switches from air to nitrous
oxide.
The fuel flow for the acetylene/nitrous-oxide flame (proportional
valve) is adjusted.
The button label turns into [N2O→air].
[N2O→Air] Switching from acetylene/nitrous-oxide flame to acetylene/air
flame:
Oxidant valve (3/2 solenoid valve) switches from nitrous oxide
to air.
The fuel flow for the acetylene/air flame (proportional valve) is
adjusted.
The button label turns into [N2O→air].
[Extinguish Extinguishes the flame:
flame] If the acetylene/nitrous oxide flame is burning, the system
switches to the acetylene/air flame and waits for a few seconds.
The fuel flow (proportional valve) is shut off.
After a few seconds waiting time (for purging the fuel from mix-
ing chamber and burner), the air supply (solenoid valve) is shut
off.
Scraper Only with 50-mm single slot burner with mounted scraper and
acetylene/nitrous-oxide flame.
Activates the scraper for cleaning the burner head.
Settings
In the Settings field, you may edit the gas flow settings:
C2H2/air Acetylene/air flame: Fuel flow = 40 – 120 NL/h

C2H2/NO2 Acetylene/nitrous-oxide flame: Fuel flow = 120 – 315 NL/h
Oxidant (total) Adjustment of auxiliary oxidant by adjusting the total oxidant
flow (Oxidant (total) = Oxidant flow + auxiliary oxidant flow).
30 - 300 NL/h
The use of the auxiliary oxidant is useful if combustible liquids
shall be analyzed, a higher oxidant flow is necessary, or the fuel
rate shall be increased.
Burner height Height of burner relative to optical axis.

Note
The attached burner is automatically detected by the burner sensor. Switching be-
tween C2H2/air and C2H2/N2O is possible only if the flame is burning, and if the
50-mm burner has installed.
8.2.2 Optimizing the flame

For the analysis, the flame can be optimized for every element line with respect to
• Fuel flow
• Burner height
• Total oxidant flow, if the use of auxiliary oxidant has been chosen in the
method.
You may optimize the flame manually by changing the parameters and observing
the signal level, or you may have the parameters searched automatically by the
application. In both cases, you may transfer the found parameters to the method at
the push of a button.
8.2.2.1 Manual flame optimization

Manual flame optimization is carried out in the Flame – Manual Optimization win-
dow.
Manual optimiza-
tion tab
Fig. 36 Flame – Manual Optimization window
Line Choose the element line for which the flame shall be optimized.
You may choose among the wavelengths defined in the meth-
od.
[Set] Moves the monochromator to the selected wavelength.
Fuel [L/h] Adjustment of fuel flow.

Burner height Adjustment of burner height relative to the optical axis of the
[mm] light path of the xenon lamp.
Oxidant (total) Adjustment of total oxidant flow, sum of the flows of oxidant
[L/h] and auxiliary oxidant.
Oxidans [L/h] Display of the oxidant flow in L/h.
Fuel/Oxidant Display of the fuel/oxidant flow ratio.
[Start] Starts the measurement. The signal is continuously being rec-
orded.
The button label turns into [Stop].
[Stop] Stops the measurement.
[Accept values] Accepts the found flame parameters for the selected element
line and transfers them to the method.
Graph Display of signal curve.
Ordinate expansion is possible via the input fields at the Y-axis.
Absorbance Display of current absorbance value.
Maximum Display of the maximum absorbance value of the running
measurement.
Procedure
1. From the Line list box, choose the desired element line.
2. Click on [Set] to drive the monochromator to the wavelength of this line.
3. Immerse the aspiration hose of the nebulizer in the sample solution.
4. Start the measurement with [Start].
5. Vary the Fuel setting by means of the arrow buttons and watch the signal
change in the graph and in the Absorbance field. Adjust the fuel rate until ab-
sorbance is maximal.
6. In the same way, adjust the Burner height, until you have found the maxi-
mum absorbance.
7. When using the flame with auxiliary oxidant, vary the Oxidant (total) parame-
ter until again you obtain the maximum signal level.
8. Repeat steps 5 to 7, until you can no longer notice a relevant increase of the
signal level.
9. Finish the measurement with [Stop].
10. Click on [Accept] to transfer the found parameters for the selected element
line to the method.
In the same way, find the appropriate parameters for all element lines defined in
the method.
Note
There is a small delay between the modifation of the parameters and the signal
response.

8.2.2.2 Automatic flame optimization

Automatic flame optimization is carried out in the Flame –Automatic Optimization
window.
Automatic optimi-
zation tab
Note
If the use of auxiliary oxidant has been chosen in the method, the flame must be
optimized manually.
The used optimization algorithm changes the settings for fuel flow and burner
height with the aim to obtain an increase in the signal level. This algorithm takes
into account the interactions between the two parameters (fuel flow and burner
height). The optimization procedure will be stopped if in three successive steps no
further increase in signal level is achieved. This means that either the maximum
signal level was reached or the change of the parameters is of no effect on the
signal level.
Fig. 37 Flame –Automatic Optimization window
Line Choose the element line for which the flame shall be optimized.
You may choose among the wavelengths defined in the meth-
od.
Position Position of the test sample on the autosampler.
[Start] Starts the measurement. The signal is continuously being rec-
orded.
The button label turns into [Stop].
All lines Perfoms the optimization for all lines of the method with the
sample solution. The sample must contains all analytes.
[Stop] Stops the measurement.
[Delete] Deletes the found values.
[Load] Loads optimized flame parameters.
[Save] Saves optimized flame parameters.
[Accept values] Accepts the found flame parameters for the selected element
line and transfers them to the method.

Table Display of found parameters.

Graph Display of signal curve.
1. Select an element Line from the list or

activate the option All lines.
2. Immerse the tube into the sample solution.
3. Start the optimization using [Start].
The dialog window for the automatic optimization is opened.
4. If appropriate, activate following settings:
Set optimized This setting has to be activated for automatic optimization

values automati- because only the parameters from the last optimization
cally for the cur- are available after the procedure is completed.
rent method
Automatically If activated, enter a file name in the respective field.
save optimiza-
tion data
5. For single line optimization: After successful optimization the parameters can
be transferred to the method by using [Accept values] if the respective set-
ting has not been activated in the start dialog.
8.2.3 Extinguishing the flame

You may extinguish the flame in different ways.
 In the Flame – Control window, click on the [Extinguish flame] button.
Routine / Extin-  Alternatively, you may activate the menu command Routine / Extinguish
guish flame flame.

8.3 Furnace
Selected technique: graphite tube technique
Working in the Furnace window, you are able to check individual graphite tube
furnace functions and make settings for analysis of individual elements.
Method Develop-
 Use a Method Development / Furnace... command or click the
ment / Furnace...
icon to open the Furnace window.
Control buttons in Furnace window

Line A list field for setting an analytical line, for which furnace pa-
rameters are to be displayed or varied.
Use arrow keys to page through the lines list as necessary.
[→Method] Transfers changes in furnace parameter settings for analytical
line to “Method“.
8.3.1 Editing a furnace program

Working in the Furnace – Furnace Program window, a furnace program (temper-
ature-versus-time program (TPZ)) can be created, displayed and edited if neces-
sary for a selected analytical line.
A furnace program may comprise a maximum of 20 working steps.
Furnace Program
tab
Fig. 38 Furnace – Furnace program window
Tabular display
A tabular display will list all working steps which are part of a currently selected
furnace program. The parameters on display are:
Step Sequential number of working step

* No function assigned to this field sofar.

Name Name of furnace program step

Temp Target temperature within step
Ramp Heating rate within step
Hold Holding time of target temperature within step
Time Total duration of working step
Gas Supply of purge gas (Purge.) and additive gas (Add.). Possible
states:
Stop No supply
Min Minimal supply rate (only purge gas)
Max Maximal supply rate
Inj. Injection step.
Sample will be injected into furnace on completion of this step.
E/P Working step for enrichment or thermal pretreatment of individ-
ual components.
Control buttons and input fields

[New] Inserts a new line at the end of a list.
[Insert] Inserts a new line before a marked list place.
[Delete] Deletes marked lines.
[Delete table] Deletes entire furnace program table.
Measuring delay Allows specification of a time delay for acquisition of measuring
signal if required.
By default, acquisition of a measuring signal will begin as the
Atomize furnace program step starts. A time setting will delay
the starting point of signal acquisition by the preset amount of
time. This function is included to allow users to wait with the
triggering of a measurement until the atomization temperature
has actually been reached and remains on a given temperature
plateau.
Copies the parameters in a line to all subsequent lines.
[Cookprogram] Loads the furnace program for a selected analytical line from
the cookbook.
[Check program] Checks the furnace program. If the furnace program is found to
contain errors of a kind that renders program execution impos-
sible, the faulty step will be displayed in a message box. The
program cannot be launched in this case. Correct the faulty
step (or change the furnace program that precedes this step).
As part of a program start, the furnace will be checked for po-
tential thermic overheat situtations (if all basic conditions are
known). If the settings for temperature or time are found to be
excessively high, a “Thermal furnace overheating” " error mes-
sage will appear during the program startup routine – the fur-
nace program will be abandoned in this case. You should then
correct the steps with the highest furnace temperature and the
longest holding time.
[Transfer drying Accepts and transfers the settings made for drying parameters
Step(s)] to the furnace programs for each analytical line.
[Transfer clean- Accepts and transfers the settings made for graphite tube bak-
ing Step(s)] ing to the furnace programs of each analytical line.

Specifying parameters for individual furnace program steps

On selection of an analytical line, a suitable furnace program will initially be loaded
from the cookbook.
 Use the [New], [Insert] or [Delete] control button as necessary to adapt the
current furnace program to your requirements.
 To edit, click a desired one of the table cells.
A list will open in this cell if preselections are limited. Numbers must be edited di-
rectly in the field.
Program steps:
Drying Solvent in sample evaporates

Pyrolysis Performs thermal pretreatment for decomposition of sample
without administration of oxygen.
Ash Performs thermal pretreatment for thermal decomposition of
sample, using a selectively involved type of additive gas (for
example, oxygen supply).
Gas adaption Gas flow is adapted to atomization conditions.
Atomize Sets analytical atoms free.
Clean Removes residual sample matter.
Temperature settings:
Temperature End temperature of this step.

Value range:
Maximal temperature up to 3000°C in steps of 1°C
Minimal temperature not less than 20°C above cooling water
temperature (preferentially 35 °C) of circulation cooler
Ramp The rate of heating intended to achieve target (end) tempera-
ture.
Value range: 1 ... 3000°C/s in steps of 1°C/s; FP (Full Power),
NP (No Power) are possible limit rates.
Hold The time for which a target (end) temperature is to be main-
tained.
Value range: 0 to 999 s less heating time
Time Total duration of a step (sum of heating time plus hold time), is
automatically calculated.
Gas supply
Purge. Flow of protective gas.

Stop No supply, active 2 s before transition to other step
Min Minimal supply rate (0.1 L/min Ar)
Max Maximal supply rate (2.0 L/min Ar)
Add. Flow of additive gas, e.g. air, nitrogen, etc.
Stop No supply, active 2 s before transition to other step
Max Maximal supply rate (0.5 L/min)
Injection step/thermic pretreatment
Inj. If marked with a "*", the particular sample (gas in HydrEA tech-
nique) will not be introduced into the graphite tube before com-
pletion of this step (pipetting into preheated tube).

E/P Only for solution analytics.

Performs enrichment /thermal pretreatment (Enrichment / Pre-
treatment)
In the case of enrichment, the sample will undergo pretreat-
ment to the point of an enrichment step during a measurement
cycle, the tube is then cooled down to room temperature and
the next sample volume introduced by pipetting.
In the case of thermal pretreatment of analytical solution and/or
modifiers, pretreat-ment will be performed up to a specified
step. At the end of this step the graphite tube has to been
cooled down and the sample will be placed into the hot tube.
The number of desired enrichment cycles, the involvement of
modifiers and the type of thermal pretreatment can be specified
in the Furnace – Modif.+Extras window (→ "Matrix modifiers,
selections for enrichment and pretreatment" p. 115).
8.3.2 Matrix modifiers, selections for enrichment and pretreatment

Solution analytics
The Furnace – Modif.+Extras window provides options for specification of the
following parameters:
• Matrix modifiers
• Settings for enrichment
• Settings for thermal sample pretreatment
Fig.39 Furnace - Modif.+Extras window for solution analytics
Selections for modifiers for matrix delimitation and thermal pretreatment must be
made for each specific line. Up to five modifiers can be specified for analysis of a
given element line.

Matrix modifiers
During each measurement, a maximum of five different matrix modifiers can be
added. These can be activated by clicking into the relevant modifier checkbox.
In order to prevent errors due to carryover effects, analytical components are rec-
orded in the following standard order:
• Blank (in case of dilution)
• Modifier 1
• ... further modifiers (if specified)
• Sample solution.
Outputs to the graphite tube occur in reverse order, i.e. the sample will be the first
to be injected. As the other components are being supplied, residual sample matter
will be washed from the dosing tube and injected into the graphite tube. This
standard order of sample (first) and modifiers (then) may be modified if necessary.
Required parameter entries for modifiers are:
Checkbox Activates modifier for analysis.

Name This list field contains the names of typically used modifiers.
Select a name from this list or enter this name directly at the
input field.
Vol. Enter discharge volume (1 to 50 µL) here.
Pos. Specifies position of modifier on sample changer.
to sample Autosampler will pick the particular modifier up, after the sample
was picked up, i.e. the sample will be injected into the graphite
tube before the sample if this box is active.
Pretreat. Sets thermal pretreatment of modifier.
Enrichment
For enrichment, a given furnace program is repeatedly performed until the speci-
fied step is reached (column E/P). As part of each cycle, the sample quantity which
is specified per sample table will be injected and pretreated, the tube is then cooled
to room temperature and the next sample volume is injected. This procedure al-
lows greater sample volumes to be placed into the furnace. Modifier volume is in-
jected only once.
Specificable enrichment modes are:
off No enrichment specified.

Permanent (only Enrichment with each sample (without special samples such as
samples) standards, etc.)
Permanent (incl. Enrichtment with each sample, including standards, QC sam-
calibration) ples and additive standards
if conc. to low Enrichment applies only to samples with a concentration level
lower than that of the detection limit.
Cycles Number of enrichment cycles (2 to 100).
Note: Given that ayn contaminant present inside the tube will
be enriched together with the actual element being analyzed,
the number of enrichment steps defined for actual samples
should be kept reasonably small.

Thermal pretreatment
For thermal pretreatment of analytical solution and/or modifiers, this option will be
executed up to the specified working step of a furnace program. At the end of this
step, the remaining components will be injected into the preheated tube.
Thermal pre- Performs thermal pretreatment of modifiers or a sample if ac-

treatment tive.
To define pretreatment of a Modifier, the related Pretreat
checkbox must be turned on.
Preheat sample Pretreats analytical solution, adds modifiers and other compo-
nents.
Warm up delay Defines waiting time from addition of components to undergo
thermic pretreatment to next components.
Fig. 40 Excample for furnace program with thermal pretreatment
Caution! Thermal pretreatment at temperature not above 300°C!

Make sure you do not select a temperature above 300 °C for a step with thermal
pretreatment. If this rule is disregarded, the tube tip will be destroyed as the re-
maining components are added into the hot tube. There will be no error message
with higher temperatures!
Solid analytics with involvement of SSA 600 solid sampler

With solid analytics, only matrix modifiers may be specified for addition. Once a
modifier has been activated, its name and volume can be defined (same as
above).
For SSA 600 without liquid dosing, modifiers must be manually pipetted onto the
sample. Addition occurs immediately before the platform is placed into the furnace
or as the last step of a full sample preparation cycle performed with the help of an
SSA 600.

For SSA 600 with liquid dosing, a modifier or liquid samples are automatically
pipetted. Up to three modifiers may be specified in this case.
8.3.3 Optimizing atomization temperature

Working in Furnace - Optimization window, you may perform a series of meas-
urements with stepped pattern of increasing settings for step end temperature, in
Optimization tab
order to determine and set the optimal pyrolese and atomization temperature for a
particular element line.
Once optimized, furnace parameter settings for atomization and pyrolese can be
saved and loaded to other methods.
Fig.41 Furnace window:Furnace program tab
Parameters and control buttons

Optimize Selects parameter for optimization: Pyrolyse or Atomization
Step number Shows the number of a selected step ina furnace program.
Start temp.[°C] Sets the lowest end temperatures of a furnace program step to
be optimized as part of a series of measurements
Step size [°C] Designates the step by which the end temperature setting will
be incremented for the furnace program step undergoing opti-
mization.
End Temp. [°C] Highest end temperature of a furnace program step to be opti-
mized as part of a series of measurements.
Note: Available for selection are only such parameters which
make sense for the particular furnace program.
Sampler pos. Position of sample in autosampler
[Start] / [Stop] Starts / terminates optimization.
[Delete ] Deletes obtained values.

[Save...] Saves optimized furnace parameters.

[Load...] Loads optimized furnace parameters.
[Accept] Validates and transfers obtained values into currently selected
furnace program.
Results display
The results of optimization can be displayed in a results window.
Graphic representation is facilitated by Furnace – Furnace program window tools.
Available for displaying are the particular autozero value and the measured extinc-
tion value:
Red line Background signal that depends on pyrolese or atomization

temperature
Blue line Specific absorption depending on pyrolese or atomization tem-
perature
Vertical cursor User-selected optimal pyrolese or atomization temperature
y-scaling If this checkbox was set, y-axis scaling will be such that the
background signal can be depicted in the best possible manner.
An optimized scaling can be separately selected for pyrolese
and for atomization.
[A->H]/[H->A] Switches the graphic between signal area (Area) and signal
height (Height).
[<] / [<] Shifts vertical lines for pyrolese or atomization temperature (de-
pending on what step was selected for optimization) to the left or
the right, thus defining a desired optimal furnace temperature.
Note
The graphic are confirm with presetting in the Option – View window.
Performing optimization
An autosampler is required to perform this series of measurements.
Optimization goal
Pyrolyse temperature: No specific and only minimal non-specific absorption

loss.
Atomization tempera- One single consistent specific extinction.
ture:
 Create a furnace program for a currently selected analytical line.

 Enter optimization settings in the Furnace - Optimization window (optimized
temperature, Start temp.[°C], Step size[°C], End temp. [°C], position of sam-
ple on autosampler).
 Prepare sample on autosampler.
 Click [Start] to trigger optimization.
Optimization will run automatically.
Measured results will be displayed in the results window and represented in
graphical form in the Furnace – Optimization window.
To display individual sample readings, click onto a measurement point of the
graphic or use a double click onto the sample line in the results window.

 Use [<] / [>] control buttons to move the vertical cursor over the graphic area
or use arrow keays as necessary to adjust optimal temperature. Then click
[Accept] to transfer this value into the furnace program.
 Repeat this procedure for all other analytical lines included in the current
method.
8.3.4 Graphical representation of furnace program / graphite tube

coating
The Furnace - Plot window provides the following functions:
• Graphical representation of furnace program
• Monitoring execution of current furnace program
Plot tab
• Coating graphite tube with iridium layer for HydrEA technique
Graphical representation of furnace program

A furnace program is represented as a graph in a temperature-versus-time coordi-
nate grid.
Black line Programmed temperature-versus-time graph

Red line While a test is running, the black line in the already completed
furnace program part is overlaid with a red line designating the
actual temperature-versus-time graph.
Inj. The injection step is marked with an ”Inj.“ identifier above the
diagram.
Green bar An enrichment phase will be marked by a green horizontal bar.
Light pink bar The integration step (measured value acquisition) is marked by a
light pink vertical bar.
Testing furnace program in trial run

Execution of a current furnace program can be tested in a trial run. Its progress will
be graphically represented.
While this trial run is going on, temperature and time values will be displayed, but
no sample will be injected. Similarly, no autozero and integration are performed.

Fig. 42 Furnace – Plot window: Testing furnace program
The plot shows the various steps of a furnace program. The red line indicates the
actual furnace temperature during program execution.
During program execution, the following values are output for digital display:
Step Furnace program step being performed

Temp.[°C] Current furnace temperature
Time [s] Time lapsed since program start
Ramp [°C/s] Current heating rate
Gas Current gas flow
Graphite tube coating

For HydrEA technique, an iridium-coated graphite tube is required. A coating pro-
cess can be controlled via the Furnace - Plot window.

Fig. 43 Furnace – Plot window: Graphite tube coating
Once the Graphite tube coating checkbox is marked, the following input parame-
ters will be enabled for selections to run this procedure.
Cycles Number of enrichment cycles for coating

Position The sample tray position that contains solution for coating
Vol.[µL] Volume of coating solution, which must be pipetted into the tube
for each enrichment step.
[Start] Triggers coating.
8.3.5 Further furnace functions

Available functions in the Furnace - Control window are:
• Information relating to the graphite tube
Control tab
• Graphite tube formation
• Baking (cleaning) of graphite tube
• Opening / closing of graphite tube
• Indication of current cooling water temperature

Fig. 44: Furnace – Control window
Graphite tube data

The Graphite tube subarea contains information items regarding the graphite
tube. This information must be defined when the tube is replaced. Itwill be automat-
ically updated hereafter. On installation of a new tube, you must set all entries to 0.
Type Tube type as per selection in Main settings window

Heat cycles Number of heating cycles of this tube
Lifetime Statistical ratio for thermic strain exposure of graphite tube as a
product of control parameters and step times of currently active
furnace program. This numerical ratio can always be estimated
only for a particular type of workjob.
Note
Before removing a graphite tube which is still in a state fit for operation, you are
recommended to record its operating data from the Graphite tube subarea in or-
der to be able to restore these values for automatic subsequent updating after the
tube has been installed again.
Formatting graphite tube

Graphite tube formatting is performed to:
• force air oxygen out of the furnace and adapt the contract pressure force of
the moving furnace part,
• recalibrate the furnace temperature,
• format a new installed graphite tube,
• clean the furnace after breaks in operation/idle periods.
Situations where furnace formatting is compulsory:

• after power to the spectrometer is turned on

• after closing a previously open furnace.
Factor Formation factor determined as part of formation

[Start] Triggers formation.
The Format tube window will appear. It shows currently
measured furnace data. Nine temperature stages (300 – 1500
– 300 – 1500 – 300 – 1000 – 1600 – 2000 – 2400 °C) are run
and the control temperatures in the inner tube space are
measured. On completion of the last step, the formation factor
will appear and the data obtained for tube temperature recali-
bration will be saved.
Clean furnace
Clean furnace is a single-step cleaning program. It works with a gas rate setting
that is fixed to maximal flow. Current parameter settings which can be modified
here will be saved with the method.
Temp Temperature of baking out (cleaning)

Ramp Heating rate
Hold The time for which baking lasts
[Start] Triggers a baking (cleaning) process, displays the Clean fur-
nace window that reports currently measured furnace date
Further furnace functions

Cooling water Shows current cooling water temperature.
temp. [°C]
Furnace LED / Turns the furnace camera on if active. A special window with a
Furnace graphite tube image will be imposed onto the screen. Sample
injection can be monitored.
The furnace camera is delivered with permanently On preset-
ting. The option to influence this setting is part of the Options
– Analysis sequence window (→ "Options for analysis se-
quence" p. 17).
[Open furnace] Opens the graphite tube furnace
Graphite tube can be retrieved or installed.
[Close furnace] Closes the graphite furnace tube.
[Reset furnace]
Temperature for The temperature level that will cause the shutter before the
opening shutter receiver to be opened.
The furnace camera is turned off at this point and the process
of measured value acquisition is prepared.
Test furnace
Checks the furnace for sensor errors. A measurement will be aborted on occur-
rence of an error situation listed here (with a corresponding error message output
to the screen).
To trigger an error test, click [Test]. On successful completion of testing, the result
will be reported by a green control lamp, on unsuccessful completion by a red con-
trol lamp.

8.4 Hydride system

Selected technique: Hydride and HydrEA technique
In the Hydride system window, you can:
• Check the state of the hydride system
• Test various functions of the system for errors
• Re-initialize the hydride system
• Load the system tubes with reagents before starting the analysis
• Rinse the system, e.g. for cleaning at the end of the analysis
 Open the Hydride system window using menu command Method Develop-
ment / Hydride... or the icon button
Method Develop-
ment / Hydride... .
Buttons in Hydride system window

[Initialize] Initializes the hydride system.
[Load system] Loads the tubes of the hydride system with reagents.
Loading of reagents is necessary before the analyses are start-
ed, after re-installation or after cleaning of the hydride system.
[Clean system] Rinses the hydride system with acid (or with reductant).
The corresponding parameters are to be entered in the Method
– Hydride window (→ "Hydride tab – Specifying the hydride
system", p. 27.
8.4.1 Control of hydride system functions

The Hydride system – Control window displays the state of the individual, control-
lable modules of the hydride system.
Fig. 45 Hydride system - Control window

Pump control
Components Switches the components pump on/off.

pump The components pump delivers the reagents of the hydride
system.
Sample pump Switches the sample pump on/off.
The sample pump delivers the liquid sample to be analyzed.
Note
If on switch on of one of the two pumps none of the two valves 3 or 4 is active,
valve 3 will be switched on automatically to prevent the liquid from flowing back.
If the sample pump is being active, the components pump will be activated, too, to
avoid liquid impoundage in the gas/liquid separator.
Control of gas paths

In the Gas path field, you can switch all ten paths of the argon gas flow that are
useful for the analysis procedure by means of solenoid valves (solenoid valve as-
semblies).
For gas paths that do not lead to the cell, you can additionally switch a large gas
stream directly to the cell by activating the Gas->Valve 2 -> Cell check box. In do-
ing so, valve 2 is opened.
Switching of sample valves

In the Sample valves field, the sample path can be switched to either the waste
bottle or the reactor by means of the solenoid valve pair (V6, V7).
Valves in gas flow

Valve 1 switches the gas flow through the tip of the batch module on and off.
Valve 3 switches argon to the set path.
Valve 4 switches argon to the set path.
Control of cell
Cell height Adjustment of cell height in the light path.

Heating on Switches the cell heating on.
The cell is heated to the temperature adjusted in the Target
input field.
After switching on and off of the cell heating, the temperature
value is displayed in the Actual field.
This function can be used for pre-heating the cell.
Heating the gold collector

Only HS 60A and HS 55A
In the Collector field, the adjustment of the gold collector is displayed and can be
varied.
Off Switches heating and cooling of gold collector off.

Heating on Switches the heating of the gold collector on.
Cooling on Switches the fan of the gold collector on.
The gold collector is cooled down.

Heat value Parameter for the bake-out temperature of the gold collector.
The value is factory-adjusted. It should not be varied unless the
thermal behavior of the gold-collector heating has changed. A
higher value corresponds to a higher temperature.
[Set] Saves the displayed heat value as new value in the hydride
system.
Clean bubble sensor

Only HS60A and HS60
The bubble sensor detects liquid in the gas path after the gas-liquid separator. If
this malfunction has been signaled by the bubble sensor during the hydride system
error test or during the measurement the gas way at the bubble sensor has to be
flushed with additional gas flow. The cleaning procedure is successful if no bubbles
are detected in the gas path for 30 s.
control lamp Only active during the cleaning process.

Bubble-Sensor red Bubbles (liquid) have been detected in the gas path.
green The gas path is free from bubbles.
[Start] Start cleaning procedure.
8.4.2 Testing the hydride system for errors

In the Hydride system – Error test window, you can test the current status of the
hydride system. If one of the error states listed in this window appears, every anal-
ysis procedure will be stopped instantly and the corresponding error message dis-
Error test tab
played on the screen.
Fig. 46 Hydride system – Error test window
Connected hydride system
Type Connected and initialized hydride system.

Version Version of hydride system firmware.

Line frequency The measured line frequency, 50 or 60 Hz, is displayed. Positi-

ve and negative deviations of 2 Hz will be tolerated; otherwise,
the error message "Line frequency" will be displayed.
Error test
The result of the test is indicated by green (for a successful test) and red (test
failed) pseudo LEDs:
To start the error test, click on the [Test] button.
A negative test result may have the following causes:
Gas pressure Required argon gas pressure not supplied.

+24 V +24 V operating voltage not applied.
Safety relay Safety relay has not switched.
Transformer Transformer is too hot or the sensor defective.
temperature
Collector tem- Gold collector is too hot or the sensor defective.
perature
Gold collector Failure in setting the rated gold collector temperature.
heating time
Cell tempera- Cell is too hot or the thermocouple defective.
ture
Cell heating Failure in setting the rated cell temperature.
time
Line frequency Line frequency is neither 50 nor 60 Hz.
Waste bottle Waste bottle is full.
Bubble sensor Liquid (bubbles) have been detected in the gas path after the
gas-liquid separator.
Cell tempera- The cell temperature sensor is defect.
ture sensor

8.5 Autosampler
8.5.1 Autosampler AS 51/52s
The autosampler is an optional accessory. You may use device-bound au-
tosamplers depending on the operating mode of the spectrometer and your specific
Method Develop- analytical needs. The type of involved autosampler is identified by ASpect LS as
ment / part of an initialization routine.
Autosampler... In the Autosampler window,
• the connected autosampler model is displayed,
• the autosampler can be adjusted,
• the autosampler can be additionally rinsed / initialized again,
• various functions can be tested.
The parameters directly relevant to the analysis (charging of sample tray, dilution,
mixing and wash steps) are to be specified in the method, the sequence and the
sample identification data.
 Open the Autosampler window using menu command Method Development
/ Autosampler... or the icon button
Control buttons in autosampler window

[Initialize] Reinitializes the autosampler.
As a general rule, the autosampler is initialized at the beginning
of each AAS working session via the Preliminary settings win-
dow (→ "Preparatory settings - Choosing the analytical task" p.
11). It may be necessary to re-initialize the autosampler, if it lost
its orientation (e.g. because you pushed against it). Communi-
cation between the autosampler, the AAS and the PC will be
established.
[Wash] Rinses the cannula of the autosampler.
If the SFS 6 Injection Switch is used, the sample path is opened
and thus the complete sample path rinsed, too. The rinse pump
is continuously delivering fresh wash solution.
Caution! Connect autosampler only to AAS in deenergized state!

Do not connect the autosampler when the AAS is in power-on condition. Failure to
comply may result in faulty communication of even destruction of the interface.
8.5.1.1 Specify autosampler AS 51/52s

The Autosampler – Parameters window provides setting options and display
functions for the following autosampler parameters:
• Autosampler type
Parameters tab • Washing parameters

• Setting options for controlled cleaning
• Function for mixing cup washing

The parameters for washing and controlled cleaning are taken from the currently
loaded method (→ "Auto sampler for flame and Hydride/HydrEA technique" pg.
32). Conversely, however, changes to the parameters made on the Autosampler
– Parameters tab, are of no influence on the entries in the method.
Fig. 47 Autosampler – Parameters window
Autosampler type
Type Selection / display of the connected type of autosampler

"-" No autosampler selected.
AS 51s Autosampler for flame, hydride, and HydrEA tech-
nique without dilution function
AS 52s Autosampler for flame, hydride, and HydrEA tech-
nique with dilution function
Tray "-" No tray attached
87 Pos Sample tray with 77 sample positions for 15 mL Sar-
stedt cups on the outer track and 10 sample posi-
tions for 30 mL Sarstedt cups on the inner track
49 Pos Sample tray with 49 sample positions for 30-mL-
Sarstedt sample cups on three tracks
30 Pos Sample tray with 30 positions for 50 mL Sarstedt
sample cups on 3 tracks
Version Version number of autosampler software.
Wash
Wash mode off Wash mode switched off. No rinsing performed au-
tomatically.
tistical series.
Wash time Wash Time in which the rinsing agent is aspirated in the wash cup.
cup
Mixing cup cy- Number of rinse cycles for the mixing cup.
cles In a rinse cycle the mixing cup is filled with wash liquid / diluent
and then emptied again.

Controlled cleaning
Controlled clean- Carry out a cleaning wash.

ing The cleaning progress is checked by repeated measurement.
(Abs.) rinsing, before the diluted samples / samples of lower concentra-
tion are analyzed.
Special functions
Wash mix cup Wash mix cup separately outside a sequence measurement.
Volume Enter volume for cleaning.
Start Wash mixing cup.
8.5.1.2 Technical parameters of the autosampler AS 51/52s

The Autosampler – Techn.Parameters window allows you to specify:
Techn. Parame-
• depth of submergence of cannula / dosing tube into the various cups
ters tab • working speed of dosing unit
• alignment of autosampler arm in relation to sample cups
Fig. 48 Autosampler – Techn. Parameters window tab for AS 52s
For the individual cup types the following actions are taken into account:
Cup Action
Sample cup Take up of sample by dosing unit or aspiration by nebulizer
(flame technique) or peristaltic pump (hydride technique).
Special cup Take up or aspiration of special samples.
Mix cup Dosing volume of analyte and diluent, as well as take up of sam-
ples after dilution.
Wash cup Rinsing of cannula and aspiration path (only with flame and hy-

dride technique).
Elements of the table
Action Available action options:

Take up – Takes up sample from cup for dispensing into mixing
cup or flame.
Dispense - Dispenses sample into mixing cup
Wash - Takes up wash solution
Type Connected autosampler model
Location Cup to which a given action refers.
Depth The depth to which the cannula submerges in units of 1 mm
Speed Designates the working speed of the dosing unit. Greater values
Level cause the dosing unit to work faster, with smaller values it will
work more slowly. Recommended values:
Take up of samples Medium speed levels
Dispense into mixing cup One of the two highest levels, so
that the fast injection leads to a complete mixing. Be-
sides, the complete mix up is supported by a fixed
wait time before the take up from the mixing cup (or
sample cup).
The take up of diluent and the separating air segment are carried
out at fixed speed.
Table subarea
Using the controls in the Table field, you can change the parameters of the select-
ed table row.
Speed Speed of dosing unit

Depth [mm] Set immersion depth of cannula / dosing tube.
The immersion depth is measured from the highest position of
the sampler arm.
Depth at pos. Position of special or sample cup at which the immersion depth is
measured.
Set If activated, the sampler arm moves over the cup for which the
positioning has to be adjusted. With sample and special cups,
this is the position selected under Depth at pos.
If not activated, the immersion depth and speed are changed
without the sampler arm moving above the cup.
8.5.1.3 Setting insertion depth and dosing speed for AS 51/52s

 On the Autosampler – Techn. parameters tab, mark the table row, the pa-
rameters of which you want to change.
Techn. Parame-
ters tab
 For the specification of sample and mixing cups, in the Depth at pos. field, set
the position on the tray, at which you want to test the immersion depth.
 Activate the Set check box to move the sampler arm to the specified cup posi-
tion.
 Watch the movement of the sampler arm and vary the Speed and Depth until
you achieve the desired result.

8.5.1.4 Functional test of the autosampler AS 51/52s

On the Autosampler – Function tests tab, you may test the functions of the au-
tosampler.
Function test tab
Fig .49 Autosampler – Function tests window
Tracker/Rotator
Driving the sampler arm to the various positions:
Cup No. Drives to the cup position selected from the corresponding list
box.
Wash position Drives to the wash cup.
Mixing position Only for AS 52s
Drives to the mixing cup
Pipetter
Only AS 52s
Speed Adjust the pipetter speed.

Volume [µL] Adjust the pipetting volume to be taken up.
Valve to bottle Switches the valve to the bottle.
The valve switches the flow between the diluent bottle and the
sample. In switching, you must hear the valve click.
[Take up] Take up the selected volume with the currently selected pipetter
speed.
[Dispense] Dispense the selected volume with the currently selected pipet-
ter speed.
[Reset] The volume taken up is dispensed again.
Dipping arm
Lowering the sampler arm at the position selected under Tracker/Rotator.
Depth Adjust the depth by which the sampler arm can be lowered.

Pumps
Wash pump Start the pump for supply from wash cup.
Mixing cup Starts the pump for pumping out the mixing cup.
pump
Test programs
Tests are provided to test the autosampler with pre-configured, dry running test
programs. The cups the sampler arm is driven to during the test must be empty!
When the test programs are finished, you are informed of the test success.
Start the selected test program with the button [Start]
Test program 1 Driving to Position 1 and immersing in cup

Rinsing of cannula
Driving to Position 33 and immersing in cup
Rinsing of cannula
Driving to Position 42 and immersing in cup
Rinsing of cannula
Test program 2 Execution of Test Program 1
Dispensing 5 mL diluent in mixing cup
Rinsing of cannula
Drains mixing cup
Dispensing 5 mL diluent in mixing cup
Rinsing of cannula
Drains mixing cup
Button [Adjust sampler]

Adjust the autosampler AS 51/52s (→ section "Adjust autosampler AS 51/52s" pg.
135).
Error test
These tests serve to test the autosampler for sensor errors. If one of the error
states listed here appears, every measurement will be aborted (on the screen a
corresponding error message will be displayed).
The error test is started with the [Test] button. If the test was successful, the indi-
cator will light green; if the test fails, it will light red.
If a test fails, this may have the following causes:
Wash bottle lev- Reports excessively low fill level of storage bottle (bottle emp-
el ty).
Diluent bottle Reports excessively low fill level of storage bottle (bottle emp-
level ty).
Tracker/Rotator Swivel drive of sampler arm and rotary drive of tray are defec-
tive.
Tray identifica- Sample tray not detected.
tion
Pipettor (drive) Dosing pump error.
Pipettor (vol- The volume taken up by the pipettor was too large.
ume)
[Adjust sampler] Opens the Adjust sampler dialog for readjustment of the au-
tosampler.
(→ section "Adjust autosampler AS 51/52s" pg. 135)

8.5.1.5 Adjust autosampler AS 51/52s

The autosamplers are supplied factory-adjusted.
Function test tab

An adjustment must be carried out in exceptional cases (e.g. following inappropri-
ate transport), if the sampler arm no longer immerses centrally in the cups. Read-
justment is carried out computer-controlled in the Adjust sampler dialog (accessi-
ble via the [Adjust sampler] button on the Autosampler – Functional Test tab).
Fig.50 Adjust sampler dialog for AS 52s
Selecting the position to be adjusted
Mixing position Alignment of sampler arm to mixing cup

Tray position 1 Alignment of sampler arm to sample cup on position 1 of the
autosampler tray
Alignment of mixing position/tray position 1
Depth Dipping depth in mm. With this field, the dipping arm can be
driven into or out of the particular cup. The immersion depth for
Mixing position and Tray position 1 is no optimizable parame-
ter. The possibility of changing the depth only serves to facilitate
assessing the cup center.
Dipping arm Buttons for changing the sampler arm position. Alternatively,
[]/[] you may press arrow keys "Arrow right" and "Arrow left" on the
PC keyboard.
Sampler tray Buttons for rotating the sampler tray. Alternatively, you may use
[]/[] the arrow keys "Arrow up" and "Arrow down" on the PC key-
board.
[Save] Saves the new parameters for the selected position. The set-
tings remain valid until you save new adjustment states.
Wash pump
Only samplers with newer firmware versions
Level Adjust wash pump speed level (levels 1-24).

[Save] Save wash pump speed.

Adjusting the autosampler

1. Place a sample cup on position 1 of the sampler tray.
2. In the Adjust sampler dialog, choose the position to be adjusted first.
3. Adjust the immersion depth in a way that the position of the sampler arm rela-
tive to the cup can be well assessed.
4. Adjust the position of the sampler arm with the buttons.
Additionally for tray position 1: Adjust the position of the sample tray with the
buttons.
5. Save the new parameters in the firmware of the autosampler by clicking on
[Save].
6. Then, repeat the above steps for the other position.
8.5.1.6 Position overview in the autosampler AS 51/52s

The sample tray positions used in the current sequence are displayed in window
Autosampler – Position.
Positions tab
The display modes All positions or Only special positions can be selected.
8.5.1.7 Supply of reagents for sample

In the window Autosampler – Reagent-Addition a reagent can be pipetted auto-
matically to the samples by using the autosampler AS 52. The reagent must be
Tab reagent sup- kept ready in a sample cup on the sample tray.
ply
Fig. 51 Autosampler – Reagent addition window
1. Enter the following parameters for the reagent:
Name Designation of the reagent

Position Position of reagent on the sample tray.

Volume [µL] Volume of the reagent which is to be supplied to the sam-

ples.
Consider factor If activated the dilution factor is taken into consideration by
the addition of the reagent.
2. Initialize the sample list with [Init. list].

3. In the sample list enter the analyte volume of the samples.
4. Mark all samples which are to have reagent added with "*".
5. Start the addition of the reagent with [Start add.].
8.5.2 Micro pipetter unit MPE 60

The micropipetter unit MPE 60 is used as an autosampler in the graphite tube and
hydrEA technique. There are two versions of the micropipetter unit:
Method Develop- • MPE 60 – autosampler for the graphite tube technique with mixing cup
ment / Au-
tosampler... • MPE 60/1 – autosampler without mixing cup
The type of involved autosampler is identified by ASpect LS as part of an initializa-
tion routine.
In the Autosampler window,
• the connected autosampler model is displayed,
• the autosampler can be adjusted,
• the autosampler can be additionally rinsed / initialized again,
• various functions can be tested.
The parameters directly relevant to the analysis (charging of sample tray, dilution,
mixing and wash steps) are to be specified in the method, the sequence and the
sample identification data.
 Open the Autosampler window using menu command Method Development
/ Autosampler... ... or the icon button

of each AAS working session via the Preliminary settings win-
dow (→ "Preparatory settings - Choosing the analytical task" p.
11). It may be necessary to re-initialize the autosampler, if it lost
its orientation (e.g. because you pushed against it). Communi-
cation between the autosampler, the AAS and the PC will be
established.
[Wash] Rinse MPE. Rinsing liquid is pumped through the sample tube
via the dosing device and dispensed in the wash cup.


8.5.2.1 Specify autosampler MPE 60

The Autosampler – Parameters window provides setting options and display
functions for the following autosampler parameters:
Parameters tab
• Autosampler type
• Washing parameters
• Setting options for controlled cleaning
• Function for mixing cup washing
The parameters for washing and controlled cleaning are taken from the currently
loaded method (→ "Autosampler for graphite tube technique (solution analytics)"
pg. 35). Conversely, however, changes to the parameters made on the Au-
tosampler – Parameters tab, are of no influence on the entries in the method.
Fig. 52 Autosampler – Parameters window for MPE 60
Autosampler type
Type Selection / display of the connected type of autosampler

"-" No autosampler selected.
MPE 60 Autosampler for graphite tube technique
Tray "-" No tray attached
89 Pos Sample tray with 77 place capacity for 2 mL sample
cups, 4 special sample places of 5 mL sample cup
volume each and 8 special sample places of 2 mL
sample cup volume each
Version Version number of autosampler software.
Wash modes
Wash mode off Wash mode switched off. No rinsing performed automat-
ically.
tistical series.
between runs Washes after each measurement, including
within a statistical series.

between components The autosampler is washed af-

ter transfer of each component into the graphite tube
(modifier, standard, sample, etc.).
Wash cycles Number of wash cycles per wash, 1 to 5
Wash cup
again in one cycle.
Controlled cleaning
Controlled clean- Carry out a cleaning wash.

ing The cleaning progress is checked by repeated measurement.
(Abs.) rinsing, before the diluted samples / samples of lower concentra-
tion are analyzed.
Special functions
Wash mix cup Rinse mixing cup separately outside the measurement.
Volume Enter volume for cleaning.
Start Wash mixing cup.
8.5.2.2 Technical parameters of the autosampler MPE 60

The Autosampler – Techn.Parameters window allows you to specify:
Techn. Parame-
• depth of submergence of cannula / dosing tube into the various cups
ters tab • working speed of dosing unit
• alignment of autosampler arm in relation to sample cups
• the automatic depth adjustment for volume decrease during the analysis
• the alignment of the MPE 60 to the graphite tube furnace.
Fig. 53 Autosampler – Techn. Parameters window tab for MPE 60

For the individual cup types the following actions are taken into account:
Cup Action
Sample cup Take up samples through doser.
Special cup Take up special samples.
Mix cup Dosing volume of analyte and diluent, as well as take up of
samples after dilution.
Wash cup Rinsing of cannula.
Graphite tube Inject sample or special sample into the graphite tube.
Elements of the table
Action Available action options:

Take up – Draws in sample from sample cup, special cup or
mixing cup.
Dispense - Dispenses sample into mixing cup
Inject - Inject sample or special sample into the graphite
tube.
Type Type of connected autosampler
Location Cup to which a given action refers.
Depth The depth to which the cannula submerges in units of 1 mm
Speed Designates the working speed of the dosing unit. Greater val-
Level ues cause the dosing unit to work faster, with smaller values it
will work more slowly. Recommended settings:
Sample take-up 3
Dispensing to mixing cup 9
Injection into graphite tube 1
Table subarea
Using the controls in the Table field, you can change the parameters of the select-
ed table row.
Speed Speed of dosing unit

Depth [mm] Set immersion depth of cannula / dosing tube.
The immersion depth is measured from the highest position of
the sampler arm.
Depth at pos. Position of special or sample cup at which the immersion depth
is measured.
Set If activated, the sampler arm moves over the cup for which the
positioning has to be adjusted. With sample and special cups,
this is the position selected under Depth at pos.
If not activated, the immersion depth and speed are changed
without the sampler arm moving above the cup.
Automatic depth correction
Automat. depth Automatically adapts the depth, to which the dosing tube will
correction submerge into sample or special cups, to a new volume.

[Sample cups] Only active if Automat. depth correction is active.

Opens the Sampler position, volumes and depths window to
allow settings for non-standard container geometries and vol-
umes of individual cups. These settings will be taken into ac-
count for automatic depth correction (→ "Automatic depth cor-
rection for MPE 60" pg. 141).
MPE alignment
[Align MPE to On selection of this control button, the screen-driven procedure

Furnace] for alignment of the MPE in relation to the graphite tube furnace
will be triggered (→ "Aligning MPE 60 to graphite tube furnace"
pg. 143).
[Open fur- Open and close furnace.
nace]/[Close fur-
nace]
8.5.2.3 Set insertion depth and dosing speed of the MPE 60

 On the Autosampler – Techn. parameters tab, mark the table row, the pa-
rameters of which you want to change.
Techn. Parame-
ters tab
 For the specification of sample and mixing cups, in the Depth at pos. field, set
the position on the tray, at which you want to test the immersion depth.
 Activate the Set check box to move the sampler arm to the specified cup posi-
tion.
 Watch the movement of the sampler arm and vary the Speed and Depth until
you achieve the desired result.
8.5.2.4 Automatic depth correction for MPE 60

The purpose of automatic correction of the depth level to which the dosing tube will
submerge into a sample cup or a special cup is to prevent unwanted contamination
Techn. Parame- of the dosing tube. To draw in a sample volume, the dosing tube will dip into a
ters tab sample cup just as much as necessary to accomplish this. As total volume removal
increases, the immersion depth will automatically be corrected.
The Autosampler – Techn. Parameters window contains immersion depth set-
tings for sample cups and special cups that will initially apply to any cup on the
sample tray.
Fill volumes or cup sizes at variance with standard cups can be separately speci-
fied and duly considered for automatic depth correction.
 Activate the Automat. depth control checkbox in the Autosampler – Techn.
Parameters window.
 Actuate [Sample cups].
The Sampler positions, volumes und depths window will show.

Fig. 54 Positions, volumes and depths window for MPE 60
With regard to individual special cups or sample cups, the following parameters
can be specified:
Position Set cup position on the tray, for which the three displayed val-
ues: volume, depth and diameter apply. Settings must be made
individually for each cup that is intended to be modified.
Volume Displays the amount of sample volume already retrieved from a
cup or allows input of lacking sample volume balance into a cup
not completely filled.
This reading is software-updated after each sample take-in se-
quence.
Depth Displays the amount of additional depth due to overall sample
withdrawal up to this moment.
This value is recalculated after each sample take-in sequence.
Total immersion depth is the sum of a specified immersion
depth (Depth column on Techn. Parameters tab) and the addi-
tional depth shown here.
Diameter Indicates the cup diameter.
This value is used as input for calculation of the depth, based
on the amount of withdrawn volume.
Diameter For cups with dimensions at variance against those of standard
checkbox cups.
Allows you to specify a diameter for each cup individually if
marked.
[Delete vol- Resets volume values for all special cups or sample cups to 0.
umes]
[Reset] Resets all volumes and the depth values of all cups to 0, resets
diameters to their latest via [OK] saved values.
Maximum dipping depth (auto correction)

A maximum allowed immersion depth can be specified in order to prevent the dos-
ing tube from hitting the cup bottom and getting twisted.

Sample cups Applies settings for maximal immersion depth to sample cups if
marked.
Special cups Applies settings for maximal immersion depth to special cups if
marked.
Depth [mm] Defines the maximal allowed immersion depth of the au-
tosampler into a sample cup or special cup.
Caution:Please note that the autosampler will at once dip
down to the new depth level if the Set checkbox is marked!
Make sure that the autosampler motion path is not blocked.
A modified setting for immersion (dipping) depth should be
saved with [Save].
Position The sample tray position in which immersion depth settings are
checked.
Set The dosing tube will dip into a cup that was specified via Posi-
tion and to a depth that was set via Depth [mm]. The immer-
sion depth can be visually checked. Caution:When the check
box Adjust is marked, the autosampler will be dipped immedi-
ately to the given depth! Make sure that the autosampler mo-
tion path is not blocked.
8.5.2.5 Aligning MPE 60 to graphite tube furnace

The process for MPE alignment in relation to the graphite tube furnace with subse-
quent setting of dosing tube immersion depth into the graphite tube is program-
Techn. Parame- guided.
ters tab
 Actuate [Align MPE to furnace] in Autosampler – Techn. Parameters win-
dow.
 Follow further instructions on the monitor screen.
1 Alignment screw 1
2 Counterlocking nut
of alignment screw 1
3 Alignment screw 2
4 Adjustment aid with
crosshair
5 Autosampler arm
6 Alignment screw 3
7 Counterlocking nut
of alignment screw 3
Fig. 55 Alignment of autosampler MPE 60

8.5.2.6 Function test of autosampler

On the Autosampler – Function tests tab, you may test the functions of the au-
tosampler.
Function test tab
Fig. 56 Autosampler– Function tests window
Tracker/Rotator
Driving the sampler arm to the various positions:
Cup No. Drives to the cup position selected from the corresponding list
box.
Wash position Drives to the wash cup.
Mixing position Move the mixing cup (for MPE 60).
Tube position Move graphite tube.
Pipetter
Speed Adjust the pipetter speed (→ "Set insertion depth and dosing
speed of the MPE 60" pg. 141).
Volume [µL] Adjust the pipetting volume to be taken up.
Valve to bottle Switches the valve to the bottle.
The valve switches the flow between the diluent bottle and the
sample. In switching, you must hear the valve click.
[Take up] Take-up the selected volume with the currently selected pipetter
speed.
[Sispense] Dispense the selected volume with the currently selected pipet-
ter speed.
[Reset] The volume taken up is dispensed again.
Dipping arm
Lowering the sampler arm at the position selected under Tracker/Rotator.
Depth Adjust the depth by which the sampler arm can be lowered.

Pumps
Wash pump Start the pump for supply from wash cup.
Mixing cup pump Starts the pump for pumping out the mixing cup.
Test programs
Tests are provided to test the autosampler with pre-configured, dry running test
programs. The cups the sampler arm is driven to during the test must be empty!
When the test programs are finished, you are informed of the test success.
Start the selected test program with the button [Start]
Test program 1 Aspirates volume from position 1

Aspirates volume from position 41
Discharges volume into graphite tube
Washes dosing tube two times
Test program 2 Aspirates diluent solution from waste bottle
Aspirates volume from position 10
Discharges volume into mixing cup
Aspirates volume from mixing cup
Discharges volume into graphite tube
Washes dosing tube
Drains mixing cup
Washes and drains mixing cup
Error test
These tests serve to test the autosampler for sensor errors. If one of the error
states listed here appears, every measurement will be aborted (on the screen a
corresponding error message will be displayed).
The error test is started with the [Test] button. If the test was successful, the indi-
cator will light green; if the test fails, it will light red.
If a test fails, this may have the following causes:
Wash bottle level Reports excessively low fill level of storage bottle (bottle emp-
ty).
Waste bottle lev- Fill level of waste bottle is too high (bottle is full).
el
Tracker/Rotator Swivel drive of sampler arm and rotary drive of tray are defec-
tive.
Tray ident. Sample tray not detected.
Pipetter (drive) Dosing pump error.
Pipetter (volume) The volume taken up by the pipettor was too large.
Button [Adjust sampler]

With [Adjust autosampler] the positioning of the autosampler arm to the various
cups of the autosampler is adjusted (→ "Adjusting the MPE 60" pg. 146).

8.5.2.7 Adjusting the MPE 60

The autosamplers are supplied factory-adjusted.
Techn. Parame-
An adjustment must be carried out in exceptional cases (e.g. following inappropri-
ters tab
ate transport), if the sampler arm no longer immerses centrally in the cups. Read-
justment is carried out computer-controlled in the Adjust sampler dialog (accessi-
ble via the [Adjust sampler] button on the Autosampler – Functional Test tab).
Fig. 57 Adjust autosampler window for MPE 60
Selecting the position to be adjusted
Mixing position Alignment of sampler arm to mixing cup

Tray position 1 Alignment of sampler arm to sample cup on position 1 of the
autosampler tray
Washing depth Insertion depth into the cleaning cup
Alignment of mixing position/tray position 1
Depth [mm] Dipping depth in mm. With this field, the dipping arm can be driv-
en into or out of the particular cup. The immersion depth for Mix-
ing position and Tray position 1 is no optimizable parameter.
The possibility of changing the depth only serves to facilitate
assessing the cup center.
Dipping arm Buttons for changing the sampler arm position. Alternatively, you
[]/[] may press arrow keys "Arrow right" and "Arrow left" on the PC
keyboard.
Sampler tray Buttons for rotating the sampler tray. Alternatively, you may use
[]/[] the arrow keys "Arrow up" and "Arrow down" on the PC key-
board.
[Save] Saves the new parameters for the selected position. The settings
remain valid until you save new adjustment states.
Adjustment of depth in the washing cup
Depth [mm] Depth of submergence into wash cup in units of 1 mm.

[Save] Saves immersion depth in wash cup.

Adjusting the autosampler

1. Place a sample cup on position 1 of the sampler tray.
2. In the Adjust sampler dialog, choose the position to be adjusted first.
3. Adjust the immersion depth in a way that the position of the sampler arm rela-
tive to the cup can be well assessed.
4. Adjust the position of the sampler arm with the buttons.
Additionally for tray position 1: Adjust the position of the sample tray with the
buttons.
5. Save the new parameters in the firmware of the autosampler by clicking on
[Save].
6. Then, repeat the above steps for the other position.
8.5.2.8 Position overview of the MPE 60

The sample tray positions used in the current sequence are displayed in window
Sampler – Position.
Positions tab
The display modes All positions or Only special positions can be selected.

8.5.3 Solid autosampler SSA 600

To run automated solid analytical procedures, the SSA 600 is applied. The type of
involved autosampler is identified by ASpect LS as part of an initialization routine.
Method Develop- The Solid sampler window provides functions as follows:
ment / • SSA 600 function test
Autosampler...
• Alignment of SSA 600 to graphite tube furnace
As the solid autosampler SSA 600 can be operated with and without liquid dosing,
the functional test and the adjustment are aligned to the autosampler specified in
the method.
 Open the Methods window with the symbol .

Select any analysis line on the Lines tab and activate the option SSA 600 with
automatic liquid pipetter on the tab Sample supply
Activate settings with [Accept].
 Use a Method Development / Autosampler... menu command or click the
icon to open the Solid sampler ... window.

[Reset] Take up sample platforms which are on various positions of the
autosampler and transport back to the sample tray.
of each AAS working session via the Main settings window (→
"Preparatory settings - Choosing the analytical task" pg. 11). It
may be necessary to re-initialize the autosampler, if it lost its
orientation (e.g. because you pushed against it). Communication
between the autosampler, the AAS and the PC will be estab-
lished.
[Align] Triggers a routine to align the SSA 600 to the graphite tube fur-
nace.

Sample preparation items which are different from those in solution analytics (de-
termination of sample platform deadweight, dosing and weighing of sample) can be
specified on the Solid tab of the result window (→ "Solid tab" pg. 81).

8.5.3.1 Function test of solid sampler

Working in the Solid Sampler – Function test window, you may check individual
functions.
Function test tab
Fig. 58 Solid sampler– Function test window
Status / Buttons Displays SSA 600 status and button that was actuated since the
latest query in appropriate color (green, orange, red).
Using [Update], the status can be queried again and the button
display be updated.
Move to posi- Performs motion to the position selected via the Pos. list field.
tion Thus no platform is taken up or put down.
Rotate tray Rotates the sample tray into a selected position.
Transport Means that SSA 600 transports a platform from a given position
to the next starting and target position.
If Take-up platform is activated, the gripper will pick up a plat-
form.
If Put-down platform is activated, the gripper will place a plat-
form down in its target location.
Gripper Opens or closes the gripper.
Lower cannula Moves the cannula downwards.
Balance Determines the weight of a platform in a specified position on
the tray (Pos.)
Weighing with tare
Before a platform can actually be weighed, the scale
must be tared. #1 indicates the tared weight. #2 con-
tains the weight of the platform (also with dosed
sample as may be the case).
[Internal calibration]
During a calibration cycle of this type, the internal
calibration graph of the scales is redetermined.
To achieve this, the scales are initially reset, their
zero-point is determined and an internal weight is
weighed. The values obtained for zero-point and in-
ternal weight will provide the input for determination

of the scales calibration graph.

Loop The autosampler transports two platforms (positions 1 and 2) in
both directions between the sample tray, the scales and the
furnace. The number of transporting cycles can be specified via
the Cycles input field.
8.5.3.2 Alignment of solid sampler

The Solid Sampler / Alignment window provides functions as follows:
Adjustment tab
• Control and adjustment of motion to individual autosampler positions
• Adjustment of the SSA 600 to the position of the graphite tube furnace
• SSA 600 with dosing unit: Automatic depth correction for taking in matrix
modifiers and special liquid samples.
• Test of liquid dosing
Fig. 59 Solid sample r– Adjustment window
Positions to ad- Selection of the position on the autosampler

justed
Buttons in group Alignment of the gripper to the set adjustment position
Adjust Position
[Open grip- Open and close gripper with software control, e.g. for changing
per]/[Close grip- the gripper tips.
per]
[Lower cannula] For liquid dosing
Lower cannula.
Group Automatic Settings for the automatic depth adjustment for the liquid dosing
Depth Adjust-
ment
[Wash] Wash dosing tube with the pre-set and with confirmed
number Wash cycles.

[Test liquid dos- Check liquid dosing.

ing]
[Change dosing Moves the piston of the dosing device downwards in order to
syringe ] enable changing the dosing device.
Monitoring & aligning individual positions

1. Select a desired position from the Position to adjust list.
2. Click [Move to] in Align position group, in order to move the autosampler to
the selected position. Put a platform up in this position and check the position
of the platform.
3. Use control buttons in this group to make positional corrections as necessary.
4. Save all modified setting by clicking the related [Save] button.
Align gripper to the graphite tube furnace

The adjustment aids matched to the furnace type are used for the adjustment of
the gripper to the graphite tube furnace.
The adjustment is controlled by software and it is started with [Align] in the au-
tosampler window.
There is a detailed description in the "Solid Autosampler SSA 600" operating in-
structions.
Rinsing the system

Only for SSA 600 with liquid dosing.
When cleaning the system diluent is taken from the supply bottle and pumped
through the entire path via the dosing device to the dosing tube and dispensed into
the wash cup.
1. Enter the number of repetitions in the entry field Wash cycles.
2. Save the entry with the symbol .

3. Use the [Wash] button to start the wash cycle.
Automatic depth correction for dosing unit

Typically, depth correction occurs automatically when working with an SSA 600,
i.e. as the volume that is drawn from dosing unit cups increases, the immersion
depth will be matched accordingly. Starting volumes other than those which were
set via Method can be corrected in this window. These settings are similar to those
for MPE 60 (→ "Automatic depth correction for MPE 60" pg. 141).

Data management and report printout
9 Data management and report printout

9.1 Creating and printing result reports
Measurement results are printed as reports. You may freely choose the content of
the printout regarding the values, spectra, concentrations, etc. to be presented.
You may also save a report layout and use it for other measurements, too.
 Open the Data– Reports window using menu command File / Print / Report if
you intend to print the current measurement results.
Extras / Data…  Alternatively, you may open the window using menu command Extras / Data…
File / Print / Report or the icon button
.
On the window following information are shown:
• name of the current result file
• information about the selected result file
• all method versions that belong to the results file (only if the method is
currently loaded or it was saved along with the results file)
 For printing of a stored result with open the standard window open and
choose the result file.
 Print window using [Print].
 Select output target and report options (→ "Selecting output target and report
options" p. 153).
 Start the printout using [Print].
Fig. 60 Data – Reports window: Selecting reports to be printed

9.1.1 Selecting output target and report options

The output target and the report options are defined in window Print.
The window Print is opened,
• when using button [Print] in window Data / Reports,
• when using button in an active window, or

File / Print / Active • when printing the content of the active window by using the menu item File
Window... / Print / Active window....
Fig. 61 Print window
Select output target

 Select the target for the output:
Target From this list box, choose the output medium.

Printer Prints to the connected default printer.
TXT Saves the report to a text file.
HTML Saves the report to an HTML file.
PDF Outputs the report as PDF file.
[Properties] If the selected target medium is Printer.
Opens the Print dialog, where you can choose the printer
and the desired printing parameters.
By default, the default printer and the global print properties
are preset or those set via menu command File / Printer
Setup….
[File name] Here, enter the file name for TXT, HTML or PDF files.
Note
The PDF converter available in ASpect CS does not convert graphics (spectra or
calibration curves). If you should need these properties, install your own PDF con-
verter. Select Printer as target medium and choose the PDF converter as the
printer to be used.

Define report content

You may individually define content and layout of result reports and save it as re-
port stylesheet.
 In the Print window, click on [Options…] to open the Report options window.
 Set the following options:
Fig. 62 Report options window
Results tab
On the report, only the selected options will be included.
Types
Sample type Adds the measurement results for the sample type to the re-
port.
Calibration Adds the calibration results to the report.
QC and other Adds the measurement results for QC samples and further
samples sample types to the report.
Actions Adds performed actions to the report. This settings documents
the Special actions defined in the sequence (pause, display-
ing calibration curves).
Results
Sample infor- Sample information data according to the result table

mation
Conc.1 Concentration of the analyzed sample
Conc.2 Concentration of the original sample (considering the specified
pre-dilution factors)
Abs. Absorbance of the sample (mean value in statistical analyses).
Single values Absorbance values of single measurements in statistical anal-
(Abs.) yses.
QC Results of quality control
Calibration plot Graphic presentation of calibration curve

Signals Absorbance signal vs. time curve (only for the 1st measurement
of a statistical series).
Page break
automatically Automatic page break at the end of the page.

after Page break after the number of measured samples defined in
the Samples field.
Additionally after Starts a new page after any change of the method.
change of meth-
od
Signals
In the Y-scale (Abs.) field, you can set the scaling for the graphic presentation of
the measured signal.
Other tab
In the Userdefined header text field, you may enter a text of up to 125 characters.
If you activate the Page break after method parameters option, a page break is
made after the presentation of the method parameters.
If you activate the Open saved document in application option, result reports
saved as TXT, HTML, or PDF file will be opened in the application associated with
the corresponding file extension.
With the setting selected in the Scaling [%] field you can vary the size of the report
printout. In this way it is possible to adapt it to other paper sizes or your specific
analysis reports.
Buttons in Report options window
[Open] Choose a stored report stylesheet in the appearing Open

standard window.
[Save] In the appearing Save As... standard window, save a report
stylesheet with the selected options.
[Default set- Reset the default result report settings.
tings]
Print preview
 In the Print window, click on [Print preview...] to open the Print preview win-
dow.
The Print preview window contains options for instant printout and page zooming.
[Print] Starts the printout to the selected printer.

Select list Selection of printer or file format for printout to file.
All All pages of the report will be printed.
Pages Prints an excerpt of continuous pages of the report. Enter the
first and the last page to be printed in the input fields displayed
right of this option button.
Choose the zoom factor for the page view.
Page From this field, choose the page to be displayed.

Cols / Rows Simultaneous display of several pages.

In the Columns input field, set the number of pages that shall
appear side by side; in the Rows input field set the number of
pages that shall appear one below the other.
Fig. 63 Print Preview
9.2 Further print functions

Beside the result records, the content of the following windows can be printed:
• Method
• Sequence
• Sample ID
• QC (Quality Control charts)
• Calibration
• Autosampler positions
 On the Aspect CS workplace, activate the window, the content of which you
want to print.
File / Print / Active  Open the Print “window title” dialog using menu command File / Print / Ac-
Window... tive Window....
 With [Options…], open the Report options dialog with the Other tab (→
"Selecting output target and report options" p. 153).
 With [Print] or [Save…] start the printout or saving to the target selected from
the Target list box.

9.3 Data management for methods, sequences and result

data
ASpect CS manages data in different ways.
Methods and sequences are saved to separate databases. The method database
is saved as "method.tps". The database holding the sequence data bears the name
"sequ.TPS".
For the results obtained by measurements, separate databases are created each.
Further results can be added to a database by later measurements. Deleting indi-
vidual samples from a database, however, is impossible. Result databases have
the file name extension ".tps".
Sample information data are stored in an Excel-readable format with the extension
".csv".
Methods, sequences and result data can be organized in the Data window. The
same dialog functions for the management of methods and sequences are also
used for the opening and the saving of these files.
 Open the Data – Data management window using menu command Extras /
Data… or icon button
Extras / Data…
.
Fig. 64 Data – Data management window
In this window, you can manage methods, sequences and results. Choose the de-
sired type of data from the Type list box.
9.3.1 The database window

Methods and sequences are saved to databases. When saving, opening, deleting,
importing and exporting methods and sequences, database windows are opened,
that have identical elements.

Fig. 65 Database window
Name Entry or display of the name of the selected method or se-

quence.
Cat.: Additional identifier (category) for the search for the method
or sequence in the database.
The identifier may contain maximally three characters.
You can restrict the number of entries to the list by entering a
category identifier in the Cat input field. If you want to have
the methods/sequences of all categories displayed, delete the
entry from the Cat field.
Method/sequence Display of the stored methods/sequences with name, version,
list date, time, category and operator.
Sort Sorts the list of methods/sequences by various criteria, such
as name/version or date/time. Depending on the selected
option, the entries may be sorted in increasing or decreas-
ing order.
Description Display or entry of additional remarks, e.g. on the use of the
method/sequence.
Current version If several versions of a method/sequence exist in the data-
only base, only the method/sequence having the highest version
number will be displayed.
In ASpect CS software, methods/sequences of the same
name will not be overwritten, but another version created and
the version number increased by 1.
9.3.2 Managing methods and sequences

The databases also provide functions for importing, exporting or deleting individual
methods or sequences from the respective databases. In the following, methods
and sequences are referred to as data records.

Note
To select several data records of the database window simultaneously, hold the
Ctrl or Shift key depressed.
Data... or icon button
Extras / Data...
.
 From the Type list box, choose the type of data record to be managed: Meth-
od or Sequence.
Exporting data records

Using the export function, you can make data records accessible to other AAS de-
vices of the same type. You may export several data records to a common file.
Export files get the following extensions: Method data records - ".MET", sequence
data records - ".seq".
 Click on [Export…] to open the database window.
 Choose the data records and click on [Export].
This will bring up the standard Save as... window.
 Enter a file name and confirm it with [Save].
The database window appears displaying the exported files.
 Close the database window with [Close] and return to the Data management
window.
Importing data records

Using the import function, you can load data records from other AAS devices of the
same type into your database. An imported file may contain several data records,
from which you can select those to be loaded.
 Click on [Import] to open the Select file for import window with the standard
functions for opening files.
 Choose the file to be imported.
 Confirm the choice with [Open].
This will bring up the database window with the presentation of name, date of
creation and category of the data records contained in the file. In the title bar of
the window, the name of the import file is displayed.
 Select the data records to be imported and click on [Import].
The data records are imported into the database. If a method/sequence of the
same name should exist already, a new version of the method/sequence will
be created.
In the database window, the current versions of the available data records ap-
pear.
 Close the database window with [Close] and return to the Data management
window.
Deleting data records

Using the delete function, you can permanently delete data records from the data-
base.
 Click on [Delete] to open the database window.
 Select the data records to be deleted.

 Click on [Delete].
The database window is being updated displaying only the remaining data rec-
ords.
With data records of the same name, the version number is kept. The versions
will not be renumbered.
Deleting data records via the File menu

 Alternatively, you may activate the database windows Delete method or De-
lete sequence via menu command File / Delete / Method... or File / Delete /
Sequence....
 Then, proceed as described above.
9.3.3 Managing results files

Results are always saved to the database during the measurement. A database
holding result data may be copied or deleted.
Data… or icon button
Extras / Data…
.
 From the Type list box, choose the Results option.
Copying results files

With the [Copy…] command, you may copy one or several databases as well as
existing spectrum files to another folder.
 Click on [Copy…] to open the Copy results file window with the overview of
existing result databases.
The results files are listed with name, size and date/time of the last change.
 Select the results databases by mouse clicks. To select several databases,
keep the Ctrl or Shift key depressed.
 Click on [Copy] to open the Select directory window.
 Choose the target folder and confirm your choice with [OK].
The results files are being copied to the selected target folder.
Deleting results files

Using this function, you may delete results files and/or spectra permanently.
 Click on [Delete…] to open the Delete results file window with the overview of
existing results files.
The results databases are listed with name, size and date/time of the last
change.
 Select the results database to be deleted by mouse clicks. To select several
databases, keep the Ctrl or Shift key depressed.
 If you want to delete the results database and possibly saved spectra, click on
[Delete].
 If you want to delete the spectrum files only, click on [Delete spectra data
only].
 Confirm the displayed query with [OK].
The files are being deleted permanently.

9.3.4 Copying lines/wavelengths files

The application allows you to copy the device-specific lines/wavelength files with
the line parameters and existing wavelength correction data to a user-defined fold-
Data management er and view them with a text editor.
tab  Open the Data – Data management window using menu command Extras /
Data... or icon button
.
 From the Type list box, choose the Lines/wavelength file option.
 Click on [Copy…] to open the Select directory window.
 Choose the target folder and confirm your choice with [OK].
The lines/wavelength files are being copied to the selected target folder.
9.4 Copying to the clipboard

9.4.1 Copying results to the clipboard
The application lets you copy the results of selected samples directly to the Win-
dows clipboard thus making them accessible to other Windows applications. The
corresponding commands are contained on the Edit menu.
Edit
Copy visible Copies the visible sample results of the current table.
columns only
(Strg+C)
Copy all col- Copies the sample results of all tables.
umns
Column titles If activated (check mark), the copy action includes the column
headers.
 Select the samples from the desired table of the results list.
Holding the Ctrl or Shift key depressed, choose the samples by mouse clicks
on the respective row.
To select all rows, use menu command Edit / Select All.
 If necessary, activate menu command Edit / Column Titles to have the col-
umn headers included in the copy action.
 Activate the desired menu command to copy the results to the Windows clip-
board.
9.4.2 Copying graphics as screenshots

You may also copy graphic windows and graphs of calibration curves, absorbance
signals or spectra as screenshots to the Windows clipboard.
 Right-click on the graphic to be copied.
This will bring up a submenu with two copy commands.

 Choose the desired command:

Copy graphic to copy the graphic only.
Copy window to copy the complete window displayed.
The selected object will be copied to the clipboard thus being accessible to
other Windows applications.
9.5 Saving results in ASCII/CSV format

You may save measurement results both automatically and manually in ASCII/CSV
format. For both export formats, the parameters for the decimal and list separator,
and the result columns to be exported are to be defined in the Options -
ASCII/CSV Export window (→ "Export options", p. 16).
Automatic continuous data export

With activated automatic continuous data export option, every entry in the results
table is instantly exported to the defined ASCII file. The name of this ASCII file is to
Continuous ASCII be defined in the Options - Continuous ASCII Export window (→ "Options for
Export tab continuous ASCII export", p. 16).
Manual data export

If you intend to export data manually, you can select the rows of the results table to
be exported.
 Select the samples in the desired results table.
Holding the Ctrl or Shift key depressed, select the samples by mouse clicks
on the respective rows.
To select all rows of the table, use menu command Edit / Select All.
Edit / Save selec-  Then, activate menu command Edit / Save selection to open the Save As
tion standard window for saving files.
 Enter the file name and confirm it with [OK].
The data will be saved in the CSV format which can be read by MS Excel and
other programs.

User Management
10 User Management
An optional software package for ASpect CS user management is available. It pro-
vides extended functionality for operation of ASpect CS in accordance with the
FDA requirements on Electronic Records & Electronic Signatures (21 CFR Part
11).
The user management package allows for one administrator level and four user
levels. A user with ASpect CS administrator rights may perform any of the following
action with the help of this user management package:
• flexible system configuration (code word and login gidelines, audit trailing,
signatures, data directories)
• creation of a user level for each user with a stepped pattern of user rights
• assignment of code words for access to ASpect CS software
• assignment of personalized working directories for methods, sequences
and results to users
• inspection and exporting of created audit trail (events log sheet)
Once the user management package is installed and configured, the System
menu item in ASpect CS will be active. You can use this menu item to access one
or more desired functions of user identity management.
Any change in user data will be permanently saved in an encoded data base on
exiting a pertaining window.
Note
In order to meet safety requirements, a Microsoft Windows 2000/XP operating sys-
tem with adequate configuration resources must be available. This applies to file
access rights and other setting actions of a kind that should be performed by an
authorized system administrator.
10.1 Hierarchy and access to functions

The user identity management package provides for one administrator level and
four user levels.
The hierarchy structure for user levels is as follows:
Administrator > level 1> level 2 > level 3 > level 4.
Access to Aspect CS functions

Administrator level
The user has full access rights to ASpect CS and to any function of user identity
management.
Level 1
Level 1 users have unlimited access to all Aspect CS functions, but are denied
access to user identity management.
Level 2
Same as level 1 users, except:
• Deletion of methods (M1 ID code)

User Management
• Deletion of sequences (P1 ID code)

• Deletion of QC rule tabs (Q1 ID code)
• Deletion of results files (R1 ID code)
An ID code is used in advisory notes to operators.
Level 3
• Saving of methods (creating methods in a method data base) (M2 ID code)
• Saving of sequences (creating sequences in a sequence data base) (P2 ID
code)
• Changes in records regarding wavelengths (W1 ID code)
Level 4
• Changes in method parameters (E1 ID code)
(users of this category can only load previously created methods and sequences
and perform measurement).
• ID code will be referred to in operating advice.
Function ID Admin. Level Level Level Level

code 1 2 3 4
Work with user ID management + - - - -
Delete methods M1 + + - - -
Delete sequences P1 + + - - -
Delete QC rule tabs Q1 + + - - -
Delete results files R1 + + - - -
Save methods M2 + + + - -
Save sequences P2 + + + - -
Make changes in wavelength W1 + + + - -
records
Make changes in methods E1 + + + + -
Load methods and sequences + + + + +
Peform measurement + + + + +
*ID code is used in operating advice.
10.2 User Management setups

User management setups can be made by an ASpect CS user with administrator
rights as part of initial installation of the user ID management software package or
at any time thereafter.
A so-called account is created for each user. An account contains a given user
profile. Where a user account is not required any longer, it can be disabled or in-
hibited. User accounts cannot be deleted.

User Management
System / User  Trigger a System / User Management... menu command or launch user man-
Managment agement via an entry button of this name in the starting menu.
On completion of login procedures, the User Management window will open.
Fig. 66 User management window
The window contains a list of registered user names with assigned passwords. It
shows the user profile details for a selected user in its right-hand subarea.
Indicator and control elements
UserID Login name of user

User Administrator, level 1 to level 4
E-signature Yes: User is authorized to electronically sign result data.
No: User has no authorization for electronic signature.
Status Active: User name allowed for use (green circle).
Disabled: User name was disabled and cannot be used (red
circle).
Password pro- Active: User login requires a code word (key)
tection Inactive: User login allowed without a code word (key
crossed out)
Valid until Unlimited: Password never expires.
Date/days: User must change his/her password on expiry
of specified term.
Full name Complete name of user
Description Optional description of user
Control buttons
[New ...] Creates new user.
Opens the Add user data window.

User Management
[Modify ...] Changes user data for a marked table line.

The Modify user data window will open for a marked table
line. The same dialog screen may be called up by double-
clicking the particular table line.
[Preferences...] Allows changes in user management configuration.
[Audit trail.... Audit trail (events logsheet)
[Exit] Terminates this application.
10.2.1 Configuring user management

For configuration, the Preferences window provides selection options as follows:
• Password policies
• Login and audit trail
• Signature meanings
• Selected data directories
 Click onto [Preferences...] in ASpect CS User Management window.
The Preferences window opens.
 Select an option group you want to change from the left column.
These setups will be valid for newly created user accounts. They should therefore
be made following installation. On exiting the window with [OK], all setups will be
saved, on selection of [Cancel], they modified settings will be discarded.
[Set default set- Sets the default settings (factory settings) for a given selection.
tings] The settings for other areas will be unaffected.
Login/password
Fig. 67 Setups for login and password policies

User Management
Login policies (for new user names)
Number of login Shows the number of invalid login attempts (max. 10).
attempts On excession of the maximum allowed number, the ASpect CS
session will be terminated after a cetrain waiting time and must
be restarted for another login. An entry (warning) is added to
the audit trail file.
Minimum user Defines the minimum prescribed number of characters for a
name length newly created user name
Password policies (for new user names)
Enforce login A password must be assigned to newly created user names.

with password
Password with Only passwords consisting of letters and numeric characters
letters and num- can be assigned. This policy equally applies to changes in
bers password.
Pasword and Only passwords which are different from the respective user
user ID must be name will be accepted. This policy equally applies to changes
different in password.
"User must For newly created users, the Change password at next lo-
change assword gon! checkbox will be turned on by default. The user will be
at next logon!" is prompted to change his/her password when logging in to AS-
active pect CS for the next time.
Password ex- On expiry of a preset term, the user will be prompted to
pires in ...day(s) change his/her password when logging in to ASpect CS. The
password is then extended by a term as set in Policies. This
value is then acknowledged as a template that can be modi-
fied for other single users (max. 999 days).
Minimum length Designates the minimum required number of characters for a
of password newly created password; number of characters: 3 to 10
Fig. 68 Setups for paths

User Management
The ASpect-CS working directory and the audit trail directory provide specification
options.
Paths
ASpect-working Working directory of Aspect CS.

directory The working directory contains a data base of methods and
sequences and results files. The working directory was defined
as part of ASpect CS installation and may be changed at this
point.
Audit Trail Path of audit trail file.
This path may be changed.
User database Path of user data base.
This path may only be changed with the help of the installation
program.
Audit Trail
Fig. 69 Settings for audit trail data
Inactive (no en- No entries will be added to the audit trail file (event log sheet).
tries)
Active Entries will be added to the audit trail file (event log sheet).
Allow measuring When active, this checkbox allows a measurement to be trig-
only with saved gered in ASpect CS only if a method was loaded and no
methods change was made in this method since it was saved for the last
time.

User Management
Signatures
Fig. 70 Editing of signature meanings
Edit list of signature meanings

This list shows those signature meanings that are selectable for signing.
Add Adds a signature meaning, e.g. created, reviewed, approved

(max. 30 characters).
Modify Changes a signature meaning that was marked in the list.
Delete Deletes a signature meaning that was marked in the list.
10.2.2 Creating a new user account

Only users with administrator access rights are authorized to create a new user
account.
 Click the [New] button in the User Management window, in order to create a
new user account.
The Add user data window appears.

User Management
Fig. 71 Editing of user data
The input fields in this window provide setting options as follows:
User ID The name that is required for a user to log in.

No checks are made for capital and small lettering. The mini-
mum name length depends on configuration settings made in
Login/Password (→ "Configuring user management" p. 166 et
seq.).
Max. length: 32 characters
Full name Full name of user. This name will serve as a constituent of the
electronic signature.
Max. length: 30 characters
Description A field for note or comment text. Entry is optional.
User level User level
Password... Opens a dialog screen for password entry.
Max. password length: 20 characters
The minimum length and other password policy rules may be
configured (→ "Configuring user management" p. 166 et seq.).
Capital lettering and small lettering are distinguished for pass-
words. If the password dialog is acknowledged without a pass-
word entry, the password protection will be canceled.
Key icon:
Password protection is active.
Key crossed out icon:
User name uses no password.
Password never Password will remain valid for unlimited time if this box is ac-
expires tive.
If it was disabled, the given password will expire within a preset
term.
The specified value is sourced from password policies. A user
may also extend his/her password in advance.

User Management
User-specific If active, this box will create the user’s own working directory in
data path this format: \ASpect-Working directory\User name.
As part of an initial login to ASpect CS the appropriate directory
structure will be created.
Use e-signature Allows the user to electronically sign for measured results if
active.
Disable user ID Prohibits the use of a user name if active.
User names can be temporarily disabled. A disabled (as op-
posed to a removed) user name cannot be reassigned to an-
other newly created user.
User must Will prompt the user to change his/her password as the next
change pass- ASpect CS session is triggered.
word at next lo-
gon
 Click [OK] to confirm all features of a newly created user account.
10.2.3 Modifying a previously created user account

 To select a user account you want to modify, click this account in the table of
the User Management dialog window, then click the [Modify] button.
The Edit user data window with selected accounts will open (→ "Creating a new
user account" p. 169).
10.3 Viewing and exporting Audit Trail

An audit trail file keeps track of certain system events and any warning or error
message that occurred during an ASpect CS session.
System / Audit  Click [Audit Trail...] in the User Management window
Trail
or:
Select the System / Audit Trailmenu command in Aspect CS.
The audit trail can now be:
• viewed
• updated
• copied for backup purposes before final deletion (only if Audit Trail was
called up from the User management window)
• exported as a "*.csv" file (only if Audit Trail was called up from the User
management window)
Note
The size of an audit trail file has no influence on system speed. However, for a file
size of 20 MB and beyond, a note will be displayed, prompting you to archive this
file and delete your entries.

User Management
Fig. 72 Audit Trail window selected in User Management window
The following parameters are documented in an audit trail file:
Type Indicates the type of an event

An audit trail keeps track of the following types of events and
marks these with symbols: Info, Warning, Error, Login and
Logout
Date/Time Designates the date and exact time of an entry (PC watch)
Time Zone Indicates the time zone to which the time of an entry is refer-
enced (Windows system control)
Name Describes an event, for details refer to Description field:
LOGIN: Logs in
LOGOUT/EXIT: Terminates an application
ADD/CHANGE/DELETE: Edits methods, sequences and user
data
PWDCHG: Allows changes in password
RUN: Triggers an analytical sequence
PRINT: Prints trailer file
SIGN: For signing of results
#nnnn: Error number
Cat. Shows the category of an event.
"USRMGMNT" is the category used to mark those entries made
in User Management. All other categories will be entered by
ASpect CS.
Operator Designates the user in login state at the moment of an entry.
Description Provides more detail about the cause of an entry.
Updating an audit trail

You may use [Refresh] to update the list of entries in an audit trail.
This may be necessary if further entries were added to a previously created audit
trail display.

User Management
Copying an audit trail for backup

(can only be performed in User Management)
For backup, an audit trail file can be copied to a user-selected path and deleted if
desired, once it has been secured.
 To trigger a backup process, click [Copy/move Audit Trail].
The Save as ... .standard window opens.
 Type in a name and save your file with [OK].
On completion of backup copying, an "Audit trail file was copied. Do you want
to delete the source file?" message is output.
 Acknowledge deletion or preserve your audit trail:
[Yes] Deletes the audit trail file. The audit trail list is empty and
begins to be filled with new entries.
[Cancel] The audit trail file will not be deleted. New entries will be
added to the existing list.
To restore a backed up aidit trail file:

 Rename this file into "EVNTLOG.TPS".
 Go to User Management and change the audit trail path to the path of the file
you want to restore. To do this:
Use a click onto [Preferences] in the User Management window to open the
window of this name. It allows configuration settings for User Management.
Enter the path of the file you want restored as audit trail path (→ "Configuring
user management" p. 166).
 Open Audit Trail again.
The restored audit trail file will come on display. Further entries will be added to
this file.
Exporting Audit Trail

(this function is only available in User Management)
Audit trail entries can be exported to a CSV file (comma separated values). This
format is supported by MS Excel (among others).
 Click [Export] to open the Export audit trail dialog field.
 Select an option for exporting:
All records Completely exports audit trail file to CSV file.

Only records Exports only such entries to a CSV file, which were made
from to within a specified period of time “from / to”.
 Use [OK] to open the Save as... standard window.

 Type in a name, then save your export file with [OK].
The audit trail file will be unchanged after exporting.
10.4 Changing a password

Depending on his/her user account settings, a user may or may have to change
his/her password at regular intervals.

User Management
System / Change  Select the System / Change password... menu command in Aspect CS.
password
The Change password dialog screen opens.
 Enter your previous password at the input field, then enter the new password
twice and click [OK].
On successful entry, a “Password changed“ message will appear.
10.5 Electronic signatures

ASpect CS allows users to electronically sign up for their result data provided the
given user has authorization to Use e-signature (→ "Creating a new user account"
p. 169). A signature will close work on a particular file so changes in this file made
at a later point in time will cause an invalid signature state.
A sign-up procedure will encode a given file and assign to this file a signed state
and the data of the signing user. In addition, an encoded signature file of identical
name (same as results file) will be created, except that this signature file carries a
*.sig data extention. It contains the checksums of the related results file, including
those of (if included) a spectrum file.
A file may be signed by more than one user.
10.5.1 Signing measured results

A file of measured results may be sealed with an electronic signature by one or
more users authorized to do so on completion of measurement or when this file is
loaded at some later point in time.
System / Sign off  Select the System / Sign off results... menu command in Aspect CS.
results
The Sign off dialog screen opens.
User ID The login name of a current user.

A user ID may be modified to facilitate signing by more
users (max. 32 characters).
Password Code word of a user (max. 20 characters).
Meaning The measning of a signature, for example, Created, Re-
viewed, Approved.
To define a list of signature meanings is the responsibility
of the User Management administrator (→ "Configuring
user management" p. 166).
Comment For optional comment (max. 256 characters)
[Sign off] Signs a given document with any settings it contains.
After actuation of [Sign off], you will be asked if this signa-
ture is granted or if the process is to be aborted. Success-
ful granting of a signature will be confirmed.

User Management
Fig. 73 Dialog screen for measured data sign off
10.5.1.1 Displaying signatures

A print preview of signed result data includes a Signatures section that is attached
to the end of the related log sheet. This section contains all electronic signatures
belonging to the particular file.
Fig. 74 Print preview with signature section
Issued by States the full user name and ID user of the individual who
signed this file.
Signed on: Date/time of signature granting

User Management
Status The signature state may take on one of the following meanings:
Valid Signature and result data are complete and correct.
Calculated checksums of a file reveal no variance
against the checksums contained in the signature file
at the moment of signing.
Invalid (signature file missing or invalid)
Failure to find signature file that belongs to data set
or signature file contains faults.
Invalid (TPS data)
Results file was modified following signature. Com-
parison between newly calculated checksums and
previously saved checksums reveals variances.
Invalid (SPK data)
A file with raw spectrum data was modified after be-
ing signed. Comparison between newly calculated
checksums and previously saved checksums reveals
variances.
Meaning The meaning of signatures
Remarks For comment text (optional)

Supplement
11 Supplement
11.1 Overview of markings used in the display of values
Remark Meaning Values Output
> Cal The mean value is larger than the working Mean val- Sequence and
range of the calibration curve. ues results window
< Cal The mean value is smaller than the working Mean val- Sequence and
range of the calibration curve. ues results window
< LOD The value is smaller than the limit of detec- Mean val- Sequence and
tion. ues results window
< LOQ The value is smaller than the limit of deter- Mean val- Sequence and
mination and larger than the limit of detec- ues results window
tion.
RSD! The mean value of sample or standard is Mean val- Sequence and
outside the range of the specified relative ues results window
standard deviation.
RR! The mean value of sample or standard is Mean val- Sequence and
outside the range of the specified relative ues results window
range.
Factor! Limit of recalibration factor for the calibra- Calibration Sequence and
tion curve was exceeded curve results window
R2(adj.) The quality of regression R2(adj.) of the Calibration Sequence and
calibration curve falls below the specified curve results window
value. Calibration
curve window
#MAN. The single value of sample or standard was Single val- Single values
manually excluded from the calculation of ues window
the mean value.
#COR. The single value of sample or standard was Single val- Single values
automatically excluded from the calculation ues window
of mean values by the Grubbs outlier test
11.2 Description of the algorithms used for spectral

background correction
11.2.1 General
Spectral background correction is performed separately for every individual spec-
trum. The measurement delivers a time-resolved absorbance signal with a number
of absorbance values that depends on the read time.
For every evaluation pixel (Method – Evaluation window, Eval. Pixels column),
an individual absorbance value is calculated and summed up over the number of
evaluation pixels.
Depending on the AAS technique used, a peak-integrated, area-integrated or
mean value is calculated from the absorbance signal.

Supplement
11.2.2 Background correction “without reference”

Calculation of the reference value
The reference value is formed by averaging of the statically set pixels of the meas-
uring range. If no static pixels have been set, averaging covers all pixels of the
measuring range, excluding a range of +/-10 pixels around the measurement pixel.
A separately measured reference spectrum is not needed.
Calculation of absorbance spectra
Abscorr=lg(I0/Ipeak)
I0 – Mean value of the pixels within the slit, excluding the measurement pixel +/-
10 pixels.
Ipeak – Measurement pixel
Limits
Flame and other molecule structures that would be covered by a separate refer-
ence spectrum are not compensated. Due to the inhomogeneous CCD illumination,
the absorbance spectrum may have a falling or a rising baseline.
This correction corresponds to the broadband D2 correction of line AAS.
11.2.3 Background correction "with reference"

Calculation of the reference value
The individual absorbance spectra are calculated from the single spectra of the
sample and the medium normalized reference spectrum. The medium normalized
reference spectrum is obtained by dividing the areas (sums) of the individual refer-
ence spectra by the area of the mean-value reference spectrum (normalized). Af-
terwards, the normalized single spectra are averaged once more.
Calculation of absorbance spectra

Due to the fluctuations of light source and atomizer, the obtained absorbance spec-
tra exhibit more or less sloping and curved baselines with different offset values.
Therefore, in a further step, a baseline is fitted for every single spectrum. For this
purpose, BG (background) correction points are set, through which a polynomial is
drawn. The fitting polynomial maximally is a second degree polynomial. The de-
gree is determined based on the number and the distribution of the correction
points. BG correction points lying apart by less than 10 pixels are united to a group.
The fitted baseline is subtracted from the absorbance spectra. Subsequently, the
absorbance value can be determined directly.
The BG correction points can be set either statically or dynamically (automatically):
Static:
The BG correction points are set manually or from a list in the range of center pixel
+/-0.5 x measuring range.

Supplement
Dynamic:
The BG correction points are found by an algorithm.
• Aim: Identification of those pixels that do not significantly differ from base-
line noise. To this end, the gradients of the observed pixel to the +/-3
neighboring pixels are calculated and tested for gradient change.
The BG correction points of the single spectra are summarized. If a certain
BG correction pixel is found with a defined frequency, this pixel will be
used as BG correction point for the mean-value spectrum.
• Side conditions: If all BG correction points lie on one side of the measure-
ment pixel, an error message will be output. In the case of one-sided cor-
rection, the extrapolation of the polynomial may lead to large errors. The
correction point algorithm will detect a gradient only if the absorbance dif-
ference between four adjacent pixels exceeds a defined amount (>2E-
4/pixel).
• The range of the measurement pixel +/- 10 pixels is excluded from the
search.
Limits
The algorithm used has fundamental problems with overlapping structures extend-
ing over the entire range of the spectral slit, as in this case no region is dominated
from baseline noise. Here, a dynamic fit of frequency is carried out, i.e. the deci-
sion criterion is gradually relaxed. If this does not result in a sufficient number of
BG correction points, static pixels will be set, which are saved in the line table as
presetting.
11.2.4 Background correction "IBC"

The IBC background correction (IBC= iterative baseline correction) is based on
filtering the intensity spectra. Background structures which are broader than the
analyte peak are eliminated. The algorithm is suited for complex spectral back-
grounds.
11.2.5 Spectrum subtraction (correction of permanent structures)

Application
Multivariate correction of flame structures and other interferences existing in refer-
ence and sample spectra at different intensities
Assumptions
• The sum spectrum is the weighted sum of the spectra of the pure sub-
stances and the noise.
• Other wavelength regions (e.g. additional analyte bands that do not exist in
the correction spectrum) do not exist, or they are excluded.
• No or only very little wavelength shifts between sample and correction
spectrum as these lead to artifacts.

Supplement
The flame structure spectrum is calculated from the reference spectrum according
to Abscorr=lg(I0/I0-Offset); for further molecule corrections, the spectra of the pure sub-
stances are required.
The basis for the calculation is the multivariate classical calibration:
y=X*b+e m – Number of wavelengths/pixel
n – Number of pure substance spectra
y – Sum spectrum (mx1)
X – Matrix of pure substance spectra (mxn)
b – Coefficient vector
+ + -1
b(estimated)=X y with X =(X’*X) X’*y (pseudo inverse)
The product of pure substance spectrum and coefficient can then be subtracted
from the sample spectrum:
yN= xN-Σ(bixi), with i = 1 ... except N (index of the spectrum of interest)
11.3 Working with Correction Spectra in ASpectCS Software

No extra sub-system is required for background correction in HR-CS AAS operat-
ing mode. The system is equipped with a CCD line of 200 pixels that are equivalent
to 200 simultaneously and independently working detectors. Some of these detec-
tors which are located on either side of an analytical line are selected and used for
corrective purposes by software tools. Any change in radiation intensity, which is
found to affect all correction pixels to an identical degree, will be automatically cor-
rected. This includes, for example, variations in lamp emission as much as any
continuous background absorption.
Events of discontinuous background absorption, which may be due to direct over-
lapping of a line with a matrix element or cases of fine-structured absorption of
molecules, can be mathematically removed with the help of reference spectra (cor-
rection spectra). This User Guide describes the procedure that is required to de-
termine correction spectra and compile corrective models in an AspectCS software
session.
11.3.1 Initial Situation

Working in the Method window with Evaluation tab selected, with reference must
be active for background correction and dynamo. for adaptation. In addition, func-
tions Save with results: Method and Spectra must be active in the Output tab.
Perform one reference measurement and one trial measurement for flame tech-
nique, perform only one trial measurement for graphite tube technique. Double-
click (with left mouse-key) the results display field of the trial measurement screen
to open the related individual sample values. A click onto [Show spectrum] will
display the pertaining spectra.
Once you have reached this display screen, you can decide if the analyte signal is
compromised by line overlap effects of matrix elements or by absorption of mole-
cules.

Supplement
Note
Refer to Welz et al.: ”High-Resolution Continuum Source AAS“ for potential inter-
fering elements or molecular bands.
Example
The zinc line at 213.857 nm may be compromised by NO molecular bands or an
iron line (see diagram view). NO molecular bands may be caused, among other
reasons, by high concentration of HNO3 in a sample solution.
11.3.2 Determining Correction Spectra

 Measure the various matrix components that cause spectral overlaps now.
Note
The concentration values of matrix components need not necessarily match those
in the respective samples. But concentration values must be high enough for
mean-value spectra to clearly show extinction values. As a compulsory precondi-
tion for correct spectral correction, only one component may be measured as pure
substance at a time.
Example
For a zinc line that is overlapped by HNO3 and iron, an HNO3 solution of higher
concentration (e.g. by 5%) and an iron solution (some hundred milligrams per liter)
will be measured as sample.
 On completion of measurement, double-click the results list to display the indi-

vidual readings and double-click the [Show spectrum] button to display the
various spectra.

Supplement
 Select [Corr. Spectrum] to save the mean-value spectrum of a matrix compo-

nent as correction spectrum.
 Assign a name to the spectrum in question and complete this process by se-
lecting [Save]. For testing the model the check box “Test model (no save
prompt)” can be selected.
 Repeat these working steps for each matrix component.
11.3.3 Compiling a Correction Model

 Double-click the results list to display the individual readings of the sample
being analyzed and click [Show spectrum] to display that sample’s spectral
display graph.
 Activate the Model option now.
 Select [New/modify model] to open the Spectral corrections window.
The sample spectrum appears.

Supplement
Use the [Add] button to open a selection screen of previously saved correction
spectra. Use a mouse-click to select a correction spectrum and complete this pro-
cess by clicking [Load]. Repeat these working steps for each individual correction
spectrum.
 Activate the Highlight corrected spectrum option in order to check the result-
ing sample spectrum for absence of overlap effects.
 For testing the model select the check box Test model (no save prompt) and
return with [Close] tot he window Spectra.
Note! The model is not saved!
 Select again [New/modify model] to open the Spectral corrections window.
Click [Save] to open the window for saving a correction model. Assign a name
to the model you want to save and complete this process by selecting [Save].

Supplement
Note
By clicking the [Mask.] button and keeping the left mouse-key depressed at the
same time, you can mark certain ranges of a spectrum you want excluded from
calculation of a correction model. By default, the analyte line range is masked (pix-
els 92 to 110). More ranges may have to be masked in cases where no pure sub-
stances were available for determination of correction spectra and where impurities
may occur in varying portions.
11.3.4 Integration of a Correction Model into a Method
 Open the current Method screen (via icon), then open the Evaluation
tab.
 Select Spectral corrections in this screen to open the related window.
 Select a desired Model in the analyte line dialog field and exit this window via
[OK].
Once a method has been saved, all subsequent measurements using this method
will integrate and follow this generated correction model. Previous measurements
can also be re-calculated with the help of this method so no new measurement is
required.

Index
12 Index F
Flame
A Adjustment 105
Automatic optimization 110
Absorbance measurement 42 Manual optimization 108
Adjust autosampler AS 51/52s 135 Flame window 105
Ashing 114 Furnace program
Atomize 114 Graphic 120
Autosampler Trial run 120
graphite tube technique 35 Furnace Program
Solid analytics 37 Edit 112
Autosampler AS 51/52s Furnace window 112
Dosing speed 132
Insertion depth 132 G
Autosampler MPE 60
Adjustment 146 Gas adaption 114
Depth adjustment 141 Graphit tube
Dosing speed 141 Coating 121
Insertion depth 141 Graphite tube
Autosampler SSA 600 Clean 124
Depth adjustment 141 Graphite tube
Autosampler window 129, 137 Sensor error 124
Autosamplers Graphite tube furnace
Flame technique 32 Format 123
Hydride and HydrEA techniques. 32 Graphite tube lifetime 123
Graphs 9
B
H
Background correction 87
Burner Hydride system
Function test 105 Cleaning 125
Buttons Heating the cell 126
generally used 8 Initialize 125
Loading 125
C Window 125
Calbratione curve I
LOD/LOQ tab 93
Parameters tab 93 Injection step 114
Residual tab 93 Integration mode 22
Calibration Intensity 102
Delete Standard 93
Calibration table L
Automatic preparation 46
Limits of detection 93
Manual preparation 45
Limits of determination 93
Cleaning
Line identification 90
controlled 34, 36
Line/Wavelength file 103
Lines
D User-defined 24
Depth correction Lines/wavelength file
MPE 60 140 View 161
Dosing speed Lists 8
MPE 60 140
M
E Menu command ?
Energy 102 Contents and Index 7
Enrichment step 115 Search ... 7
Menu command Edit

Index
Clear Results Table 82 User Management 165

Column titels 161 Menu command View
Column Titles 161 Close Display Windows 69
Copy 9, 65 Detail results... 82
Copy all columns 161 Update result list 76
Copy visible columns only (Strg+C) Menu Command View
161 Open Display Windows 69
Insert 9 Menu command Window
Paste 65 Cascade 69
Save selection 162 Tile horizontal 69
Select All 161 Tile vertical 69
Menu command Extras MPE 60 autosampler
Data... 19, 159 Align to graphite tube 143
Data… 152, 157, 160
Options... 14 O
Menu command File
Offline mode 6
Delete / Method... 160
Delete / Sequence... 160
Main Settings 11
P
New Method 21 Pyrolyse 114
New Sample Information File 63
New Sequence 58 R
Open method 57
Open results 76 Result window
Open Results... 81 Solid tab 81
Open Sample Information File 66
Open Sequence 62 S
Print / Active window... 153 Sample moisture 64
Print / Active Window... 156 Scientific Mode 15
Print / Report 152 Solid analytics 12
Print / Report... 82 Solid autosampler window 148
Printer Setup… 10, 153 Solution analytics 12
Save / Method 57 Spectrometer window
Save / Sample Information 66 Opening 99
Save / Sequence 62 Stock standards
Start Offline 76 define manually 46
Menu command Method Development
Autosampler 129, 137, 148 T
Flame... 105
Furnace.. 112 Temperature-time program 112
Hydride... 125 Thermal furnace overheating 113
Method... 21 Thermal pretreatment 115
QC... 95
Sample ID... 63 U
Sequence 58 User management
Spectrometer... 99 Account 164
Menu command Routine User Management
Break 70 Hierarchy 163
Continue... 70 User profile 165
Extinguish flame 111
Reprocess... 75 W
Run Selected Sequence Row... 70
Start Sequence 68 Washing
Stop 70 AS 52s 34
Wash 75 MPE 60 37
Menu command System
Audit Trail 171
Change Password 174
Sign off results 174

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What are the main sections covered in the manual?

What are the main sections covered in the manual?

What customization options are available in ASpect CS?

What customization options are available in ASpect CS?

ASpect CS

Software for HR-CS AAS

Phone: Hotline: + 49 (0) 3641 / 77-7407

General information about Analytik Jena AG

Copyrights and Trademarks

contrAA is a registered trademark of Analytik Jena AG in Germany.

Publication No.: 160:004.23

Edition – Septembre 2011

© Copyright 2011 Analytik Jena AG

ASpect CS Issue 09/2011 1

8.2 Flame ........................................................ 105 9 Data management and report

2 Issue 09/2011 ASpect CS

10 User Management .................................. 163 11.2.1 General ..................................................... 177

11.1 Overview of markings used in the display 12 Index ........................................................ 185

ASpect CS Issue 09/2011 3

4 Issue 09/2011 ASpect CS

Described software version

1.1 User manual conventions

ASpect CS Issue 09/2011 5

This is a note to be followed to avoid operating errors and obtain

1.2 Starting and exiting ASpect CS

ASpect CS is being started.

6 Issue 09/2011 ASpect CS

1.3 General information on operation

1.3.2 The Help function

1.3.3 The menu bar

ASpect CS Issue 09/2011 7

View Opening and closing windows showing graphs and information

1.3.4 Frequently used control elements

[OK] Closes the window and accepts the settings.

8 Issue 09/2011 ASpect CS

Buttons accessible in lists

[Append] Appends a new table line to the end of the list.

1.3.5 Function keys

[F1] Activates the context-sensitive online help.

ASpect CS Issue 09/2011 9

1.3.6 Choosing a printer

1.4 General measurement procedure

10 Issue 09/2011 ASpect CS

2 Preparatory settings - Choosing the analytical

Fig. 1 Main Settings window

Flame contrAA 300 / contrAA 700

ASpect CS Issue 09/2011 11

Sample state and tube tye

liquid Samples are available in liquid (dissolved) state.

Routine Automatic run of analysis methods

12 Issue 09/2011 ASpect CS

ASpect CS Issue 09/2011 13

3.1.1 View options

Fig.2 Options – Display window

14 Issue 09/2011 ASpect CS

Show toolbar Shows the toolbar.

Subwindows can Activates the Maximize system button (square) in subwin-

3.1.2 Save paths

ASpect CS Issue 09/2011 15

Temporary data Folder for files created temporarily by the application.