Analytik Jena Contraa 700 Labrecycling

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contrAA 700

High Resolution Continuum Source


Atomic Absorption Spectrometer

User Manual
Service: Analytik Jena AG
Kundendienst
Konrad-Zuse-Str. 1
07745 Jena
Germany

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


Fax: + 49 (0) 3641 / 77-7449
E-Mail: [email protected]

General information about Analytik Jena AG


on the internet: http://www.analytik-jena.de

Copyrights and Trademarks

Microsoft, Windows 7/8, MS Excel are registered trademarks of Microsoft Corp.


The identification with ® or TM is omitted in this manual.

Documentation number: 161:102.23


Edition – January 2014
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 2014 Analytik Jena AG


Table of contents

Table of contents
1 Fundamental Information .................................................................... 7
1.1 Intended Use .................................................................................................. 7
1.2 User manual conventions ............................................................................... 7
2 Safety instructions ............................................................................... 9
3 Specifications ..................................................................................... 13
3.1 Technical data .............................................................................................. 13
3.1.1 Technical data of contrAA 700 ..................................................................... 13
3.1.2 Control computer data .................................................................................. 15
3.1.3 Data for graphite tube technique .................................................................. 15
3.1.4 Data for flame technique .............................................................................. 16
3.1.5 Data regarding flame technique accessories ............................................... 17
3.2 Guidelines and standards............................................................................. 19
4 Installation requirements ................................................................... 20
4.1 Ambient conditions ....................................................................................... 20
4.2 Floor space requirements and weight .......................................................... 21
4.3 Energy supply ............................................................................................... 22
4.4 Gas supply ................................................................................................... 23
4.5 Gases in graphite tube technique ................................................................ 23
4.5.1 Gases for flame technique ........................................................................... 23
4.6 Laboratory fume hood .................................................................................. 24
4.7 System layout and general view .................................................................. 25
5 Functions and design of the contrAA 700 ....................................... 27
5.1 Physical measuring principle of HR-CS AAS ............................................... 27
5.2 Xenon lamp .................................................................................................. 29
5.3 Graphite tube atomizer ................................................................................. 30
5.3.1 Graphite tube furnace................................................................................... 31
5.3.2 Gas flows in furnace shroud ......................................................................... 32
5.3.3 Graphite tube variations, furnace parts and inserts ..................................... 33
5.3.4 Radiation sensor .......................................................................................... 34
5.3.5 Furnace camera ........................................................................................... 34
5.4 Accessories for graphite tube technique ...................................................... 35
5.4.1 Autosampler AS-GF ..................................................................................... 35
5.4.2 Solid autosamplers SSA 600 and SSA 6z ................................................... 36
5.5 Flame system ............................................................................................... 37
5.5.1 Automatic gas control system ...................................................................... 37
5.5.2 Burner-nebulizer system unit ....................................................................... 37
5.5.3 Burner and flame type .................................................................................. 40
5.5.4 Sensors ........................................................................................................ 40
5.6 Accessories for flame technique .................................................................. 41

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Table of contents

5.6.1 AS-F and AS-FD autosamplers .................................................................... 41


5.6.2 JUN-AIR 6/S piston compressor .................................................................. 42
5.6.3 SFS 6 injection module ................................................................................ 42
5.6.4 Scraper – Automatic burner head cleaner for nitrous oxide flame ............... 43
5.6.5 HPT burner head .......................................................................................... 44
5.7 Supplementary accessories to Hg/hydride systems .................................... 44
6 Installation and start-up .................................................................... 45
6.1 Utility supply and control terminals ............................................................... 45
6.2 Installing and connecting the contrAA 700 ................................................... 47
6.3 Installation and start of ASpect CS software ................................................ 48
6.4 Graphite tube technique ............................................................................... 48
6.4.1 Terminals in sample compartment for graphite technique ........................... 48
6.4.2 Software presettings for graphite tube technique ......................................... 50
6.4.3 Inserting the graphite tube into the graphite tube furnace............................ 51
6.4.4 Graphite tube formatting ............................................................................... 52
6.4.5 Cleaning the graphite tube / cleanout........................................................... 53
6.5 Completing and installing the AS-GF autosampler ...................................... 54
6.5.1 Installing AS-GF ........................................................................................... 54
6.5.2 Adjusting the AS-GF ..................................................................................... 56
6.5.3 Uninstalling the autosampler AS-GF ............................................................ 58
6.6 Flame technique ........................................................................................... 59
6.6.1 Flame technique terminals in sample compartment..................................... 59
6.6.2 Software presettings for flame technique ..................................................... 60
6.6.3 Installation for manual sample feeding ......................................................... 60
6.6.4 Installation for continuous operation mode / with samples delivered by
autosampler .................................................................................................. 63
6.6.5 Uninstalling the autosampler AS-F/AS-FD ................................................... 66
6.6.6 Installation of SFS 6 injection module .......................................................... 66
6.6.7 Replacement of burner ................................................................................. 67
6.6.8 Add-on installation of scraper ....................................................................... 67
6.6.9 Operation of the HPT burner head ............................................................... 69
6.7 Starting the contrAA 700 with accessory units up ........................................ 69
6.7.1 Turn-on sequence, daily start of work .......................................................... 69
6.7.2 Turn off sequence......................................................................................... 70
7 Care and maintenance ...................................................................... 71
7.1 Maintenance summary table ........................................................................ 71
7.2 Basic system unit.......................................................................................... 73
7.2.1 Fuse change ................................................................................................. 73
7.2.2 Reactivating the safety circuits of the cooling water circuit .......................... 73
7.2.3 Cleaning the sample compartments ............................................................. 74
7.2.4 Removing and installing the xenon lamp...................................................... 75
7.2.5 Check cooling water level ............................................................................. 76

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Table of contents

7.3 Maintaining the graphite tube furnace .......................................................... 78


7.3.1 Cleaning the furnace windows ..................................................................... 78
7.3.2 Cleaning the graphite surfaces .................................................................... 79
7.3.3 Cleaning and changing the graphite tube .................................................... 80
7.3.4 Replacing the electrodes and the furnace jacket ......................................... 80
7.4 Burner-Nebulizer System ............................................................................. 85
7.4.1 Disassemble burner-nebulizer system unit .................................................. 86
7.4.2 Clean burner ................................................................................................. 87
7.4.3 Clean Nebulizer ............................................................................................ 89
7.4.4 Clean mixing chamber.................................................................................. 89
7.4.5 Clean siphon ................................................................................................ 90
7.4.6 Assemble burner-nebulizer system unit ....................................................... 90
7.4.7 Cleaning the sensor of the burner ................................................................ 91
7.5 Autosampler AS-GF ..................................................................................... 92
7.5.1 Washing the dosing tube .............................................................................. 92
7.5.2 Servicing the dosing tube ............................................................................. 93
7.5.3 Replacing the metering syringe .................................................................... 95
7.5.4 Clean-up after cup overflow ......................................................................... 96
7.6 Automatic samplers AS-F, AS-FD ................................................................ 96
7.6.1 Washing the sample paths ........................................................................... 96
7.6.2 Washing the mixing cup of the AS-FD ......................................................... 96
7.6.3 Replacing the canulas and guide on the autosampler arm of the AS-FD .... 97
7.6.4 Replacing the canula on the autosampler arm of the AS-F ......................... 97
7.6.5 Replacing the intake tube ............................................................................. 98
7.6.6 Replacing the tube set for diluent and washing liquid at the AS-FD ............ 98
7.6.7 Clean-up after cup overflow ......................................................................... 98
7.7 Compressor JUN-AIR 6/S ............................................................................ 99
8 Transportation of the contrAA 700 ................................................. 100
9 Disposal ............................................................................................ 101
10 Abbreviations / terms....................................................................... 102
11 EC Declaration of Conformity ......................................................... 104

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Index of figures

Index of figures
Fig. 1 Dimensional front-side view of contrAA 700 .......................................................25
Fig. 2 Top-side dimensional view of contrAA 700 ........................................................26
Fig. 3 Layout view of contrAA 700 ................................................................................26
Fig. 4 Schematic comparison of physical measuring principles of LS AAS and HR-CS
(with flame techniques) .......................................................................................27
Fig. 5 Optical path in contrAA 700 ................................................................................28
Fig. 6 Xenon lamp without housing ..............................................................................29
Fig. 7 View of graphite tube atomizer ...........................................................................30
Fig. 8 Graphite furnace structural view .........................................................................31
Fig. 9 Primary and Secondary Gas flows in the Graphite Tube Furnace .....................32
Fig. 10 Graphite tube furnace shroud .............................................................................33
Fig. 11 Graphite tube variations .....................................................................................33
Fig. 12 Furnace jacket, adapters and inserts .................................................................34
Fig. 13 Autosampler AS-GF ...........................................................................................35
Fig. 14 Solid sampler ......................................................................................................36
Fig. 15 Setup of the burner-nebulizer system.................................................................38
Fig. 16 Nebulizer mixing chamber burner system ..........................................................39
Fig. 17 Burner types .......................................................................................................40
Fig. 18 Autosampler AS-FD with separate Fluidik module .............................................42
Fig. 19 SFS6 injection module ........................................................................................43
Fig. 20 Scraper mounted to 50-mm burner head ...........................................................43
Fig. 21 HPT burner head ................................................................................................44
Fig. 22 Main power switch and connector strip terminals for utility supplies and controls
on the right-hand side of the contrAA 700 ..........................................................45
Fig. 23 Connector strip with supply and control connector terminals .............................46
Fig. 24 Rear panel view of contrAA 700 with ports and terminals for gas and electric
power supply, including fuse holders .................................................................46
Fig. 25 Elements in sample compartment for graphite tube technique ..........................48
Fig. 26 Terminals at graphite tube furnace .....................................................................49
Fig. 27 Preview screen of ASpect CS with graphite-tube related setting options ..........50
Fig. 28 FURNACE / CONTROL window ...............................................................................51
Fig. 29 Graphite tube furnace open with graphite tube installed ....................................52
Fig. 30 Installing the AS-GF ...........................................................................................54
Fig. 31 Aligning the AS-GF with the furnace using the set screw and adjusting screw 155
Fig. 32 AS-GF adjustment ..............................................................................................56
Fig. 33 Terminals at the burner-nebulizer system unit available for flame technique ....59
Fig. 34 Terminal facilities provided in sample compartment walls .................................60
Fig. 35 Flame technique, manual sample delivery .........................................................61
Fig. 36 Flame mode, continuous with autosamplers AS-FD and SFS 6 ........................63

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Index of figures

Fig. 37 Rear of the autosampler AS-FD ......................................................................... 65


Fig. 38 Dosing unit at the Fluidik module of the AS-FD ................................................. 65
Fig. 39 SFS 6 installed at the contrAA 700 for manual sample delivery ........................ 66
Fig. 40 Screws in front-side burner jaw .......................................................................... 68
Fig. 41 Fixing rail with burner mounted / knurled thumb screws at scraper ................... 68
Fig. 42 HPT burner head mounted on the mixing chamber ........................................... 69
Fig. 43 Safety circuit switch for hardware ....................................................................... 74
Fig. 44 Xenon lamp housing ........................................................................................... 76
Fig. 45 Xenon lamp, installed ......................................................................................... 76
Fig. 46 Cooling water tank below graphite tube furnace ................................................ 77
Fig. 47 Identical markings at the furnace windows facing upward ................................. 79
Fig. 48 Furnace tools ...................................................................................................... 80
Fig. 49 Deinstalling and taking the burner-nebulizer system unit apart ......................... 86
Fig. 50 Mixing chamber and nebulizer disassembled .................................................... 86
Fig. 51 Withdrawing the nebulizer from the mixing chamber ......................................... 87
Fig. 52 Fittings of the burner........................................................................................... 88
Fig. 53 Burner, disassembled ......................................................................................... 89
Fig. 54 Spacers inserted in burner jaws ......................................................................... 89
Fig. 55 Components of the nebulizer ............................................................................. 91
Fig. 56 Sensor of the burner ........................................................................................... 91
Fig. 57 Window "Autosampler / Function tests" in the ASpect CS software .................. 93
Fig. 58 Dosing tube at the AS-GF .................................................................................. 93
Fig. 59 Dosing unit at AS-GF and AS-FD ....................................................................... 95

contrAA 700 Issue 01/2014 5


Index of tables

Index of tables
Table 1 Dimensions and weights of the contrAA 700 and its system components .........21
Table 2 Power requirements ...........................................................................................22
Table 3 Gases in the Graphite Tube Technique .............................................................23
Table 4 Gases for flame technique ..................................................................................24
Table 5 Laboratory fume hood requirements ..................................................................24
Table 6 Use and sample volume of different graphite tube variations ............................33
Table 7 Maintenance summary table ..............................................................................72
Table 8 Fuses ..................................................................................................................73

6 Issue 01/2014 contrAA 700


Fundamental Information

1 Fundamental Information
1.1 Intended Use
The contrAA 700 is an atom absorption spectral photometer to allow sequential analysis of
metal and non-metal traces in liquid and dissolved samples. Running under PC control, the
contrAA 700 provides a high resolution continuum source atom absorption spectrometer tool
for flame, hydride and graphite tube technique. It is intended for determination of metal and
non-metal traces in liquid and dissolved samples.
Combined with an autosampler, the contrAA 700 can work as a multi-element automatic
setup for routine analytical jobs. It performs an initial calibration of the elements under
analysis by sequentially processing the related calibration standards at first and sequentially
processing the actual samples in a second step. Hence, after each sample measurement,
the results are available for all elements that were subject to analysis.
All operating selections such as spectrometer settings, burner height and fuel gas values
and temperature-versus-time programs for electro-thermic atomization are automatically
assigned in accordance with actual methodology parameters so they may differ from
element line to element line. The control software relies on the Windows operating system to
accomplish full operation control of the basic equipment unit and connected accessory items
plus related data acquisition and data evaluation processes. Including the analytical back-
ground is automatically determined and simultaneously available on the analysis line. The
control software includes standard values for methodological settings that relate to an
analysis line. Prefabricated line parameter settings are available for each measurable
element of the periodic table (also referred to as "cookbook”) to facilitate getting started in
analytics. They can be used as an initial base for editing one’s own multi-element
methodologies. The control software also provides comprehensive representation and
storage capabilities for signals and parameters measured, for GLP-compliant logging and
various quality control options, including a possibility to maintain and update quality control
cards.

1.2 User manual conventions


The following warning and information symbols are used in this manual:

WARNING
Indicates a potentially hazardous situation.
If it is not prevented, death or serious injuries (incapacitation) may result.

CAUTION
Indicates a potentially hazardous situation.
If it is not prevented, minor or moderate injuries and material damage may result.

CAUTION! HOT SURFACE!


Touching the hot surface can cause burns.

WARNING! DANGER OF ELECTRIC SHOCK IF TOUCHED!

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Fundamental Information

IMPORTANT
Indicates application hints and other especially useful information without any resulting
hazardous or damaging situations.

The manual uses the following conventions:


 Chapters and illustrations are numbered consecutively.
 Every illustration has its own caption.
 Instructions for actions/steps of operation are numbered consecutively and united in
action units.
 Menu and option sequences in software are subdivided by "/", e.g. FILE / OPEN.
Buttons or keys are marked by square brackets, e.g. [OK].

8 Issue 01/2014 contrAA 700


Safety instructions

2 Safety instructions
For your personal safety and for the trouble free and safe operation of the contrAA 700, read
this section carefully before starting it up.
Follow all safety instructions given in this manual and pay attention to all messages and
notes displayed on the screen by control software.
In addition, follow the safety instructions for system components of other manufacturers (e.g.
PC, printer, autosampler) supplied together with the device. In particular, read and follow the
safety notes given on the labels of reagents and the information on their handling, storage
and disposal.

INTENDED USE!
The contrAA 700 may only be used for the atomic absorption spectrometry techniques as
described in this manual.

LOCAL REGULATIONS!
Comply with the local safety regulations relevant to the operation of the device (e.g.
occupational safety regulations, accident prevention regulations).
References to potential hazards made in this manual do not replace the relevant
occupational safety regulations to be complied with.

PERSONNEL!
The contrAA 700 may only be operated by qualified persons who have been additionally
trained for this type of work and have familiarized with the information given in this manual
and in the accompanying manuals of accessories and system components.
Work on electrical equipment may only be performed by qualified and approved electricians.

EXPLOSION AND FIRE PROTECTION


The contrAA 700 must not be operated in explosion-risk environments.
Smoking is not allowed in the operating room of the contrAA 700.
The operator is responsible for establishing a control regime that ensures that nitrous oxide
and acetylene connections are leak-proof.

INSTALLATION AND INITIAL START-UP


Work for installation, assembly and repair of the contrAA 700 may not be performed by
anyone other than Customer Service personnel of Analytik Jena AG or technicians
specifically authorized by Analytik Jena AG. Any unautho-rized intervention will create
potential danger to users and in terms of operational safety and will restrict actual warranty
claims.

SHUTDOWN IN EMERGENCY SITUATIONS!


Switch off the contrAA 700 with the power switch on the right side panel. Disconnect the
power cable from the power outlet.
Switch off installed system components with the power switch of the connected multiple
socket outlet, which should be placed in a way to allow fast access.
Caution! In doing so, there is the risk of data loss and damage to the operating system on
the PC!

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Safety instructions

ELECTRIC SHOCK!
The contrAA 700 is powered by electrical voltage. Extremely hazardous electrical
voltages are applied to several components in the system!
To ensure the specified class I product protection standard (PE conductor connection), the
line power plug may not be connected to any power point other than a CEE-compliant line
socket. The electric PE device must not be rendered ineffective by adding cable extensions
without a protective conductor (→ section "Energy supply” p.22).
To perform work on its electrical system, turn power to the contrAA 700 off in all cases and
detach the line power plug. There will be no safe cutting of line power supply, unless the
line plug is removed. After turning off with the main power switch, some parts of the
spectrometer, including its outlet socket, will continue to carry line voltage.
Only service technicians of Analytik Jena AG and authorized specialists are allowed to
remove the back panel of the device.
Only service technicians of Analytik Jena AG and specially qualified electricians are allowed
to open system components, particularly the housing of the xenon lamp.

ELECTRIC SHORTS TRIGGERED BY PIECES OF JEWELLERY


There is potential danger of electric shorts between the two furnace parts or a furnace part
and the furnace substructure. Shorting pieces of jewellery will heat up strongly and are likely
to cause skin burns.
Do not wear (metallic) jewellery (notably, no necklaces) while working at or with the
contrAA 700. Disregarding this rule may imply potential danger of shorts with the electrically
heated graphite tube.

OPERATING MATERIALS, HAZARDOUS SUBSTANCES


The operator is responsible for the selection of the substances used in the process as well
as for their safe handling. This applies, in particular, to radioactive, infectious, toxic,
corrosive, combustible, explosive and otherwise hazardous substances.
In handling hazardous substances, comply with the relevant local safety regulations and
guidelines.
Always observe the notes given on labels.
Always use labeled vessels, protective goggles and rubber gloves.
The contrAA 700 may only be operated under an active laboratory fume hood to withdraw
ozone, combustion gases of samples, and toxic and combustible byproducts of sample
preparation.
Treat biological samples in compliance with the relevant local regulations for the handling
of infectious material.
The operator is responsible for disposing of waste material, such as filter residues of the
compressor, in an environmentally conscious manner and in compliance with the relevant
local regulations.

COMBUSTIBLE AND EXPLOSIVE GASES


Be careful if acetylene is escaping! Acetylene is an explosive gas that is easily detected by
its smell.
Shut down the contrAA 700 if gas paths are leaking and fuel gas valves or safety devices of
the automatic gas control system are defective.
Keep vessels holding combustible solvents or samples containing volatile and combustible
substances away from the flame.

10 Issue 01/2014 contrAA 700


Safety instructions

XENON LAMP AND LAMP HOUSING


Inside the quartz bulb of the xenon lamp, there is an overpressure of 2 MPa, which may
increase up to 7 MPa in operation!
Only service technicians employed with or authorized by Analytik Jena AG are allowed to
open the lamp housing.

UV RADIATION AND DAZZLING HAZARD


Protect your eyes!
Never look at the radiation of the xenon lamp or the burner flame without wearing UV
protective goggles.
In flame mode, always keep the door of the sample compartment closed while the flame is
ignited.
The xenon lamp, in particular, emits very intense light in the visible and UV region!

OZONE
Inadmissibly high toxic ozone concentrations are produced by the interaction of the UV
radiation of the xenon lamp and the N2O burner flame with the ambient air.
The contrAA 700 may only be operated under an active fume hood.

OPERATION OF HIGH-PRESSURE GAS CYLINDERS AND GAS PLANTS


Fuel gas and oxidant are supplied by high-pressure gas cylinders or local gas plants.
Make sure to fully comply with the local safety regulations and guidelines relevant to the
operation of high-pressure gas cylinders and gas plants.
High-pressure tubes and pressure-reducing valves may only be used for the specified
gases.
Keep supply tubes, fittings and pressure-reducing valves for N2O (nitrous oxide) free from
grease.
Weekly perform leak tests of all gas connections including nebulizer and mixing chamber.
Carefully ventilate the cylinder location after having replaced the gas cylinder.

HIGH TEMPERATURES
In flame mode, high temperatures are generated.
Allow for appropriate cooling times!
Do not touch hot components during or directly after measurements.
Allow for appropriate cooling times before undertaking maintenance or replacing such
components as burner head and lamps.
Keep combustible materials away from the device.

VENTILATION
Take care to ensure that the ventilation systems on the contrAA 700 and the accessory units
are always functional. Covered vents, ventilation slots, etc. may result in malfunction or
damage to the device.

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Safety instructions

CLEANING AND MAINTENANCE


Except for the work described in Section "Care and maintenance” p.71, service,
maintenance and repair work on the contrAA 700 may only be carried out by service
technicians employed with or authorized by Analytik Jena AG. Non-compliance involves the
risk of misalignment or damage to the device.
To externally clean the contrAA 700, only use a slightly moistened, but not dripping cloth.
For cleaning in the sample compartment of the contrAA 700, take suitable precautions,
especially for the protection against contaminated and infectious materials.

FLAME MODE
Do not use pure oxygen or air enriched with oxygen as oxidant.
Ensure that the flame sensor is always functional.
If gas paths are leaking, or if detect a fault on the fuel gas valves or the safety devices of the
automatic gas control system, switch off the contrAA 700 until the fault has been remedied.
Use the acetylene cylinder only in an upright position and secured against falling over. When
the cylinder pressure drops below 100 kPa, replace the cylinder to prevent acetone from
entering the automatic gas control system.
Keep vessels holding combustible solvents and samples containing volatile, combustible
constituents away from the flame.
Ignite and operate the flame only with the sample compartment door being closed.
Never leave burning flames unattended.
The nebulizer pressure must not drop below 70 kPa.
When working with the nitrous oxide flame, use a scraper or remove carbon deposits
manually with the scraper from the burner slot. For combustion gas flows exceeding 250
NL/h pay attention to stubborn deposits. Remove these where necessary to ensure the
functionality of the scraper.
When carrying out maintenance work on the nebulizer/burner system, clean all contaminated
parts.

GRAPHITE TUBE TECHNIQUE


Use only that type of inert gas which this User Manual specifies for graphite tube technique.
Do not look into the graphite tube opening, unless you have put on safety goggles. Splashes
of sample matter and hot graphite particles may cause eye or face injury.

REPLACEMENT OF GRAPHITE TUBES, SPARE PARTS


Use solely spare parts from Analytik Jena AG in all cases.
Graphite tubes for the contrAA 700 are custom-manufactured units and are only available
(for ordering) from Analytik Jena AG. Refrain from using graphite tubes of any other type.
Failure to comply may damage the contrAA 700.

SENSITIVE ELECTRONICS
System components must not be electrically connected to, or disconnected from, the
contrAA 700, unless they are de-energized. This also applies to electrical connection
between different system components.

12 Issue 01/2014 contrAA 700


Specifications

3 Specifications
3.1 Technical data
3.1.1 Technical data of contrAA 700
Optical system
Reflecting optics with protective coating and optical system in light-proof casing

Monochromator Echelle grating double monochromator of F=380 mm focal length, with variable intermediate
slit; preliminary monochromator with quartz prism. Wavelength selection is accomplished via
extra neon radiation source reflected into the beam
Wavelength range 185 – 900 nm
Spectral band width 2 pm at 200 nm
Grating Echelle grating
Optical bench Optics mounted to solid base plate for stability and robustness.
encased photometer Protection against humidity and waste gas.
Detector Two-dimensional FFT backside illuminated CCD with high quantum efficiency and enhanced
UV sensitivity

Lamp
Xenon short-arc lamp with UV arc in hot spot mode; automatic hot-spot tracking;
simultaneous drift correction

Lamp current 9-16 A / 8 A in stand-by mode


Operating mode DC, for monitoring of lamp operating life and ignition pulses
Power supply Power supply unit integrated in spectrometer

Display modes
Absorption 0 … 3.99
Concentration Range of values: 5-place (0.001 … 99999), freely selectable unit
Energy 0 - 35000 counts

Signal analysis
Time resolved Mean value, maximum value of absorption, integral of absorption
Spectrally resolved Spectrum with 50 to max. 200 pixels

Power supply
Power requirements 200 / 220 / 240V ±10% factory-selectable
Frequency 50/60 Hz
In-house line fuse Fusible link ≥ 35 A inert
protection, installation No automatic circuit breakers!
side
Typical mean power Basic unit: 2100 VA
consumption Basic unit with PC, monitor and autosampler: 2800 VA
Maximum current 52 A for 8 s or 85 A for 1 s, respectively
consumption

contrAA 700 Issue 01/2014 13


Specifications

Outlet socket Same as inlet socket (200/220/240V ±10%, 50/60Hz)


for connection of accessory units: PC, compressor, hydride system
Overvoltage category II acc. to DIN EN 61010-1
Pollution degree 2 acc. to DIN EN 61010-1
Protection class I
Internal protection IP 20
standard

When connecting components other than a PC or monitor to the output socket, there is the
risk of exceeding the admissible limit value of leakage current.

Instrument fuses
G-type fuse links (5×20 mm²) under IEC 60127.

Number of fuse Type Protected current circuit


F3 T 6,3 A/H Power socket
F4 T 6,3 A/H Power socket
F5 T 6,3 A/H Spectrometer
F6 T 6,3 A/H Spectrometer
F7 T 3,15 A XE power supply
F8 T 3,15 A XE power supply

Furnace fuse
Type Protected current circuit
TR5-T 100 mA Graphite tube furnace

Line input fusing


Line input fuses may not be replaced by anyone other than Customer Service personnel of
Analytik Jena AG or technicians duly authorized to handle such jobs by Analytik Jena AG.
gL-G-fuse inserts (10×38 mm²) according to 60947-3.

Number of fuse Type Protected current circuit


F1 32 A/T Line power input
F2 32 A/T Line power input

Ambient conditions
acc. to DIN ISO 90022-2:2003 / 01

Corrosion protection Device is corrosion-proof against the samples to be analyzed


Operating temperature +10 °C to 40 °C
Humidity Max. 93% at +40 °C
Storage temperature –40 °C to +70 °C
(desiccant)

Dimensions and weights


Weight 185 kg
Dimensions 1200 mm × 570 (645) mm × 765 mm
(W x H x D):
Transportation Only with transporting handles firmly screwed in.

14 Issue 01/2014 contrAA 700


Specifications

3.1.2 Control computer data


Computer PC Pentium 1 GHz with 512 Mbyte RAM
(minimum requirements) 40 Gbyte hard disk,
43-cm color monitor (17")
VGA graphic card
800x600 pixels resolution or higher ,
CD ROM
Ports:
– Mouse port
– Printer port
- USB port (USB 1.1 or 2.0) for contrAA 700
Printer HP DeskJet Ink Jet Printer
HP Laser Jet Laser Printer
Operating system Windows XP Professional

3.1.3 Data for graphite tube technique


Graphite Tube Furnace
Type of sample Liquid
Solid
Type of tube IC tube (wall atomization)
IC tube with 1-PIN platform
IC-Rohr solid sample
All tube types are pyro-coated.
Volume max. 50 µL
Temperature setting Temperature can be set between room temperature and
3000 °C in steps of 1 °C
Temperature-time Up to 20 steps can be freely programmed within determined limits, 0 to 999 s/step, in
programming (Furnace intervals of 1 s
program) Temperature increase (Ramp):
1°C/s to 3000°C/s linear and max. non-linear ramps (Full Power FP / No Power NP)
Control of inert gas and aux. gas
Inserting injection and enrichment steps
Determining starting point for autozero and integration
Cooling water Integrated cooling, sediment-free 20 to 40°C
Inert gas Argon 4.8 and superior
Permitted components:
Oxygen ≤ 3 ppm
Nitrogen ≤ 10 ppm
Hydrocarbon ≤ 0.5 ppm
Humidity ≤ 5 ppm
Consumption max. 2 L/min
(depending on temperature-time program)
Inlet pressure 0.6 to 0.7 MPa

contrAA 700 Issue 01/2014 15


Specifications

Safety circuits report if transformer for furnace heating is overheated


errors if the graphite tube is broken
if the graphite tube furnace is overheated
if the graphite tube furnace is open during operation
if there is a shortage of cooling water
if the inlet pressure of the inert gas is too small

Autosampler AS-GF
Autosampler with Dilution Function, complete PC Control

Sample tray 108 positions


Sample cups 100 pieces, 1.5 mL
Special cups 8 pieces, 5 mL
Pipetter volume 1 to 50 µL
Wash volume 0.5 mL, number of wash cycles can be selected
Program methods Standard
Modifier
Dilution
Addition
Automatic enrichment
Mass 7.2 kg

Cooling
A cooling system requiring no scheduled maintenance which is integrated with the
spectrometer for heat removal from the Xe-lamp and the graphite furnace, working based on
the water-air exchange principle.

Accessories for Direct Solid Analysis


SSA 600 Solid autosampler for automated mode
SSA 6 Solid autosampler for manual mode

3.1.4 Data for flame technique


Types of Flame
Acetylene/air Single-slot burner 50 mm, coded (standard)
Single-slot burner 100 mm, coded (optional)
Acetylene/nitrous oxide Single-slot burner 50 mm, coded

Oxidant
Compressed air and N2O Inlet pressure: 300 to 600 kPa
(nitrous oxide)
Nebulizer flow rates
Air 400 to 600 NL/h
N2O 320 to 480 NL/h
Auxiliary oxidant 30 to 315 NL/h
(air or N2O)
Total oxidant
Air 400 to 700 NL/h
N2O 320 to 700 NL/h

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Specifications

Fuel gas
Acetylene Inlet pressure: 80 to 150 kPa
Consumption: 40 to 315 NL/h

Nebulizer
Operating principle Pneumatic concentric jet nebulizer
Material Platinum/Rhodium tube, PEEK nozzle, PEEK cap
Nebulizer 0.7 Flow rate 4 to 7 mL/min

Siphon Monitoring
Operating principle Float, corrosion-proof

Burner Adjustment
Height 4 to 16 mm, automated
Depth 3 mm, manual
Rotation 0 to 90 degrees, manual

Safety Circuits
Monitoring Burner and burner type
Fuel as pressure
Siphon fill level
Flame
Oxidant inlet pressure (air and N2O)

3.1.5 Data regarding flame technique accessories


Autosampler AS-F
Autosampler without dilution function, completely PC-controlled

Sample tray 139/ 15


Sample cups 129 pieces, 15 mL
Special cups 10 pieces, 50 mL
Sample tray 54/ 50
Sample cups 54 pieces, 50 mL
Power supply Via AAS basic instrument
Wash bottle 2L
Mass 6.5 kg

Autosampler AS-FD
Autosampler with dilution function, completely PC-controlled

Sample tray 139/ 15


Sample cups 129 pieces, 15 mL
Special cups 10 pieces, 50 mL
Sample tray 54/ 50
Sample cups 54 pieces, 50 mL
Dosing unit in the Fluidik module 5 mL

contrAA 700 Issue 01/2014 17


Specifications

Power supply Via AAS basic instrument


Wash bottle 2L
Bottle for diluent 2L
Mass (total) 10.0 kg
Autosampler 6.5 kg
Fluidik module 3.5 kg

Injection Module
PC-controlled

Sample volume for single analysis 300 µL (minimum volume)


Power supply Via spectrometer

Piston Compressor JUN-AIR 6/S Standard


Tank capacity 15 L
Dimensions (diameter × height) 400 mm × 480 mm
Power supply 230 V, 50 Hz or
230 V. 60 Hz
Weight 28 kg

Scraper
PC-controlled

Power supply Via spectrometer

Hg/Hydride Systems
HS 60 modular; HS 55 modular; HS 50
Refer to Hg/Hydride Systems user manual.

18 Issue 01/2014 contrAA 700


Specifications

3.2 Guidelines and standards


Protection Class and Degree of Protection
The contrAA 700 is classified in Protection Class I.
The Degree of Protection of the casing is IP 20.

Device Safety
The contrAA 700 complies with the following safety standards
 DIN EN 61010-1 (VDE 0411T.1; IEC 61010-1)
 DIN EN 61010-2-061 (IEC 61010-2-061)

Electromagnetic Compatibility (EMC)


The contrAA 700 has been tested for radio interference suppression and noise immunity. It
complies with the requirements of
 DIN ISO 9022-3:2000
 DIN ISO 9022-32-03-0
 DIN ISO 9022-2:2003/01

EC Directives
The contrAA 700 has been manufactured and tested in compliance with standards that meet
the requirements of EC Directives 2006/95/EG and 2004/108/EG. The device was delivered
in perfect, technically safe condition. To maintain this condition and ensure safe operation,
observe the safety and operating instructions given in this manual. In addition, observe the
operating instructions supplied along with accompanying accessories and system
components of other manufacturers.

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Installation requirements

4 Installation requirements
CAUTION
The device may only be set up, installed and repaired by service technicians employed with
or authorized by Analytik Jena AG. Any unauthorized tampering with the device will limit the
rights to claim under warranty.

For system installation, temporary assistant labour is required. Customer Service personnel
will perform system testing and document the results in a special contrAA 700 test certificate.
The owner/operator will be responsible in connection with anything not directly included in
contrAA 700 delivery, but necessary for normal operation. For contrAA 700 operation, certain
local and specific utility requirements must be met:
 Suitable installation site
 Sufficient floor space
 Ambient conditions
 Supply of fuel gas and oxidant
 Laboratory fume hood
 Mains connection

CAUTION
Pay attention to the instructions given in Section "Safety instructions" p. 9.
See to it that occupational safety regulations are complied with. References to potential
hazards do not replace the valid occupational safety regulations!

Potential hazards when working with the contrAA 700 include:


 Burn hazard by flame and hot burner components
 Hazard from electric current
 UV radiation hazard
 Hazard from the generation of ozone and nitrogen oxides
 Hazard in handling high-pressure gas cylinders
 Hazard from toxic and chemically aggressive substances

4.1 Ambient conditions


 Do not set up the contrAA 700 directly beside a door or window. The installation site
of the contrAA 700 should be free of draft, dust, corrosive vapours and vibration.
 Do not set up the contrAA 700 near sources of electromagnetic interference.
 Avoid direct exposure of the contrAA 700 to sunlight and radiation from heaters. In
extreme cases, provide room air conditioning.
 You are advised to prepare samples and store wet-chemical materials in a separate
room.
 In the operating room of the contrAA 700, smoking is not allowed.

20 Issue 01/2014 contrAA 700


Installation requirements

 Operating temperature range: +10°C to 40°C


 Storage temperature range -40°C to 70°C,
use desiccant.
 Max. operating humidity 93% at 40°C
 Storage humidity 10% to 30%,
use desiccant

4.2 Floor space requirements and weight


 Minimum size of work bench:
1880 mm × 700 mm, height to be selected according to ergonomic aspects
 Carrying capacity of work bench: 230 kg
 Additional floor space for JUN-AIR S6 piston compressor and PC where included
 Bench surface quality: wipe-proof, scratch-proof and corrosion-proof, not moisture-
absorbing
Set up the work bench to allow easy access from all sides.

Component Width [mm] Height [mm] Depth [mm] Weight [kg]


On the work bench
contrAA 700 1180 570(645) 765 185
AS-GF 250 550 380 7,2
AS-F 340 350 460 6,5
AS-FD
Autosampler 340 350 460 6,5
Fluidik module 360 310 165 3,5
HS 60 modular 360 370 240 14
HS 55 modular 360 370 240 14
HS 50 270 210 190 2
Under the work bench
Compressor JUN-AIR ∅ 400 480 28
6/S

Table 1 Dimensions and weights of the contrAA 700 and its system components

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Installation requirements

4.3 Energy supply


WARNING! NOTE CONNECTION DETAILS OF AVAILABLE MAINS
SUPPLY!
Comply with VDE (German Electrical Engineering Association) rules and local provisions
when performing electrical installation work!
The mains connection point must be properly grounded.
Do not use adapters in line power supply cabling.
Do not use automatic circuit breakers.

The contrAA 700 requires single-phase AC current supply for operation. Its current loading
rate can be as high as 85 A at the maximum heating rate for a short time (1 s). During this
phase, line voltage at the contrAA 700 should not drop by more than 6%. If actual values are
found to differ from these specifications, you are requested to consult with us. Adequate
accessory units can be additionally supplied.
For optimal system function, it is essential that mains connection be performed in a proper
manner and using adequate cross-sections for cabling. The mains connection point must be
protected with 35 A inert on the facility side and must have been installed near the operating
site prior to contrAA 700 delivery. The power supply cord is 3 meters long. A CEE surface-
type socket outlet (2-pole + E Blue 5UR 3 206-2 220/32 from Siemens) is provided under the
contract of delivery.
All other components of the contrAA 700 (e.g. PC, printer, etc.) are connected to the same
phase as the basic system unit via a 5-position manifold that is plugged into a socket on the
back of the contrAA 700. If you use your own PC and printer configuration and want to
connect this configuration via the 5-position manifold, then make sure that the specified limit
value for permissible working current is not exceeded. To prevent dramatic variations in
voltage level, you should not connect the contrAA 700 to a current circuit that is shared with
other power-intensive consumers.

Power Requirements
Voltage 200 / 230 /230 V ±10% factory-set to Customer request, or
such other voltage level as provided for in contract of delivery
Frequency 50/60 Hz
or such other frequency as specified in contract of delivery
Mean typical power 2100 VA
consumption
Maximum current 85 A for 1 second or
consumption 52 A for 8 seconds, respectively
Fusing (on line side) 35 A, fusible link, inert, single-phase
Do not use automatic circuit breakers!
Power consumption of 700 VA while cell is heated
hydride subsystem 400 VA in steady operation

Table 2 Power requirements

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Installation requirements

4.4 Gas supply


4.5 Gases in graphite tube technique
The required inert gas is used to protect the graphite components of the atomizer, which are
subjected to extreme temperatures. The inert gas is used as a means of transport for the
pyrolysis components accrued during the analysis. The purity of the inert gas is extremely
important for the analysis and for the lifetime of the graphite tube.
By additionally inserting oxidizing gas (e.g. air or oxygen) during the pyrolysis step, the
pyrolysis of the sample, i.e. the divide off of the matrix components, may be accelerated. The
oxidizing gas is inserted via the "Gas Additional” connector on the device’s rear side.
The gas pressure at the spectrometer must be between 0.6 and 0.7 MPa.

VORSICHT
If the inert gas is supplied by pressure cylinders, these must be secured to the wall in an
upright position with cylinder mounts outside the laboratory space.

The required pressure reducing valve for the inert gas cylinder, and the argon pressure tube
are supplied. The standard tube length is 5 m. If other tube lengths are preferred, please
contact the customer service department at Analytik Jena AG.

Recommended Inert Gas Input Pressure Consumption


Recommended for graphite tube mode: 6 - 7 bar max. 2 L/min (depending on the temperature-
Argon 4.8 or superior time program)
Permitted components:
Oxygen ≤ 3 ppm
Nitrogen ≤ 10 ppm
Hydrocarbon ≤ 0.5 ppm
Humidity ≤ 5 ppm

Table 3 Gases in the Graphite Tube Technique

4.5.1 Gases for flame technique


For the flame technique, oxidant (compressed air and N2O if necessary) and fuel are
required. The purity of the gases is extremely important for the analysis. The piston
compressor JUN-AIR 6/S can be used to supply the compressed air. If compressed air is
supplied by the operator’s own compressed air connection, please consult the service
department at Analytik Jena AG. N2O is supplied by pressure cylinders or by an existing
mains line.

CAUTION! INSTALLATION OF HIGH-PRESSURE GAS CYLINDERS


If fuel gas supply is from high-pressure cylinders, the cylinders must be installed upright in
gas cylinder cabinets or mounted to the wall with cylinder holders outside the laboratory
room.

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Installation requirements

The pressure gas tubes are supplied with the device, the pressure-reducing valves are
optional.
 Tube length for connection to cylinder 5m
 Tube length for connection to compressor 5m
On request, you may also use tubes of other lengths. If you intend to do so, please consult
the Service Department of Analytik Jena AG.

Fuel gas and oxidant Inlet pressure Consumption


Compressed air, oil-free, grease-free, 4 - 6 bar Max. 700 NL/h
particle-free
N2O, oil-free, grease-free, purity 2.5 4 - 6 bar Max. 700 L/h
Acetylene 0,8 – 1,5 bar Max. 315 NL/h
Purity 2,5 (for flame photometry): better than 99.5 Vol% relative
to C2H2, without acetone.
Minor constituents: Hydrogen compounds of As, S and P

Table 4 Gases for flame technique

4.6 Laboratory fume hood


CAUTION! TURN SUCTION DEVICE (FUME HOOD) ON FOR NORMAL
OPERATION!
Do not operate the contrAA 700 without fume hood!
Direct waste gas to the outside and avoid blockage!

The laboratory fume hood shall exhaust noxious combustion residues of the flame and any
produced ozone. Ozone is produced by the interaction of air and the UV radiation emitted by
the xenon lamp and the burner flame. The used fume hood should be made of material that
is resistant to heat and corrosion. The first six meters of the fume hood should be made of
metal.

Parameters Properties
Material V2A
Exhaust capacity with nitrous oxide flame Approx. 8 to 10 m3/min
Exhaust capacity with air flame Approx. 5 m3/min
Hood opening Approx. 200 × 200 mm
Distance to top edge of device Approx. 200 to 300 mm
Tube diameter Approx. 100 to 120 mm

Table 5 Laboratory fume hood requirements

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Installation requirements

4.7 System layout and general view


The contrAA 700 provides a compact tool that has been conceived for desktop operation. Its
footprint requirements follow from the total of components included in a given analytical
workplace.
Located beside the basic system unit are the PC with monitor, printer, keyboard and mouse
pad. The PC and printer can also be placed on a standard available PC trolley.
The samplers for the flame mode AS-F or AS-FD are hung in the right sample chamber of
the contrAA 700. The storage bottle for wash liquid of the AS-F or the Fluidik module of the
AS-FD are placed next to the AAS device.
The accessories for the graphite tube technique – autosampler AS-GF for dissolved samples
or Solid Autosampler SSA 6 or SSA 600 for solid samples – are hung in the left sample
chamber.
For placement of accessory items for Hg/hydride technique (HS 55/60 modular), an extra
table on the left-hand side in front of the contrAA 700 is used.
Located on the floor in a position directly beside the product are these components:
 collector flask for undispersed sample liquid, washing liquid of autosamplers and
residual liquid of mercury hydride subsystem
 JUN-AIR 6/S compressor.

Fig. 1 Dimensional front-side view of contrAA 700

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Installation requirements

Fig. 2 Top-side dimensional view of contrAA 700

Fig. 3 Layout view of contrAA 700

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Functions and design of the contrAA 700

5 Functions and design of the contrAA 700


5.1 Physical measuring principle of HR-CS AAS
The measuring principle of both High Resolution Continuum Source Atomic Absorption
Spectrometry (HR-CS AAS) and classical Line Source AAS (LS AAS) is based on the
absorption of primary radiation by the analyte atoms in their ground state. The measured
absorbance signal constitutes a measure of concentration of the respective element in the
analyzed sample.
Every AAS device consists of the following basic modules:
 Light source
 Atomizer
 Monochromator
 Detector
 Evaluation unit (PC)

Emission (HCL) Emission (Xe)

Absorption(Flame) Absorption(Flame)

Monochromator Monochromator
(low resolution) (high resolution)

Detector Detector
(Photomultiplier) (CCD line)

Signal of line source Signal of continuum source

Fig. 4 Schematic comparison of physical measuring principles of LS AAS and HR-CS


(with flame techniques)

Light source
In HR-CS AAS, the element-specific light source of classical AAS (hollow cathode lamp
(HKL)) is replaced by a single continuum source, a xenon short-arc lamp, which is used for
all elements and lines. Due to the special electrode geometry of the xenon short-arc lamp, a
hot arc spot ("Hot-Spot”) is caused that ensures very high radiation density and continuous
emission throughout the entire spectral range (190 – 900 nm). This way, all analysis lines of
interest are available without any restrictions and at any time – concerning both the
resonance wavelengths of the elements to be analyzed and all secondary wavelengths
without the technical limitations caused by specific properties of the HCL, such as exit
window and emission intensity. In addition, absorption lines or bands of diatomic molecules
(PO, CS, ...) can be used analytically for element determination.

Atomizer
The contrAA 700 is designed to allow the following atomization techniques:

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Functions and design of the contrAA 700

 burner and nebulizer system in flame mode


 cross-heated graphite tube in EA mode
 cell unit in hydride and Hg cold vapour technique
 SSA 600 solid sampler combined with a graphite tube
The graphite tube atomizer and the burner and nebulizer system (BZS) are firmly installed in
the sample compartment of the contrAA 700. For this reason, no retrofitting is required for
conversion to another atomization technique.
The cell unit of Hg/hydride systems must be mounted onto the mixing chamber in lieu of the
burner head.
Alternatively, hydride technique may be combined with graphite tube technique. HydrEA
technique ("Hydride technique with electrothermic atomization”) relies on the fact that metal
hydrides or mercury vapour are enriched and atomized at 2100°C or 800°C, respectively, on
a preheated graphite tube which is coated with indium or gold.
With its graphite tube technique, the contrAA 700 is also suited for direct solid sample
analysis with special SSA 600 sample peripherals. Through direct determination of trace
elements in a solid sample, the otherwise time-consuming and contamination-inducing
procedures for sample decomposition – a major error source in analytical solution routines –
are excluded.

Monochromator
The selectivity of the analysis is realized by a high-resolution double monochromator based
on a prism and an Echelle grating monochromator. In this way, a very compact design and a
high spectral resolution (high spectral dispersion of radiation) of λ/Δλ =145 000 is achieved,
which corresponds to a spectral band width of < 2 pm per pixel at 200 nm. The
monochromator is wavelength-stabilized by the use of an integrated neon source. The
wavelength accuracy is achieved by monochromator calibration, when a wavelength is
adjusted based on the physically defined neon lines.

Fig. 5 Optical path in contrAA 700

Detector
In place of the exit slit of the monochromator, which in classical LS AAS isolates the analysis
line from other radiation emitted by the HCL before it reaches the detector, in HR-CS AAS a
low-noise, UV-sensitive semiconductor detector is used (CCD line detector). This detector
does not only detect the intensity on the analysis line, but also its spectral neighborhood. In
this way, a spectral region of up to 1 nm around the analysis line is detected simultaneously
and at a high resolution.

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Functions and design of the contrAA 700

Evaluation unit
Background correction is by polynomial formation through selected reference points. The
selection of these reference points may be performed manually by the user; by default,
however, it is done automatically through software. The reference points are dynamically
selected for every spectrum using a special algorithm and based on criteria ensuring
approximation to the actual baseline on the measuring pixel that is as accurate as possible.
If a fine-structured background overlaps the analysis wavelength, a multivariant method can
be applied. To this end, reference spectra of matrix constituents are used for the polynomial
forming least-squares fit. If atom lines directly overlap with the analysis wavelength, it is also
possible to perform interelement correction (IEC). For this correction, spectral lines are used,
which are adjacent to the interfering element and captured by the observation width of the
detector (e.g.: correction of spectral interference of Fe at the analysis wavelength of Zn at
213 nm or Se at 196 nm).
Lamp drift and all broad-band effects are instantly eliminated from the spectrum by automatic
and simultaneous background correction with correction pixel assignment. In this way, a
simultaneous double-beam system is realized with only one optical path, which results in
clearly higher measurement stability compared to classical LS AAS. While the sensitivity of
this technique is comparable to that of LS AAS, it features clearly improved signal-to-noise
ratios and thus lower detection and determination limits. These are achieved by the use of
the CCD line detector of the contrAA 700 with extremely low noise compared to the
photomultipliers customary in LS AAS and to the use of the high-energy xenon short-arc
lamp with its very high light intensity.

5.2 Xenon lamp


The continuum source used on the contrAA 700 is a xenon short-arc lamp.
Due to the special electrode geometry of the xenon short-arc lamp, a hot arc spot ("hot spot”)
is formed that emits a very high radiation density throughout the entire spectral range (185 –
900 nm).
During the analysis, the position of the arc spot is monitored and automatically readjusted.
This way, warm-up effects by lamp drift are avoided. All drifts of the xenon lamp are
simultaneously corrected for in the spectra through correction pixels.

Fig. 6 Xenon lamp without housing

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Functions and design of the contrAA 700

5.3 Graphite tube atomizer


The electrothermic atomizer (EA) is an integral part of the contrAA 700. It is also a core part
for working in EA mode and HydrEA technique.

1 Furnace jaws 7 Cooling water connector


2 Furnace window 8 Vertical adjustment
3 Fuse at graphite tube furnace 9 Cooling water connections
4 Furnace camera illuminator 10 Heavy current cable
5 Radiation sensor 11 Gas connector, black tube
6 Gas connector, black tube 12 Furnace window

Fig. 7 View of graphite tube atomizer

The furnace system includes a graphite tube with lateral contact pieces located on the jacket
side for tube heating in transversal direction. This cross-heated graphite tube is an essential
function unit. It serves as atomizer for liquid sample volumes injected with the autosampler
AS-GF or an IC sample carrier containing a small amount of solid substance introduced with
the help of solid sample peripherals. At the same time, the cross-heated graphite tube also
serves as a heating resistance of the electric furnace.

Remarks relating to graphite tube furnace operation


 Constant temperature ratios along the entire tube length
 Realization of linear temperature-time runs according to a sensorless control model
on the basis of saved thermoelectrical parameters and an adaptive control
 Simple design and simple to manufacture, and therefore cost-effective geometries of
the transverse-heated graphite tube and the other graphite components.
 Protective gas flows, independent of each other and symmetrical to the furnace
center, which ensure effective graphite tube and furnace window cleaning, and
which also ensure fast and safe transport of the thermally disintegrated products of
the sample for disposal.
 Small consumption of protective gas, at the same time ensuring effective protection
against interference with atmospheric oxygen.

30 Issue 01/2014 contrAA 700


Functions and design of the contrAA 700

The analytical advantages of the graphite tube technique, in conjunction with the background
compensator, consist of the high selectivity and problem-free trace and ultra-trace analysis
of real samples with a complex matrix.
In the analysis, each sample runs through a furnace program (temperature-time program)
with the aim of drying wet samples and of separating out any distorting incidental substances
before atomizing.
The furnace program runs in four basic steps:
 Drying the sample
 Thermal treatment, separating or ashing distorting sample incidental substances
(matrix)
 Atomizing the sample
 Cleaning the graphite tube and preparing for the next measurement.
The operator optimizes these basic steps for each analysis problem with the control software
Aspect Cs.

5.3.1 Graphite tube furnace


The transverse-heated graphite tube, with its contact surfaces, is pneumatically pressed and
held against annular shaped graphite electrodes which are in water-cooled metal bodies.
Between the metal bodies, which carry the electrodes, there is an additional graphite
component: The furnace shroud. Together with the graphite electrodes, it forms a closed
inner chamber around the graphite tube which stabilizes the heat emission conditions of the
graphite tube and also guarantees chemically inert ratios. For pre-adjustment of the position
of the graphite tube when the atomizer is open, the furnace shroud has defined supports on
the inside. When closing the movable furnace component, the tube is raised to the resting
position and pressed into the contacts, without touching the furnace shroud. This action can
be reproduced.
1 Furnace window
2 Graphite tube, installed
3 Dosage opening with graphite funnel insert
4 Fixed furnace component
5 Furnace shroud
6 Furnace window
7 Movable furnace component, open
8 Graphite electrode in the movable furnace
component
9 Ceramic ring

Fig. 8 Graphite furnace structural view

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Functions and design of the contrAA 700

5.3.2 Gas flows in furnace shroud


The gas channels for separate supply of the primary gas flow (cleaning gas) and the
secondary gas flow (protection gas) are housed in the furnace shroud. Oxidizing or reducing
gases (O2 or H2) can be added to the primary gas flow if necessary. The have a positive
effect on the charring step. When using oxygen, temperatures >500 °C should be avoided
since the graphite tube itself will then be attacked.
The primary gas flow has the task of removing all gases which occur in the graphite tube
during the drying and charring step; of preventing condensation effects of the samples on the
furnace windows and of influencing the residence time of the analyte atoms in the path of the
beam. During atomization, the primary gas flow is generally interrupted in order to achieve
the longest possible residence time for the atom in the path of the and to increase the
sensitivity of the measurement. The secondary gas flow sweeps the graphite tube and also
reaches the outside through the funnel of the dosage opening.
The secondary gas flow is responsible for ensuring that the graphite tube is surrounded by
inert gas, even when the primary gas flow has stopped, and thus provides protection against
oxidation by atmospheric oxygen

1, 3 Primary Gas Flow (cleaning gas)


2 Secondary Gas Flow (protection gas)

Fig. 9 Primary and Secondary Gas flows in the Graphite Tube Furnace

The thermal flow in the furnace shroud is realized via a cylindrical attachment to the fixed
furnace component. The operating temperature of the atomizer is thus increased by desired
amounts so that, at its inner walls, condensation effects of the analyte (the sample) are
avoided.
The conical attachment on the opposite side of the furnace shroud, together with the sealing
ring in the rotatable furnace component, forms an exactly defined slit and thus guarantees a
safe sealing of the cell inner chamber from any penetrating surrounding air. If the tube in the
furnace shroud is broken, the sealing ring in the movable furnace component prevents a
short circuit between the furnace components.
The furnace shroud is bored in the direction of the optical axis, the outer cylinders support
the furnace window (quartz cell window). These can be pulled off easily for cleaning
purposes by a twisting.

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Functions and design of the contrAA 700

1, 4 Cylinder for the furnace window


2, 3 Mount: Conical attachment

Fig. 10 Graphite tube furnace shroud

When changing from the normal tube to the platform tube, or to solid analysis, please ensure
that the platform tube limits the free opening for the beam on one side. The graphite tube
furnace can be aligned to the HCL beam path by a delicate vertical movement of the mount.

5.3.3 Graphite tube variations, furnace parts and inserts


 Standard graphite tube
 Graphite tube for solid analysis
 Graphite tube with PIN platform

1 Graphite tube, standard 3 Graphite tube with PIN platform


2 Graphite tube for solid analysis

Fig. 11 Graphite tube variations

Graphite tube variation Sample volumes Use


Standard graphite tube max. 50 µL Aqueous samples (samples not requiring
complex analysis)
Alternative for solids (solid technology)
Graphite tube with PIN platform max. 50 µL Aqueous samples
Standard graphite tube for solids analysis Solids (solid technology)
(without dosing opening)

Table 6 Use and sample volume of different graphite tube variations

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Functions and design of the contrAA 700

Fig. 12 Furnace jacket, adapters and inserts

No. Furnace part / insert Function


1 Platform (sample carrier) Accommodates solids samples.
2 Adjusting aid for SSA 600 Adjusts the solid autosampler SSA 600.
3 Pipetter insert Funnel opening to the pipetting channel.
4 Solid adapter Seals the pipetter opening.
5 Adjusting aid Adjusts the autosampler AS-GF.
6 Electrode Contacts tube wings.
7 Furnace jacket Accommodates the graphite tube.

Table 1 Furnace parts and inserts

5.3.4 Radiation sensor


On the side of the graphite tube furnace, diagonal to the direction of the beam, is a
measuring layout for recalibration of tube temperatures. This radiation sensor uses a semi-
conducting receiver to pick up radiation from the inner chamber of the graphite tube. Using
two wavelengths for detection, an independent quotient signal is derived for temperature
measurement which is independent of the degree of radiation of the graphite tube.
Recalibration takes place when formatting the graphite tube.

5.3.5 Furnace camera


A furnace camera is turned on and off under software control. The user screen of ASpect CS
provides a separate window with a furnace camera image. The furnace camera monitors a
process sequence from the point of sample injection into the graphite tube to completion
point of drying. This makes it possible to directly supervise, and correct if necessary, motion
for submergence of the dosing tube into the graphite tube, for dispensing of a sample, as
well as other process components, including the drying process. Prior to pyrolysis, the
furnace camera is automatically turned off.
To illuminate the graphite tube, an illuminator unit is mounted in a lateral position (to be
turned on concurrently with the furnace camera.

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5.4 Accessories for graphite tube technique


5.4.1 Autosampler AS-GF
The autosampler AS-GF is used in EA mode for feeding liquid samples and in the HydrEA
method for feeding reaction gas into the graphite tube.

IMPORTANT
Manual pipetting is not recommended because of the poor reproducibility rate.

1 autosampler arm with canula restraint


2 tube guide
3 sample tray with sample tray cover
4 dosing unit (500 µL)
5 waste bottle
6 storage bottle for wash solution
(or diluent)

Fig. 13 Autosampler AS-GF

The autosampler AS-GF accepts defined volumes of different solutions and places them into
the graphite tube. It enables the
 Addition of up to five modifiers to the sample solution
 Transport of the sample solution to the thermal pretreatment in the tube
 Enrichment of samples
 Placement of components in the preheated tube
 Separate transport of components with intermediate washing
 Automatic preparation of standards by dilution or by different volumes
 Fixed, preselected or intelligent sample dilution
 Fully automatic multi-element mode (night mode possible)
The sample tray of the AGS-GF has space for 100 sample cuts (with V = 1.5 mL) and 8
central cups for diluent, special samples, standards, modifiers etc. (with V = 5 mL).

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The AS-GF is hung in the adapters provided in the sample chamber and electrically
connected to the contrAA 700. The device parameters of the AS-GF are set with the ASpect
CS control software.

5.4.2 Solid autosamplers SSA 600 and SSA 6z


The solid samplers SSA 600 and SSA 6z are absolute preconditions for the solids analysis in
the graphite tube technique. These enable reproducible placement of the IC sample carrier
mounted with the solid sample into the graphite tube.
The solid autosampler SSA 600 enables automatic transport of solid samples into the
graphite tube furnace. Weighing is performed fully automatically with an integrated
microbalance. The solid autosampler SSA 600 has 84 sample positions when using two
sample plates.
The SSA 6z is conceived for manual operation and requires an external balance. The
sample mass must be transferred manually to the sample table.
A full description of the solid autosamplers can be found in the operating instructions "Solid
Autosampler SSA 600" or "Solid Autosampler SSA 6z".

SSA 600 with liquid dispensing SSA 6z for manual sample supply

Fig. 14 Solid sampler

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5.5 Flame system


Flame atomic absorption spectroscopy is used for the determination of trace elements in the
concentration range from mg/L to µg/L and for the determination of principal components.
The technique requires a flame with constant properties. The composition of the flame must
be adjusted to the element to be analyzed. The device provides the motorized vertical
adjustment of the nebulizer-mixing chamber-burner system by 12 mm thus making it
possible to move the flame zone with the maximum absorption into the beam path. For the
measurement of principal components, the burner head can be swiveled by 90° on the
burner neck until it is at right angles to the beam thus shortening the absorption path of light
through the flame.
The sample solution is aspirated by a pneumatic concentric jet nebulizer and sprayed into
the mixing chamber. In the mixing chamber, the sample aerosol is mixed with acetylene and
auxiliary oxidant before it emerges from the burner slot. The flame is either 5 or 10 cm long
and a few millimeters wide depending on the burner type used. The beam transmits the full
length of the flame.

5.5.1 Automatic gas control system


The automatic gas control system ensures acetylene and oxidant supply to the flame at
defined flow rates and free from pressure fluctuations. It allows reliable and safe ignition and
quenching of the flame. The automatic gas control system has three gas inlets for acetylene,
air and nitrous oxide.
The fuel gas flow is adjusted in 5-L steps between 40 and 315 NL/h acetylene via a
proportional valve integrated in the control path. The air flow first fills the 600 cm³ gas tank,
before it is released to the nebulizer. In both normal and emergency cases, the flame is
quenched by an air flow coming from the tank. The oxidant flow through the nebulizer is
defined by its setting and the admission pressure. An additional flow of oxidizing agent (air or
nitrous oxide) can be turned on in three pre-set flow rates.
Initially, the air flow is enabled, the fuel gas flow is then turned on. A spiral-wound filament
comes out of the sample compartment’s back wall to swing over the burner center and ignite
the flame. One may switch from acetylene-air flame mode to acetylene-laughing-gas flame
mode by disabling air supply while releasing nitrous oxide supply and increasing the rate of
fuel gas supply. A burning acetylene-laughing-gas flame is extinguished in reverse order.

5.5.2 Burner-nebulizer system unit


The nebulizer produces the aerosol of the sample solution needed for the atomization in the
flame. The oxidant is supplied to the nebulizer through a lateral connector. It flows through
the concentric jet formed by the corrosion-proof platinum-rhodium tube and the plastic nozzle
made of PEEK. Sample solution is expelled from the tube and further sample solution
aspirated by the produced negative pressure. The position of the tube end relative to the
nozzle determines the aspiration rate and the aerosol output. It is manually adjustable by
means of an adjusting screw and lock nut.
The sample aerosol hits the impact bead, where larger droplets condense and then drain
away through the siphon. The fuel gas flow hits the impact bead at right angles. Once
generated, the aerosol flows through the mixing chamber to the burner. On passing through
the mixing chamber, it reaches equilibrium conditions. More great droplets are then
separated out as a result of gravitational force effects, equally draining away through the
siphon. Aerosol is atomized by the flame. The aerosol containing smaller droplets is
evaporated when entering the flame and then atomized in its hot zone. If the solvent

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evaporates incompletely, the accuracy of the analytical result is adversely affected, as


background absorption is increased by the scattering of radiation on unevaporated droplets.

1 Combustion gas supply 6 Siphon


2 Baffle ball 7 Outflow from siphon
3 Nebulizer 8 Float switch
4 Sample liquid supply 9 Impeller
5 Oxidant supply 10 Mixing chamber tube

Fig. 15 Setup of the burner-nebulizer system

The setup of the mixing chamber nebulizer system optimizes the aerosol formation and
ensures that the system is easy to maintain. The outlet into the siphon is located in the
immediate vicinity of the nebulizer. Large drops drain off immediately and do not enter the
mixing chamber. The impeller retains droplets and stabilizes the aerosol cloud. Potential
liquid residues can continuously rise in the mixing chamber tube towards the nebulizer and
drain off to the siphon. Furthermore, the baffle ball is permanently centered on the nebulizer
so that a readjustment after cleaning the mixing chamber nebulizer system is not required.

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1 Burner 9 Fixing screw for siphon


2 Fixing screw for burner 10 Siphon
3 Combustion gas supply 11 Connection of siphon sensor
4 Additional oxidant supply 12 Siphon outlet
5 Locking ring for nebulizer 13 Siphon sensor
6 Nebulizer 14 Screw joints of mixing chamber parts
7 Sample liquid supply 15 Safety plug
8 Oxidant supply 16 Mixing chamber tube

Fig. 16 Nebulizer mixing chamber burner system

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5.5.3 Burner and flame type


The contrAA 700 can be operated with the following types of flames and corresponding
burners:
 Acetylene/air flame with 50-mm single-slot burner (standard burner) or 100-mm
single-slot burner for more sensitivity
 Acetylene/nitrous oxide flame with 50-mm single-slot burner
If the range of elements to be analyzed includes both elements that are easy to atomize and
those hard to atomize, only the standard 50-mm single-slot burner should be used to avoid
the need to change the burner between measurements.
Use of the different flame types:
 Acetylene/air flame can be used for most of the elements.
 Acetylene/nitrous oxide flame is requited for elements that are hard to atomize, such
as boron, aluminum and silicon.
1 50-mm single-slot burner (standard)
2 100-mm single-slot burner

Fig. 17 Burner types

The burners are made of titanium and thus inert against aggressive sample solutions. The
burners can be easily exchanged and continuously rotated up to 90° between two stops.
One of the stops is adjusted in such a way that the burners are in alignment with the optical
axis. The 90° stop ensures the insensitive position of the burner at right angles used for the
determination of the principal components.

5.5.4 Sensors
The burner-nebulizer system is monitored by various sensors that ensure operational safety.
 A float switch in the siphon signals the correct fill level of 80 mm water column.
 Two reflective couplers identify the burner type by means of a code.
 A UV-sensitive sensor is used to monitor the flame.
In addition to the above mentioned sensors, the mixing chamber is equipped with a pressure
relief valve. This valve opens should the flame flash back into the mixing chamber.
The control software evaluates the sensor signals and additionally monitors gas pressures,
gas flow rates and the status of the flame.

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5.6 Accessories for flame technique


5.6.1 AS-F and AS-FD autosamplers
Manual or automatic sample supply may be employed in the flame technique and the
mercury/hydride technique. Automatic operation and multi-element analysis are possible if
an autosampler is used. The parameters are set and the function is controlled with the
contrAA 700 control software.
The contrAA 700 P can be operated with the following autosamplers:
 The autosampler AS-F is an automatic autosampler.
 The autosampler AS-FD also has a dilution function.
The autosamplers use sample trays with the same diameter. The following sample tray types
are available:

139 positions Sample tray with 129 sample positions for 15 mL Sarstedt cups on the
outer track and 10 sample positions for 50 mL Sarstedt cups on the inner
track
54 positions Sample tray with 54 positions for 50 mL Sarstedt cups

The sample trays should be selected according to the requirements of the sample analysis:
 Available sample volume
 Type of signal evaluation
The software controlled autosampler arm reaches all the positions intended for sample-
taking. The dipping depth into the sample and the special cups is preset, however, it can be
adjusted via the control software.
The contrAA 700 supplies the autosamplers with operational voltage. Tray and autosampler
arm are driven by stepping motors. The tray is rotated. The autosampler arm is rotatable and
can be lowered by 120 mm.
On the top of the autosampler AS-F there is a wash cup with overflow next to the sample
tray. In the autosampler AS-FD the wash cup is located in a plastic block together with a
mixing cup. A diaphragm pump delivers the washing liquid from the supply bottle into the
wash cup – this action cleans the dipped canula by washing it inside and out. Excess
washing liquid flows through the overflow into the waste receptacle, which is under the table
during the wash cycle.
The autosampler AS-FD features an extra Fluidik module with a dosing unit (5000 µL). The
Fluidik module is electrically connected to the autosampler and is supplied with operating
voltage via the contrAA 700. Standards or samples are diluted in the mixing cup by first
placing the concentrate into the mixing cup. Then the diluent is added at a high dosing speed
(max. volume: V = 25 mL). A fixed waiting time ensures complete mixing. A second
diaphragm pump extracts the residual liquid that has not been taken up by the nebulizer.
The autosampler AS-FD with dilution function features the following advantages:
 Preparation of standards for the calibration by diluting one or several stock
standards in the mixing cup
 Dilution of the sample if its concentration is too high, i.e., its element content is
higher than 110 % of the calibration standard with the highest concentration
 Dilution of all samples at freely selectable dilution ratios up to a ratio of 1:500

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1 Sample tray with cover 4 Storage bottle for diluent


2 Autosampler arm 5 Fluidik module
3 dosing unit (5000 µL) 6 Storage bottle for washing liquid

Fig. 18 Autosampler AS-FD with separate Fluidik module

5.6.2 JUN-AIR 6/S piston compressor


If no in-house compressed-air supply is available, it is useful to use a compressor that
produces the air required for the acetylene/air flame.
The JUN-AIR 6/S Piston Compressor is available as option. The produced compressed air is
free from water, dust and oil. With a maximum operating pressure of 800 kPa and a 15-L air
tank, the compressor meets the demands on compressed air supply. For its operation,
observe the instructions given in the operating manual of the JUN-AIR 6/S Piston
Compressor.

5.6.3 SFS 6 injection module


SFS 6 Injection Module (Segmented Flow Star) is available as optional accessory. It may be
used in combination with an autosampler or in manual mode.
On the one hand, it allows washing or carrier solution to be aspirated continuously thus
keeping the burner at a constant temperature by the aerosol; on the other hand, it allows
small sample volumes to be measured reproducibly against a carrier solution (e.g. n-
butanol).
The operating principle of the SFS 6 Injection Module is based on a magnet with two inlets
and one outlet to the nebulizer. The sample aspiration tube is located at the energized inlet.
It is immersed directly into the sample or connected to the aspiration capillary of the
autosampler. The non-energized inlet is connected to the aspiration tube for the washing or
carrier solution. These are the two switching states:
 Basic state: Sample path is blocked, while the carrier solution path is free
 Active state: Sample path is free, the carrier solution path is blocked
The parameters for controlling the SFS 6 Injection Module are entered via the control
software.

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1 Control cable port


2 Tube to washing solution
3 Support
4 Short piece of tube to nebulizer capillary
5 Sample tube

Fig. 19 SFS6 injection module

5.6.4 Scraper – Automatic burner head cleaner for nitrous oxide


flame
The Scraper, an intelligent burner head cleaner, is recommended for the continuous and fully
automated operation with the nitrous oxide flame. When working with the nitrous-oxide flame
and particularly the fuel-rich C2H2/N2O flame, as is used for the analysis of such elements as
Si, W, Mo and Sn, carbon will deposit on the burner slot over longer periods. If these
deposits are not removed completely, this will lead to clogging of the burner slot, which in
turn will result in irreproducible measurement results.
Using the scraper, the cleaning procedure will be fully automated. Once activated in software
and stored as method parameter, the scraper guarantees a continuous and reproducible
measuring process without any disturbances and interruptions. You can choose among
various cleaning intervals depending on flame composition and need. On the other hand, the
scraper can also be used for the automation of the burn-in process of the nitrous-oxide
flame. If activated in the flame monitor, a cleaning step is carried out every 30 s. This way,
undisturbed burning in of the nitrous oxide flame is possible.
1 Power cable for scraper
2 Knurled thumb screw
3 Scraper
4 Fixing screw for burner
5 Knurled thumb screw
6 50mm burner head

Fig. 20 Scraper mounted to 50-mm burner head

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The scraper is attached to the burner head with the help of two knurled thumb screws. It can
be removed if not required.
The scraper can be retrofitted to a 50mm burner.

5.6.5 HPT burner head


The HPT burner head, which consists of a 50 mm burner, hinged holder and slit quartz tube,
is available as an option for the air-acetylene flame. The HPT burner head is used to
increase the residence time of the atoms in the flame, which helps to achieve higher
sensitivity particularly for lightly volatile elements such as Cd, Pb, Zn and Hg.
The quartz glass has a slit with a length of 50 mm on opposite sides to allow the flame to
pass through. The holder ensures that the slits are aligned to the burner head.
The HPT burner head is recommended for use up to an acetylene-air ratio of 0.16 to prevent
the deposit of soot on the quartz tube.
1, 4 Tension spring
2 Slit quartz glass
3 50 mm burner
5 Handle
6 Hinged holder

Fig. 21 HPT burner head

5.7 Supplementary accessories to Hg/hydride


systems
The range of available Hg/hydride systems covers anything from a simple batch system for
users with small sample rates to fully automated continuous system.
HS 50: basic batch system with pneumatic principle of operation.
The quartz cell is heated by the acetylene/air flame.
HS 55 modular: batch system with electrically heated cell unit with or without "Hg Plus"
module for Hg detection.
The reduction agent solution is metered by a 1-channel hose pump.
HS 60 modular: Hg/hydride system for flow injection operation with electrically heated cell
unit with or without "Hg plus" module for Hg detection.
For a description of Hg/hydride systems, you should refer to the relevant accessory unit
manuals.

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6 Installation and start-up


CAUTION
No unauthorized tampering!
The device may only be set up, installed and repaired by service technicians
employed with or authorized by Analytik Jena AG.
Any unauthorized tampering will limit the right to claim under warranty. For the installation
and start-up of the device, the instructions given in Section "Safety instructions" p. 9 must be
observed. Compliance with these safety instructions is a requirement for the trouble-free
installation and functioning of your AAS measurement environment. Always observe all
warning and information labels affixed to the device or displayed by the contrAA 700 control
software.
To ensure trouble-free operation of the contrAA 700 take care to always keep the ambient
conditions specified in Section "Installation requirements" p. 20. If you intend to relocate the
contrAA 700, proceed as described in Section "Transportation of the contrAA 700" p. 100.

6.1 Utility supply and control terminals


Supply cabling and tubing is connected by Customer Service personnel of Analytik Jena AG
as part of the contrAA 700 installation work package.
The main power switch is located on the right-hand side of the contrAA 700. Also located on
the right-hand side are the terminals for PC and accessory units in easily accessible
positions. Utility supply inlet ports for 0gas and current are provided on the back.
For transportation and installation work, a pair of carrying handles must be screwed in on the
right-hand and the left-hand side. On completion of installation work, these handles must be
unscrewed and the openings sealed with plugs.
1 Utility supply terminals for gas, electric
power and fuses
2 Connector strip
3 Carrying handle
4 Main power switch
5 Carrying handle

Fig. 22 Main power switch and connector strip terminals for utility supplies and controls
on the right-hand side of the contrAA 700

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1 Port for furnace camera PC


2 Unassigned USB port
3 Port contrAA 700 – PC
4 Unassigned I/0 port for triggering
5 Port contrAA 700 – PC (for service only)
6 Fuses for xenon lamp F7/F8 T 3,15 A
7 Port for AS-FD, AS-F autosampler
8 AS-GF port
9 Port for SSA 600 solid autosampler
10 Port for hydride systems
11 Unassigned port

Fig. 23 Connector strip with supply and control connector terminals

1 Fuel gas port (C2H2)


2 Nitrous oxide port (N2O)
3 Air inlet
4 Fuses F5, F6
5 Linie power outlet for accessory units
(5X distributor strip)
6 Fuses F3, F4
7 Fuses F1, F2 (only may changed by
service technicians authorized by
Analytik Jena AG)
8 Power supply cord for contrAA 700
9 Extra gas supply port for graphite
furnace (standard: argon)
10 Inert gas supply port for graphite
furnace (argon)

Fig. 24 Rear panel view of contrAA 700 with ports and terminals for gas and electric
power supply, including fuse holders

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6.2 Installing and connecting the contrAA 700


CAUTION! INSTALLATION ONLY BY CUSTOMER SERVICE!
nitial installation by authorized Customer Service personnel of Analytik Jena only!

CAUTION!
Ensure that new operating site complies with installation requirements!
Refer to chapter "Installation requirements" p. 20.
Follow safety instructions in chapter "Safety instructions" p.9.
Take care that applicable rules of industrial and occupational safety are observed.
References to potential danger cannot be regarded as replacement of valid laws of industrial
labour safety!

Aids and auxiliary tooling


 4 plastic sealing plugs
 17 mm W/F open-end wrench (included in delivery)
 19 mm W/F open-end wrench (included in delivery)

Working steps
1. Unscrew four carrying handles and store them away.
2. Cap the mounting holes with sealing plugs.
3. Install gas supply tubing:
Tighten acetylene gas connector with 19 mm W/F open-end wrench. Left-hand
threading!
− Slide argon tube onto tube clip.
− Tighten air supply connector with 17 mm W/F open-end wrench.
− Tighten acetylene gas connector with 19 mm W/F open-end wrench. Left-hand
threading!
− Tighten nitrous oxide connector with 19 mm W/F open-end wrench.
4. Inspect gas connection points for absence of leakage (refer to section "Utility supply
and control terminals" p. 45).
5. Check cooling water level and refill if necessary (refer to section "Check cooling water
level" p. 76).
6. Provide electrical connections for contrAA 700 operation (refer to section "Energy
supply" p. 22).
7. Use USB cable for connection between PC and contrAA 700 (3 in Fig. 22 p. 45).
8. Further required working steps:
− Install ASpect CS software.
− Complete contrAA 700 configuration as required for selected atomization
technique.

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6.3 Installation and start of ASpect CS software


Installation and start of the ASpect CS software required for the control of the spectrometer
are described in the ASpect CS user manual.

6.4 Graphite tube technique


6.4.1 Terminals in sample compartment for graphite technique
1 AS-GF suspension bracket at left sample compartment
wall
2 Graphite tube furnace with terminals
3 AS-GF suspension bracket at right sample compartment
wall
4 Fixing screw for protective cover
5 In-depth adjustable mechanical stop for AS-GF
6 Fixing screw for protective cover

Fig. 25 Elements in sample compartment for graphite tube technique

The graphite tube furnace comes factory-adjusted. Its supply facilities for gas and cooling
water are firmly attached to the graphite tube furnace.
A cooling water tank is located behind the protective cover below the furnace space.

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1 Furnace jaws with electrodes 7 Cooling water terminals


2 Furnace window 8 Vertical adjustment
3 Fuse at graphite furnace 9 Cooling water terminals
4 Illuminator for furnace camera 10 Heavy current cable
5 Radiation sensor 11 Gas inlet, black tube
6 Gas inlet, black tube 12 Furnace window

Fig. 26 Terminals at graphite tube furnace

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Installation and start-up

6.4.2 Software presettings for graphite tube technique


The preview screen of ASpect CS software provides options for desired graphite tube
technique settings. The software user screen with methodological and operating parameters
needs to be adapted accordingly.

Fig. 27 Preview screen of ASpect CS with graphite-tube related setting options

Selectable options are:

Group Option Description


TECHNIQUE GRAPHITE Uses graphite tube furnace for atomizing technique
FURNACE

HYDREA Uses hydride systems HS 55 or HS 60 modular in


combination with graphite tube furnace
SAMPLE LIQUID Analyzes liquid samples (uses AS-GF as autosampler).
STATE

SOLID Analyzes solid samples (uses SSA 600 or SSA 6z).


TUBE TYPE Only with liquid samples.
W ALL Uses IC graphite tube.
PLATFORM Uses IC graphite tube with 1-PIN platform.

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6.4.3 Inserting the graphite tube into the graphite tube furnace
Installing and removing a graphite tube is necessary after changing the atomization method
and also after a certain number atomizations have been executed with the same graphite
tube.

CAUTION
Never touch the graphite tube with bare fingers! Fingerprints burn into the surface, and this
causes premature damage to the pyrolysis coating of the tube.

Inserting the graphite tube into the graphite tube furnace

1. Click Furnace dialog screen in ASpect CS. Change to Control tab.

Fig. 28 FURNACE / CONTROL window

2. Open graphite tube furnace by clicking the [OPEN FURNACE] control button.
3. Clean furnace shroud and electrodes if necessary (→ section "Cleaning the graphite
surfaces" p. 79).
4. Use tweezers or wood pulp to manually insert the graphite tube into the graphite tube
furnace space in such a position that the tube is freely supported of the furnace shroud
pads and the pipettor opening faces toward the top.
For working with a graphite tube for solid substance analysis with not pipettor opening,
any of its sides may be turned upward.
5. Close graphite tube furnace by clicking the [CLOSE FURNACE] control button.
6. Enter parameter settings for HEAT CYCLES and LIFE TIME in TUBE subarea as required for
the currently installed graphite tube.

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7. Format graphite tube. Actuate [FORMATION] control button (→ section "Graphite tube
formatting" p.52).
1 Furnace window
2 Graphite tube, installed
3 Dosage opening with graphite funnel insert
4 Fixed furnace component
5 Furnace shroud
6 Furnace window
7 Movable furnace component, open
8 Graphite electrode in the movable furnace
component
9 Ceramic ring

Fig. 29 Graphite tube furnace open with graphite tube installed

Removing the graphite tube from the granite tube furnace


CAUTION! DANGER OF SKIN BURNS!
Allow enough time for the graphite tube furnace to cool down before you remove the
graphite tube.

CAUTION!
Do not touch the graphite tube with bare fingers under any circumstances!
Fingerprint marks will burn in, thus causing early destruction of the tube’s pyrolysis coating.

1. Open graphite tube furnace by clicking onto button [OPEN FURNACE] in the FURNACE /
CONTROL screen (Fig. 26 p. 49).
2. Use plastic tweezers to extract the graphite tube, use wood pulp for manual removal.
3. Insert new graphite tube (see above) and/or close graphite tube furnace.

6.4.4 Graphite tube formatting


Graphite tube formatting is performed to:
 force air oxygen out of the furnace and adapt the contact pressure force of the
movable furnace part,
 recalibrate the tube temperature,
 format a newly inserted graphite tube,
 clean the furnace after a break in operation.
The furnace must be formatted:
 after turning the spectrometer on
 after closing the previously open furnace

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A running formatting program includes nine pre-programmed temperature stages.


A formatting sequence can be triggered in the FURNACE / CONTROL window. While formatting
is in process, the FORMAT FURNACE window will display the current values for temperature
stage, time and heating rate. During the first five stages, the furnace and the graphite tube
will be cleaned and conditioned (contact points between graphite tube and electrodes are
adapted accordingly). Specific sensor technology is then used to measure the tube
temperature in the remaining four stages. On completion of the last temperature stage, the
formatting factor for tube temperature correction will be output. Once corrected, the furnace
temperature will ensure proper measuring results.
If the formatting factor is found to be ≥ +10%, there will be no automatic temperature
correction, yet the current temperature-versus-time program can be launched after a
respective screen message was acknowledged.

1. In ASpect CS use to switch to the FURNACE / CONTROL window.


2. Enter specific data on the current graphite tube:
New graphite tube HEAT CYCLES 0
LIFETIME 0
Used graphite tube HEAT CYCLES Current value of the graphite tube
LIFETIME Current value of the graphite tube

3. In the TUBE area click the [FORMATION] button.

6.4.5 Cleaning the graphite tube / cleanout

1. In ASpect CS use to open the FURNACE / CONTROL window.


2. In the CLEAN FURNACE area set the following parameters:
TEMP. [°C] Final temperature to be reached during clean out.
The final temperature should be approx. 50 °C higher than the
previous atomization temperature.
RAMP [°C/S] Heating rate
HOLD [S] Set the hold time

3. Start the cleanout with the [START] button in the furnace area. Cleaning may be
repeated several times, if required at a higher temperature.

Clean out/evaporation of iridium-coated graphite tube (HydrEA


technique)
The following temperature program must be used for the iridium-coated graphite tube (see
also operating instructions for the accessories):

Clean-out Evaporation
TEMP. [°C] 2200° C 2600°C or more
RAMP [°C/S] 500° C/s 500° C/s
HOLD [S] 10 s Do not select a higher hold time than 10 s
otherwise this may exceed the load limit of the
furnace.

Clean out or evaporation can be repeated several times.

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6.5 Completing and installing the AS-GF auto-


sampler
6.5.1 Installing AS-GF

VORSICHT! ELECTRONICS MAY BE DAMAGED!


Turn the contrAA 700 off before beginning work for installation of the AS-GF!
Action for making or breaking an electrical plug-in contact may cause a short with destroying
effect.

1 Left support in the sample chamber 7 Right support in the sample chamber
2 Adjusting screw 1 (for Y coordinate) 8 Wash cup
3 Adjusting screw 2 (for X coordinate) 9 Sample tray with cover
4 Tube holder 10 T valve of the dosing unit
5 Tube guide with clamp nut 11 Dosing syringe
6 Adjusting screw 3 (for X coordinate) 12 Lock screw for piston rod

Fig. 30 Installing the AS-GF

NOTE
Select a safe location to perform completion of the AS-GF. The device can tilt easily.

1. Turn the contrAA 700 off before you proceed to work for AS-GF installation!
2. Install the tube guide (5 in Fig. 30) to the autosampler arm of the AS-GF and attach
using the lock screw.
3. Screw the dosing tube into the right opening of the T valve (10 in Fig. 30) on the dosing
unit. Feed the dosing tube through the tube holder on the back of the autosampler and

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on the autosampler arm. Insert the dosing tube into the tube guide (5 in Fig. 30) until the
tube end protrudes approx. 8 mm from the tube guide at the bottom; attach the tube
using a clamp nut.
4. Plug the control cable into the socket at the back of the AS-GF and lock it in place.
5. Hang the AS-GF on the supports in the sample chamber (1 and 7 in Fig. 30). Using a
spirit level, check whether the autosampler is suspended horizontally; if necessary, align
the autosampler using the depth-adjustable stop in the sample chamber (5 in Fig. 25 p.
48).
6. If necessary, align the AS-GF with the furnace (coarse adjustment):
manually rotate the autosampler arm over the dosing opening in the graphite tube. If the
dosing tube does not align with the opening, the suspension of the autosampler must be
moved forward or back. To this end unhook the autosampler from the sample chamber.
Move the left and right suspension mounts with the aid of adjusting screw 1 and the set
screw (2 and 4 in Fig. 31). Hook the autosampler back in.

1 Slider with left suspension mount 3 Slider with right suspension mount
2 Adjusting screw 1 4 Adjusting screw

Fig. 31 Aligning the AS-GF with the furnace using the set screw and adjusting screw 1

7. Plug the control cable into the socket on the connection strip of the AAS device on the
right side (autosampler graphite connection, 8 in Fig. 23 p. 46).
8. Place and fix the sample tray on the axis of the AS-GF.
9. Place the sample cover until it sits in the guide rail.
10. Switch on the computer and the contrAA 700, wait for the initialization steps to
complete, start the Aspect CS software.
11. If necessary, fit the dosing syringe to the dosing unit (→ Section "Replacing the
metering syringe" p. 95).
12. Perform a fine adjustment of the autosampler (→ Section "Adjusting the AS-GF“ p. 56).

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Preparing the autosampler for the HydrEA technique


Prior to installing the HydrEA technique the graphite tube must be coated with iridium or gold
(see hydride system manual). Use the dosing tube used during graphite operation for this
purpose.
1. Switch off the AAS device and install the hydride system (e.g. HS 60 modular).
2. For the HydrEA technique remove the tube guide and dosing tube from the autosampler
arm of the AS-GF. Install the titan canula to the autosampler arm and attach it using the
lock screw.
3. Attach the reaction gas tube to the titan canula.

6.5.2 Adjusting the AS-GF


The AS-GF has already been installed in the sample chamber in accordance with section
"Installing AS-GF" p. 54. The fine alignment of the AS-GF to the furnace is supported by
software. The autosampler is aligned such that samples can be optimally deposited in the
graphite tube.

1 Adjusting screw 1 5 Adjusting aid with crosshair


2 Lock nut of alignment screw 1 6 Adjusting screw 3
3 Adjusting screw 2 7 Lock nut of alignment screw 3
4 Clamp nut

Fig. 32 AS-GF adjustment

1. Start the ASpect CS software and open the AUTOSAMPLER window with the symbol
, change to the tab TECHN. PARAMETERS.
2. Start the adjustment using the [ALIGN MPE TO FURNACE] button.
3. Follow the prompts in the dialog fields of the software.
In the running program the following takes place:
− Alignment of the AS-GF with the furnace

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− Adjustment of the dipping depth


Carry out the following work steps successively:
− Withdraw the dosing tube approx. 8 mm from the canula of the autosampler and fix
it with a clamp nut.
− Replace the pipetter insert in the graphite tube furnace by the adjusting aid with
crosshair.
− Lower the autosampler via the software to the adjusting aid.
− Align the X direction with the buttons [LEFT]/[RIGHT] to the crosshair.
− Adjust the Y direction using the adjusting screw 1.
− If required, readjust the X direction using the adjusting screws 2 and 3.
− Adjust the Z direction software-controlled:
Lower the autosampler arm up to the upper edge of the adjusting aid until the
dosing tube just dips into the dosing opening.
Adjustments for X and Z direction are saved in the software.
− Secure the positions of the adjusting screws with lock nuts.
− Remove the adjusting aid and insert the dosing funnel.
Adjust the injection depth in the graphite tube:
– Lower the autosampler arm via the software. The dosing tube dips into the graphite
tube.
– Loosen the clamp nut, place the dosing tube onto the tube bottom, check position
with furnace camera if necessary, and fasten with clamp nut.
– Move the autosampler arm software-controlled to the optimum dispensing depth
(approx. - 0.8 mm for 20 µL sample volume).

IMPORTANT
For further configurations of the autosampler see the instruction manual "Aspect CS" /
section "Technical autosampler parameters".

Populating the sample tray of the AS-GF


4. Populate the positions of the AS-GF as follows:
Positions 1-100 1.5 mL sample cups
Positions 101 – 108 5 mL special cups
5. Place the sample cover with a tight fit.
6. Next step: fill the wash bottle. If necessary, empty the waste bottle and dispose of the
waste correctly. Measure.

IMPORTANT
The population of the sample tray must match the software configuration in the method or in
the sample ID.

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6.5.3 Uninstalling the autosampler AS-GF


7. Switch off the contrAA 700!
8. For HydrEA coupling:
Remove the reaction gas tube from the titan canula. Remove the titan canula from the
autosampler arm, by loosening the clamp nut.
9. Remove the control cable from the socket in the right side wall of the AAS device
(autosampler graphite connection).

10. Release adjusting screw 1 and unhook the autosampler AS-GF.

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6.6 Flame technique


6.6.1 Flame technique terminals in sample compartment

1 Automatic ignition unit 9 Sample liquid supply


2 Burner 10 Siphon drain tube
3 Markings for alignment on the mixing chamber 11 Connection for oxidant (tube with two blue
tube and the holding fixture markings)
4 Stud bolt for fastening the burner 12 Suspension AS-F / AS-FD, left
5 Suspension for SFS 6 13 Connection for additional oxidant (tube with a
blue marking)
6 Suspension AS-F / AS-FD, right
14 Connection for fuel gas (tube with red marking)
7 Connecting sockets for siphon sensor, injection
switch SFS 6 and scraper 15 Fixing screw for holder bracket of burner-
nebulizer system unit
8 Vertical adjustment of burner-nebulizer system
unit

Fig. 33 Terminals at the burner-nebulizer system unit available for flame technique

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1 Mounting holes for autosampler 4 Terminal for siphon monitoring


2 Suspension point for autosampler 5 Terminal for SFS 6 injection switch
3 Scraper terminal

Fig. 34 Terminal facilities provided in sample compartment walls

6.6.2 Software presettings for flame technique


Use the preview screen of ASpect CS software (Fig. 27 p. 50) to select Flame option in
Technique group. The software user screen with methodology and operating parameters
will be adapted accordingly.

6.6.3 Installation for manual sample feeding


Manual sample feeding means that a sample is directly delivered to the burner-nebulizer
system unit.
The SFS6 injection switch can be optionally used.

WARNING! ELECTRONICS MAY BE DAMAGED!


Turn the contrAA 700 off before beginning work for installation!
Action for making or breaking an electrical plug-in contact may cause a short with destroying
effect.

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1 Burner 6 Sample container


2 Holder bracket at vertical adjustment mechanism 7 Sample tablet Collector trough
3 Mixing-chamber-nebulizer system unit 8 Siphon drain tube
4 Supply cable of siphon sensor 9 Gas terminals
5 Sample aspiration tube

Fig. 35 Flame technique, manual sample delivery

1. Remove the red protective cap from the mixing chamber tube.
2. Attach the mixing chamber nebulizer system without burner to the holding fixture for the
height adjustment.
The marking on the mixing chamber tube must be positioned above the edge of the
holding fixture (12 in Fig. 33 p. 59).
3. Put the collection under the burner-nebulizer system.
4. Hang the sample tray in the guides under the device.
5. Lead the outlet tube from the connector of the siphon through the opening in the tray
and attach it on the connector or the corresponding opening in the lid of the receiving
bottle.
Note: Position the outlet tube at a constant incline. If necessary shorten the tube. Tube
must not dip in the liquid.
6. Fill the siphon with water via the mixing chamber tube until water flows out via the outlet
tube.
7. Connecting the gas supply:
− Connect fuel gas (tube with red marking) (14 in Fig. 33 p. 59)
− Connect oxidant (tube with 2 blue markings) (11 in Fig. 33 p. 59)
− Connect additional oxidant (tube with 1 blue marking) (13 in Fig. 33 p. 59)

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8. Attach the required burner (50 mm or 100 mm depending on the measurement task) on
the mixing chamber tube, turn to the stop position and clamp. Ensure that the burner is
positioned correctly.
9. Injection module SFS 6
If you are working with injection module SFS 6, install injection module SFS 6
(→Section "Installation of SFS 6 injection module" p. 66).
10. Place the sample and wash cups on the tray.
11. Attach the aspiration tube to the nebulizer canula.
12. Hang the safety glass in and slide it in front of the burner.
13. Switch on the contrAA 700 and start the software.

Deinstallation for manual sample feeding


1. Turn the contrAA 700 off.
2. If operation included the SFS 6 injection module, the SFS 6 injection module must be
shut down (→section "Installation of SFS 6 injection module" on page 66).
3. Remove sample and wash cups from the tray.

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6.6.4 Installation for continuous operation mode / with samples


delivered by autosampler
In continuous operation mode, sample feeding is accomplished by an AS-F or an AS-FD
autosampler.

1 Storage bottle for diluent 6 Tube from autosampler arm to the SFS 6
2 Fluidik module with dosing unit 7 Injection module SFS 6 (where applicable)
3 Storage bottle for washing liquid 8 Tube for diluent (thick canula) and sample intake
tube (thin canula)
4 Tube for washing liquid to the SFS 6
9 Sample intake tube
5 Encased tubes for washing liquid and
diluent

Fig. 36 Flame mode, continuous with autosamplers AS-FD and SFS 6

CAUTION! RISK OF DAMAGE TO THE ELECTRONICS!


Switch off the contrAA 700 P prior to any installation!
Connecting or disconnecting electrical contacts might damage the sensitive electronics of
the contrAA 700.

Installing the burner/nebulizer system


1. Switch off the contrAA 700.
2. Remove the red protective cap from the mixing chamber tube.
3. Attach the mixing chamber nebulizer system without burner to the holding fixture for the
height adjustment.
The mixing chamber must be aligned to the height adjustment, the marking on the
connector must be above the edge of the holding fixture (3 in Fig. 33 p. 59).
4. Slide the collection tray under the burner/nebulizer system in the sample chamber.

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5. Plug the outlet tube from the connector of the siphon to the connector or the
corresponding opening in the lid of the collection bottle.
Note: Position the outlet tube at a constant incline. If necessary shorten the tube. Tube
must not dip in the liquid.
6. Fill the siphon with water via the mixing chamber tube until water flows out via the outlet
tube.
7. Plug the connector of the siphon sensor to the connection on the right sample chamber
wall (4 in Fig. 34 p. 59).
8. Connecting the gas supply:
− Connect fuel gas (tube with red marking) (14 in Fig. 33 p. 59)
− Connect oxidant (tube with 2 blue markings) (11 in Fig. 33 p. 59)
− Connect additional oxidant (tube with 1 blue marking) (13 in Fig. 33 p. 59)
9. Attach the required burner (50 mm or 100 mm depending on the measurement task) on
the connector, turn to the stop position and clamp. Ensure that the burner is positioned
correctly.

Installing the injection module


If you are working with injection module SFS 6, install injection module SFS 6 (→Section
"Injection module SFS 6" p. 66)

Installing the autosampler


1. Hang the autosampler in the corresponding supports of the sample chamber (Fig. 33 p.
59). Adjust the adjusting screw at the right suspension mount in such a way that the
autosampler cannot slip out of the mounting hole (3 in Fig. 37 p. 65).
2. Place the Fluidik module (for AS-FD) or storage bottle for washing liquid (for AS-F) next
to the AAS device.
3. Plug the control cables for connecting the autosampler to the Fluidik module and the
AAS device into the connections on the rear of the autosampler and lock them in place
(1 and 2 in Fig. 37 p. 65).
4. Plug the control cable into "Sampler flame" connection on the right-hand wall of the
contrAA 700 (7 in Fig. 23 p. 46) and lock it in place.
5. Attach the outlet tube to the outlet connector of the autosampler (backplate, 4 in Fig.
37). Attach the outlet tube to the connector or the corresponding opening in the lid of the
collection bottle.
Note: Position the outlet tube at a constant incline. If necessary shorten the tube. Tube
must not dip in the liquid.
6. Screw the tube for the washing liquid to the rear of the autosampler (5 in Fig. 37).
Note: In the AS-FD the tubes for connecting the autosampler and the Fluidik module
are attached to each other by encasing and are numbered. The tubes are attached to
the rear of the autosampler using the attachment lug. Marking Wash tube "2".
7. In the AS-FD feed the dosing tube for the diluent (marking "1") through the tube guide at
the autosampler arm and plug it onto the thicker canula of the autosampler arm.
Note: The autosampler arm can be moved manually when switched off.
8. Attach the sample intake tube to the nebulizer.
9. Plug the sample intake tube through the tube guide at the autosampler arm onto the thin
canula of the autosampler arm.
10. Place the sample tray onto the autosampler housing, make sure it latches.
Note: The controller does not start the autosampler or stops automatically if no sample
tray has been placed.

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11. Place the sample cover until it sits in the guide rail.
1 Fluidik module connection
2 AAS connection
3 Suspension mount with adjusting screw
4 Connector for outlet tube
5 Screw for wash tube

Fig. 37 Rear of the autosampler AS-FD

Preparing the Fluidik module (for AS-FD)


1 Storage bottle for washing liquid
2 Diluent connection
3 Dosing tube connection (to AS-FD)
4 Dosing syringe, consisting of piston
and glass cylinder
5 Dosing syringe with attachment screw
6 Storage bottle for diluent

Fig. 38 Dosing unit at the Fluidik module of the AS-FD

1. If necessary, fit the dosing syringe to the dosing unit (→ Section "Replacing the
metering syringe" p. 95).
2. Place the storage bottles for the wash liquid (left) and diluent (right) into the bottle
holders of the Fluidik module.
3. Immerse the short tube (marking at the tube "3") into the storage bottle for the diluent.
Screw the second tube end to the valve (2 in Fig. 38)
4. Screw the dosing tube for the diluent (encased, marking "1") to the second connection
of the valve (3 in Fig. 38).
5. Immerse the hose for the wash liquid (marking "2") into the storage bottle.

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6.6.5 Uninstalling the autosampler AS-F/AS-FD


1. Switch off the contrAA 700.
Uninstalling the autosampler
2. Detach the sample intake tube from the thin canula of the autosampler arm.
3. Detach the tube for the wash liquid at the rear of the autosampler.
4. For the AS-FD detach the dosing tube for the diluent from the thicker canula. Pull the
two encased tubes out of the attachment lug at the rear of the autosampler.
5. Pull the outlet tube from the connector of the autosampler (backplate).
6. Detach both control cables at the rear of the autosampler.
7. Take the autosampler out of the sample chamber.
Uninstalling the injection module
If the injection module SFS 6 was used during operation, decommission the injection module
SFS 6 (→Section "Shutting the SF 6 injection module down" p. 67).

6.6.6 Installation of SFS 6 injection module


Installing SFS 6 injection module

1 Tube connecting to sample/autosampler 3 Communication cable to controller


2 Tube connecting to nebulizer 4 Tube connecting to rinsing solution

Fig. 39 SFS 6 installed at the contrAA 700 for manual sample delivery

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1. Screw aspiration tubes into free ports of the injection module as follows:
− medium-long tube into upper port – to sample or autosampler
− short tube into sidewayse port – to nebulizer
− long tube into lower port – to rinsing solution
2. Manual operation mode: Hinge injection module into its designated suspension points at
the front of the vertical adjustment mechanism.
Working with an autosampler: Hang injection module into position at the right holder of
the autosampler.
3. In the default setting (not powered), the tube for carrier solution is now released for flow.
4. Plug control cable into the lower two-pole jack terminal at the right sample compartment
wall and screw it firmly on.
5. Mount short tube piece onto the nebulizer needle.
6. Dip tube for rinsing solution (long tube) into the storage bottle for rinsing solution.
7. Dip sample tube (tube of medium length) into the sample container and connect with the
aspiration needle of the autosampler.

Shutting the SF 6 injection module down


1. Remove the intake tubes out from the washing liquid bottle and the sample cup (for
manual operation), or pull them off the intake canula of the autosampler, allowing the
system to drain.
2. Pull off the short piece of tube from the nebulizer canula.
3. Detach the control cable of the SFS 6 from the AAS, remove the injection module.

6.6.7 Replacement of burner

CAUTION! DANGER OF SKIN BURNS!


Use burner fork (optional accessory item) to remove the burner when in hot state. Or wait
until burner has cooled down sufficiently.

1. Push sample compartment door up.


2. Release fixing screw of burner and take burner off. If burner fork is available, us burner
fork this purpose.
3. Place new burner onto the mixing-chamber tube, rotate it into 0° (mechanical stop)
position and lock it with the fixing screw.

6.6.8 Add-on installation of scraper


When working with the nitrous oxide flame it is recommended to use a scraper. Alternatively,
carbon deposits can be manually removed from the burner slot with the scraper. The scraper
is delivered ready installed on the 50 mm burner upon request. It can also be retrofitted to a
50 mm burner.

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CAUTION
For combustion gas flows > 250 NL/h pay attention to stubborn deposits. Remove these
where necessary to ensure the functionality of the scraper.
On special request the scraper comes factory-installed to the 50 mm burner. It can also be
retrofitted to a 50 mm burner.
1. Turn screws out of front-side burner jaw (arrows in Fig. 40).
2. Unscrew fixing rail (1 in Fig. 41) using knurled thumb screws (2 in Fig. 41) from the
scraper.
The knurled thumb screws are captive so they will be kept inside the holder device of
the scraper.
3. Mount fixing rail to burner head. Use long titanium screws and nuts (included in
delivery) for this purpose. Pass screws through front-side burner jaw and screw fixing
rail on with nuts.
4. Set scraper onto the guide pins of the fixing rail (2 in Fig. 41) and use knurled thumb
screws to fix the scraper (3 in Fig. 41).

Fig. 40 Screws in front-side burner jaw

1 Fixing rail for scraper 3 Knurled thumb screws


2 Guide pins

Fig. 41 Fixing rail with burner mounted / knurled thumb screws at scraper

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6.6.9 Operation of the HPT burner head

CAUTION!
The HPT burner head can only be used for the air-acetylene flame up to a fuel gas-air ratio
of 0.16.

1. Insert the quartz tube in the holder.


Make sure that the pin in the left V bearing is positioned in the existing groove on the
face side of the quartz tube. This ensures that the quartz tube slits are aligned to the
burner slit.
2. Set the HPT burner head on the connector of the mixing chamber and clamp.
3. Set a burner height of 12 mm or more for flame ignition and operation.
4. To ignite the flame, tilt the holder with quartz tube forwards. As soon as the flame has
ignited, already fold back the holder during the active ignition process.

Fig. 42 HPT burner head mounted on the mixing chamber

6.7 Starting the contrAA 700 with accessory units


up
6.7.1 Turn-on sequence, daily start of work
1. Turn power to the contrAA 700 on: Actuate green ON/OFF switch at the right lateral wall
panel for this purpose.
2. Turn PC on and wait for computer program to be completely initialized. The monitor will
display some application icons, among them the ASpect CS program icon.
3. Launch ASpect CS program session. Double-click with the mouse pointer onto the
ASpect CS icon to do this.
4. Once the ASpect CS software session has started, trigger initialization of accessory
units using software tools in MAIN SETTINGS window.
5. Turn printer and compressor on if required.

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 The AAS system is operational now and you may proceed to actual work (for
preparation of analytical jobs and measurement).

6.7.2 Turn off sequence

NOTE
Having turned the xenon lamp off, one should wait for another 30 seconds allowing the
lamp’s cooling loop to continue in operation before shutting the AAS system actually down.

1. At PC, ASpect CS application program: select FILE / CLOSE.


2. If settings have not been saved so far, define whether unsaved data/ unsaved
information is to be saved before the program will be terminated.
3. If xenon lamp is still on or was turned off after a time less than 30 seconds:
The screen will inquire if the xenon lamp is to be shut down. If the lamp is turned off, the
running ASpect CS session will be terminated after a delay time of 30 seconds.
4. Ramp PC down.
5. Transfer all main power switches into Off position (in this order):
− PC
− AAS
− Printer
− Compressor
 The AAS system is completely shut down.

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7 Care and maintenance


CAUTION! OBSERVE THE SAFETY INSTRUCTIONS!
The user must not perform any care and maintenance on the device and its components
other than those described in this Section.
Only service technicians employed with or authorized by Analytik Jena AG are allowed to
carry out repairs on the contrAA 700.
In maintenance work, observe all guidelines, standards and safety instructions specified in
Section "Safety instructions” p. 9.
To ensure perfect and safe functioning of the contrAA 700, it should be inspected on an
annual basis by service technicians from Analytik Jena AG.
Only use spares from Analytik Jena AG. Laboratory items used for routine operation can be
ordered from Analytik Jena AG.

WARNING! ELECTRIC SHOCK!


Turn power off and remove the line power plug from its socket before you proceed to
service work of any kind on the contrAA 700. Removal of the line power plug will safely
break line power supply to the contrAA 700. After turning off with the main power switch,
some parts of the spectrometer, including its outlet socket, will continue to carry line voltage.

7.1 Maintenance summary table


System component Action Reason / Periodicity
Basic unit
Fuse Fuse change As required
Sample compartment Cleaning of sublimed substances Regularly
Removal of residual liquids from the When residues are found
tray in the tray
Cleaning of beam entrance and exit On visual inspection
windows in the sample compartment When energy loss is
detected
Graphite tube furnace
Graphite tube Clean by performing a bake cycle via Daily
cleaning program of control software.
Iridium-coated Bleed iridium layer. After approximately 500
graphite tube atomization cycles or for
re-coating
(irregularities will falsify
measured results)
Furnace window Use non-shedding piece of cloth weekly
slightly moistened with alcohol for
wiping down.
Use a commercially available
detergent for UV-cells (e.g. HELLMA
NEX II) to clear away stubborn dirt.

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Graphite electrodes Clean contact faces of elec-trodes At regular intervals


with cotton wool wad, non-shedding
piece of cloth slightly moistened with
alco-hol or using blotting paper.
Check for wear, replace if necessary. Every six months
Pipetting insert Clean and rinse. May be required on a
daily basis, depending on
the type of samples
Autosamplers AS-GF / AS-F and AS-FD
Dosing tube/ Check for freedom from deposits, Regular inspection, since
needles kinks and cracks. sedimentation may falsify
measured results
Wash cup, mixing Clean At regular intervals
cup
Gas connection ports
Check for absence of leakage When tubing connections
were restored and on
noticing a distinct drop of
pressure at a manometer
Burner-nebulizer system unit
Disassemble and clean Depending on sample
material being analyzed
(medical samples or
samples with high salt
contents)
JUN-AIR 6/S piston compressor
Air tank Drain condensed water under Monthly
pressure
Pressure reducer Drain condensed water Monthly
Filter
Water separator Drain warter. Every three months
Recirculation cooling of Xe-lamp and graphite tube furnace
Compensation tank Check compensation tank for fill level. Monthly
Refill tap water as necessary.
Fans (in back wall) Keep dirt/contamination away At any time
Table 7 Maintenance summary table

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7.2 Basic system unit


7.2.1 Fuse change

WARNING!
Make sure to switch off the contrAA 700 before changing a fuse!

Protective fusing is located at the back of the contrAA 700, at the terminals bar and the
sample compartment of the graphite tube furnace. All fuses are provided with special
labelling.

Fuses at the back panel (see Fig. 24 p. 46)

Number of fuse Type Protected current circuit


F3 T 6,3 A/H Power socket
F4 T 6,3 A/H Power socket
F5 T 6,3 A/H Spectrometer
F6 T 6,3 A/H Spectrometer

Fuses at the terminal bar (see Fig. 23 p. 46)

Number of fuse Type Protected current circuit


F7 T 3,15 A Xenon lamp
F8 T 3,15 A Xenon lamp

Furnace fuse (see Fig. 7 p. 30)

Type Protected current circuit


TR5-T 100 mA Graphite tube furnace

Table 8 Fuses

WARNING!
The fuses of the line power inlet (F1 and F2) may only be changed by service technicians
employed with or authorized by Analytik Jena AG!

7.2.2 Reactivating the safety circuits of the cooling water circuit


The temperature of the cooling water circuit is monitored by means of two safety circuits.

Protection of the xenon lamp from overheating


The first safety circuit automatically deactivates the xenon lamp if the cooling water
temperature exceeds 60°C. When the cooling water temperature is below the limit value
again, the lamp is switched on when the contrAA 700 is reactivated and initialized.

Protection from uncontrolled furnace heating


A second safety circuit protects the AAS in the event of a possible communication error
between control (PC) and spectrometer from uncontrolled heating of the furnace. In the
event of a failure, this safety circuit switches off the power supply of the device hardware if
the cooling water temperature exceeds 65°C. Damage to the device that would be caused if

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the furnace is still heating can be avoided. If the second safety circuit has switched off the
power supply, the error message "Timeout autosampler" appears when the contrAA 700 with
graphite tube technique is reactivated.
The second safety circuit can be reactivated manually:
1. Open the right front door of the lamp chamber.
2. Operate the small red switch on the back of the lamp chamber (arrow in Fig. 43).
3. Switch the contrAA 700 back on and start the software ASpect CS.
If the lamp ignites and no error message appears, the device is ready.

Fig. 43 Safety circuit switch for hardware

7.2.3 Cleaning the sample compartments


 Clean the sample compartment regularly with a lintfree cloth moistened with alcohol.
 If there are liquid residues in the sample compartment tray, e.g. from the drain of the
siphon or the autosampler, pull the tray frontward, empty it and wipe it with a dry
cloth.
 When you notice detect energy losses, check the beam entrance and exit windows
for cleanness:
Clean the windows with a lintfree cloth (optics cloth) moistened with alcohol taking
care to leave no streaks.

IMPORTANT
After cleaning the sample chamber window with alcohol, it takes approx. 1 h until the
complete UV transmission has been restored.

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7.2.4 Removing and installing the xenon lamp

WARNING! ELECTRIC SHOCK!


Switch off the contrAA 700 at the mains switch. It is very important that you also remove the
mains plug from the 35 A connection before replacing fuses!

CAUTION! CONTAMINATION OF THE LAMP WINDOW!


Do not touch the lamp window when exchanging the lamp! Decontaminations have a
negative impact on the lamp properties!

1. Open the lamp chamber door (at the front on the left of the sample chamber of the
graphite tube furnace).
2. Place a cloth or similar under the couplings. Small amounts of water may occur when
disconnecting the couplings.
Disconnect the quick couplings for the cooling water at the bottom of the lamp housing.
To disconnect the couplings, press on the (metal) interlock until it clicks into place, then
pull out the coupling part to the bottom.
The coupling parts contain valves that close automatically when they are being
disconnected. This keeps cooling water from escaping. A few drops, however, will still
escape from the coupling parts.
3. Use the hexagon socket wrench (5 mm) with T-handle (part of the scope of delivery) to
unscrew the horizontal attachment screw of the lamp housing completely.
This pushes the lamp housing forward on the two guiding pins and the electric plug
connection (not visible) is removed.
4. Pull on the handle of the lamp housing with one hand and hold the housing at the
bottom with the other hand. Pull the housing to the front and off of the guiding pins.
Note: Keep a firm grip on the lamp housing when pulling it off the guiding pins. The
housing is heavy!
Do not touch the lamp window!
5. Put the removed lamp housing to the side.
6. Stick the new lamp housing on the guiding pins and push it toward the back.
Note:Do not touch the lamp window!
7. Screw in the attachment screw of the lamp housing completely using a hexagon socket
wrench and tighten the screw.
This presses the lamp housing to the back on the two guiding pins and into the electrical
multipole plug connection.
Note: It must be possible to screw in the lamp housing without noticeable resistance!
Do not use force!
8. Connect the cooling water hoses to the bottom of the lamp housing.
Press the plug connectors of the hoses into their counterparts at the lamp housing (left
hose - left inlet; right hose - right inlet) and push them in as far as they will go.
Note: There should be an audible click when the hoses are plugged in and the interlock
in the connection piece of the lamp housing should pop out.
9. Switch on the contrAA 700.
10. Make sure that circulation pump works and cooling water flows back to the stabilization
vessel.
Note: If the pump is running and no cooling water flows back, one (or both) plug
connector/s is not adjusted correctly. In this case disconnect the couplings again and
press them in properly.

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11. Check the filling level in the stabilization vessel of the circulating pump and fill with tap
water if required (→ Section "Check cooling water level" p. 76).
The fill level will decrease slightly after the lamp has been installed. This is due to the
heat sink of the lamp filling with cooling water. The displaced air is released via the
stabilization vessel after a few seconds.
Tighten the cover of the stabilization vessel by hand only.
12. Mop up any drops of water.
13. Close the lamp chamber door.

1 Fixing screw 1 Handle


2 Electric plug connector 2 Fixing screw
3 Guiding pin
4 Couplings for cooling water connection
6 Pump

Fig. 44 Xenon lamp housing Fig. 45 Xenon lamp, installed

7.2.5 Check cooling water level


Inspect for proper cooling water level on a monthly basis. The tank containing the liquid
volume for cooling the graphite tube furnace and the xenon lamp is located below the
graphite tube furnace.

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1 Sensor to monitor cooling water level


2 Cover
3 Cooling water tank

Fig. 46 Cooling water tank below graphite tube furnace

1. Unscrew fixing screws from cover sheet (4 and 6 in Fig. 25, p. 48), then remove cover
sheet.
2. Unscrew and pull off sensor terminal for cooling water level (1 in Fig. 46).
3. Unscrew cover (2 in Fig. 46).
4. Refill cooling water tank with tap water until water level reaches 2 cm above the upper
edge of the square tank.
5. Screw on cover with moderate force.
6. Screw cooling water level sensor firmly on.
7. Attach cover sheet with the help of screws.

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7.3 Maintaining the graphite tube furnace


After a prolonged operation time, sample residues, modifiers and sublimated carbon
particles of the graphite tube are deposited on the contact surfaces of the graphite
electrodes, the furnace jacket, the radiation sensor and the pipetter insert. These deposits
can be a source of contamination and can lead to increased deviations of the formatting
factor.
A damaged furnace jacket, ceramic ring and graphite tube can be the cause of substandard
analysis results.

CAUTION! THERE IS A RISK OF BURNING YOURSELF ON THE HOT


GRAPHITE TUBE FURNACE!
Allow the graphite tube furnace to cool down before attempting any service or maintenance
work.

CAUTION! DO NOT DAMAGE THE FURNACE WINDOW!


Do not touch the quartz panes of the furnace windows with your bare fingers!
Fingerprints burn in.

7.3.1 Cleaning the furnace windows

CAUTION!
Do not clean the furnace windows in an ultrasonic bath. This may lower the UV permeability
of the windows.
Do not touch the quartz panes of the furnace windows with your bare fingers! Fingerprints
burn in.
Danger of brittleness for rubber seals. When cleaning the furnace windows with alcohol,
make sure that the rubber seals do not come in contact with the alcohol.

IMPORTANT
After cleaning the sample chamber window with alcohol, it takes approx. 1 h until the
complete UV transmission has been restored.

Only use cleaning solution for cleaning (order no. 407-320.002).


Preparation of the cleaning solution: Use a mixture of demineralized water and 1 vol%
cleaning solution.
1. Pull off the furnace windows by hand with a twisting motion.
2. Fill the glass beaker with cleaning solution until the furnace window is fully immersed.
3. Allow the solution to soak at 25 to 30 °C for approx. 30 min.
4. Remove the furnace window from the cleaning bath (use plastic tongs or similar, do not
touch optical surfaces) and rinse under deionized water (<1 µS/cm).
5. Blow dry with compressed air or argon.
6. Re-attach the furnace windows.
The furnace windows are tilted in the holders. Identical markings must face upward!

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7. If the furnace windows are too loose or if the sealing rings of the furnace windows
exhibit brittleness and cracks, replace the sealing rings.

Fig. 47 Identical markings at the furnace windows facing upward

7.3.2 Cleaning the graphite surfaces


The graphite surfaces must be cleaned after daily use as required.
1. Switch on the contrAA 700 and start the ASpect CS software (the movable furnace part
must be pressurized to be opened/closed).

2. In ASpect CS use to open the FURNACE window. Go to the CONTROL tab.


3. Open the furnace with the [OPEN FURNACE] button.
4. Remove the pipetter insert from the furnace jacket and clean it in 0.1 - 1 N HNO3.
Then wash thoroughly with slightly acidic or demineralized water.
5. Clean the contact surfaces of the electrodes in the movable furnace part with cotton
swab, lint-free cloth soaked in alcohol or blotting paper.
6. Clean the inner surfaces of the furnace jacket with a cotton swab.

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7.3.3 Cleaning and changing the graphite tube


Clean the standard graphite tube
Daily
Work steps, see Chapter "Cleaning the graphite tube / cleanout" p. 53.

Clean the iridium-coated graphite tube


Daily
Work steps, see Chapter "Cleaning the graphite tube / cleanout" p. 53.

Evaporation of iridium coating in the graphite tube


After approx. 500 atomizations or for a new coating.
Work steps, see Chapter "Cleaning the graphite tube / cleanout" p. 53.

Replacing the graphite tube


If the graphite tube appears to be burnt, the pyrolytic coating is worn out.
At a formatting factor ≥ +10 % an automatic temperature correction no longer takes place.
Further use of the graphite tube is limited. The graphite tube should be replaced.
Work steps, see Chapter "Inserting the graphite tube into the graphite tube furnace" p. 51.

7.3.4 Replacing the electrodes and the furnace jacket


If the electrodes have been cleaned and the graphite tube has been exchanged and the
formatting factor is still > 10 the electrodes and the furnace jacket must be replaced. You can
have the customer service perform these tasks as part of the annual maintenance.
If you wish to replace these parts yourself, you will need furnace tools which can be supplied
optionally.
1 Inserting tool for electrodes
2 Press-out tool
3 Inserting tool for furnace jacket
4 Face spanner
5 Ratchet wrench

Fig. 48 Furnace tools

1. Switch on the contrAA 700 and start the ASpect CS software (the movable furnace
part must be pressurized to be opened/closed).

2. In ASpect CS use to open the FURNACE / CONTROL window.


3. Open the furnace with the [OPEN FURNACE] button.

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4. Unscrew the covering screw from the


movable furnace part.

5. Withdraw the knurled pin and fold the


movable furnace part down.

6. Loosen the insulating ring carefully with the


face spanner and unscrew it completely by
hand.
Caution!
Risk of breaking the insulating ring!
Do not jam the face spanner!

7. Screw the press-out tool into the movable


furnace part with the spindle turned back all
the way to the stop and press out the
electrode completely using a ratchet
wrench. Unscrew the press-out tool from
the furnace part completely.

8. Pull the furnace window off of the furnace


jacket and remove the pipetter insert.

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9. Pull out the three gas tubes and carefully


screw out the three gas connectors.

10. Screw out the covering screw at the rear of


the fixed furnace part by hand.

11. Screw the press-out tool into the fixed


furnace part with the spindle turned back all
the way to the stop and press out the
electrode and the furnace jacket completely
using a ratchet wrench. Loosen the press-
out tool and unscrew it completely.

12. Arrange a new electrode parallel to the


fixed furnace part and secure it with the
inserting tool (small bracket).
13. Use the ratchet wrench to insert the
electrode to the stop. Loosen the inserting
tool and remove it.
Caution! Risk of breaking the electrode!
Make sure that the electrode and the
furnace part are parallel when positioning
and inserting the electrode. If the electrode
is unintentionally positioned askew, remove
completely and start again.

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14. Align the furnace jacket with the rectangular


opening parallel to the furnace body and
fasten it with the inserting tool (large
bracket).
15. Insert the furnace jacket to the stop. Loosen
the inserting tool and remove it.
Caution! Risk of breaking the furnace
jacket!
When inserting, always make sure that the
furnace jacket and the fixed furnace part
are in parallel. If the furnace jacket has
unintentionally been positioned askew,
remove completely and start again.

16. Check the sealing rings of all three gas


connectors and replace if damaged.
17. Screw the long gas connector (arrow in
figure on left) (for the outer gas flow)
transversely from below finger-tight into the
fixed furnace part.
Attach the gas tube that is marked with a
white ring onto the long gas connector.
18. Screw the two short gas connectors (for the
inner gas flow) into the furnace jacket on
both sides.
Attach the two other gas tubes to the
corresponding gas connectors.

19. Screw in the covering screw at the rear of


the fixed furnace part by hand.

20. Attach the furnace window to the furnace


jacket and insert the pipetter insert.
Caution! Similar markings at the furnace
windows must face upward.

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21. Arrange a new electrode parallel to the


movable furnace part and secure it with the
inserting tool (small bracket). Insert the
electrode to the stop into the jaw using the
ratchet wrench.
Caution! Do not tilt the electrode. It may
break!
22. Any graphite dust should be removed by
suction or blown away.

23. Screw in the insulating ring by hand and


tighten it moderately using the face
spanner.
Caution!
Risk of breaking the insulating ring!
Do not jam the face spanner!
24. Check visually that the insulating ring
protrudes approx. 0.3 mm from the jaw.
25. Attach the furnace window to the furnace
jacket and insert the pipetter insert.

26. Insert the knurled pin (arrow) to the stop


into the furnace jaw and the connecting rod.
The connecting rod must be in the front
position.

27. Screw the covering screw to the movable


furnace part.

28. Close the furnace with the [CLOSE FURNACE] button.

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7.4 Burner-Nebulizer System


The burner-nebulizer system has to be cleaned at regular intervals, indicated by the
following:
 Irregularities in the flame hem of the burner flame. Washing with diluted acid in the
active program and blowing the burner out does not bring about any improvement.
 The sensitivity given in the cookbook for an individual element is not achieved
despite changing the composition of the gas.
 Build-up on the burner slit, which occur during analysis of solutions with a high salt
content, cannot be removed by the cleaning stick.

WARNING! SERIOUS RISK OF BURNING!


Allow the burner to cool down before attempting any service or maintenance work.

1. Take burner-nebulizer system apart.


2. Clean burner.
3. Clean nebulizer.
4. Clean siphon.
5. Clean mixing chamber.
6. Assemble burner-nebulizer system.
7. Adjust burner-nebulizer system (optimize flame).

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7.4.1 Disassemble burner-nebulizer system unit


1 Stud bolt on the burner
2 Mixing chamber tube
3 Mixing chamber screw joints (4 x)
4 Locking ring for nebulizer
5 Fixing screw for siphon
6 Connection of siphon sensor
7 Outlet tube from the siphon
8 Screwed tube connections on the
mixing chamber head and the
nebulizer
9 Safety plug
10 Knurled head screw on the holding
bow

Fig. 49 Deinstalling and taking the burner-nebulizer system unit apart

1 Safety plug 7 Nebulizer connection with locking ring


2 Mixing chamber tube 8 Impact bead
3 Impeller 9 Nebulizer with connection for oxidant and
connection for sample tube
4 Mixing chamber head with connections for gases,
nebulizer and siphon 10 Siphon
5 Connection for fuel gas 11 Siphon sensor
6 Connection for additional oxidant

Fig. 50 Mixing chamber and nebulizer disassembled

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Fig. 51 Withdrawing the nebulizer from the mixing chamber

1. Loosen the stud bolt (1 in Fig. 49, p. 86) on the burner and remove the burner from the
connector.
2. Unscrew the screwed tube connections on the mixing chamber head and the nebulizer
(8 in Fehler! Verweisquelle konnte nicht gefunden werden.) and pull off the tube from
the nebulizer connector.
3. Turn the locking ring of the nebulizer (4 in Fig. 49) to open the locking. Withdraw the
nebulizer from the mixing chamber head, holding the nebulizer in the groove (Fig. 51, p.
87).
Caution: Connector for gas connection may break when being pulled.
4. Unscrew the connection of the siphon sensor (6 in Fig. 49) on the rotating arm and pull it
off.
5. Pull off the outlet tube from the outlet connector of the siphon (7 in Fig. 49).
6. Loosen the knurled head screw of the siphon (5 in Fig. 49) and pull the siphon down.
7. Empty the siphon.
Caution! The solution in the siphon is acidic.
8. Unscrew the insert of the siphon sensor, remove the sensor from the siphon (11 in Fig.
50 p. 86).
9. Hold the system tightly, loosen the knurled head screw on the holding bow of the mixing
chamber tube (10 in Fig. 49), rotate the holding bow backwards and remove the system.
10. Withdraw the safety plug (1 in Fig. 50) from the mixing chamber.
11. Loosen the four screw joints of the mixing chamber (3 in Fig. 49) and disassemble the
mixing chamber into the chamber head and the chamber tube.
12. Remove the impeller (3 in Fig. 50) from the chamber tube.
13. Unscrew the gas connections for fuel gas and additional oxidant.

7.4.2 Clean burner


1. Clean the burner, exposing it to a jet of running water.
2. Clean the burner, keeping it for 5 to 10 minutes in an ultrasound bath of 0.1% HNO3
with the burner jaws facing down.

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Working steps in cases of very tenacious encrustation


3. Undo the fittings (2 in Fig. 52) of the burner jaws on the burner body and remove the
burner jaws.
4. Undo the fittings of the burner jaws against each other (1 and 3 in Fig. 52).
5. Remove the burnt residue build-up with the burner cleaner (timber wedge).
6. Clean the burner jaws in 0.1 N HNO3, and then wash with distilled water.
7. Screw the burner jaws together, making sure that the ends of the spacers on the burner
slit extension and the end faces are flush .
Caution: The spacers must not protrude over the upper side of the burner jaws (arrow
in Fig. 54)! When using a scraper, it remains attached.
8. Screw the burner jaws onto the burner body, the dowel pins (4 in Fig. 52) on the burner
ensure correct positioning.

CAUTION! USING THE SCRAPER!


When the spacers protrude over the upper side of the burner jaws, the scraper can get
caught and burn!

1;3 Burner jaw fittings against each other


2 Fittings of the burner jaws with the burner body
4 Dowel pins on the underside of the burner jaws

Fig. 52 Fittings of the burner

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1 Burner jaw
2 Spacers
3 Burner jaw
4 Burner body

Fig. 53 Burner, disassembled

Fig. 54 Spacers inserted in burner jaws

7.4.3 Clean Nebulizer


1. Put the nebulizer for several minutes in an ultrasonic bath with approx. 1% nitric acid or
organic solvent (isopropanol).
2. Turn the impact bead (8 in Fig. 50, p. 86) slightly and pull it off the nebulizer. Should the
impact bead stuck; put the nebulizer again in the ultrasonic bath.
3. Insert the cleaning wire into the nebulizer canula and clean the canula by moving it up
and down several times.
4. Attach the baffle ball on the nebulizer and lock it by turning slightly.

7.4.4 Clean mixing chamber


Mixing chamber tube and chamber head:
1. Clean with saltpeter, diluted mineral acid, or the appropriate solvent according to the
substances analyzed.
2. If the mixing chamber is cleaned with a diluted mineral acid, wash thoroughly with
distilled water after cleaning.

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7.4.5 Clean siphon


1. Clean with saltpeter, diluted mineral acid, or the appropriate solvent according to the
substances analyzed. Clean the channels with a round brush.
2. If the siphon is cleaned with a diluted mineral acid, wash thoroughly with distilled water
after cleaning.
3. Wash the float holder.

7.4.6 Assemble burner-nebulizer system unit

CAUTION! CHECK CONNECTIONS FOR LEAKAGE!


When connecting the supply tubes, ensure correct connection. Insert the seals and check for
leakage.
Tighten all screws by hand only.

1. Working steps for assembly Check all sealing rings of the chamber head, connections
and the nebulizer, replace worn out sealing rings, pull on seals and ensure correct
positioning.
2. Hold the impeller at the handle and insert it into the mixing chamber tube. Lock by
pressing slightly.
3. Stick the mixing chamber parts (chamber tube and chamber head) together, align the
sides so that they are flush and screw (3 in Fig. 49 p. 86).
4. Screw the siphon sensor (11 in Fig. 50, p. 86) in the siphon. Stick the siphon on the
chamber head, align the sides so that they are flush and fasten with knurled head screw
(5 in Fig. 49).
5. Attach the safety plug (1 in Fig. 50) on the chamber tube.
6. Screw the connections for fuel gas and additional oxidant (5 and 6 in Fig. 50) with the
sealing rings into the mixing chamber head.
7. Stick the nebulizer (9 in Fig. 50) into the chamber head and fasten using the locking
ring.
Note: If the nebulizer cannot be stuck easily into the chamber head, slightly grease the
sealing rings with the lubricant supplied (Apiezon grease).
8. Fasten the mixing chamber nebulizer system at the height adjustment using the holding
bow (10 in Fig. 49). The marking must be above the edge of the holding fixture. Screw
the knurled head screw at the holding bow tightly.
9. Plug the cable of the siphon sensor (6 in Fig. 49) into the connection on the rotating arm
(take care with the lug) and screw tight.
10. Set the burner on the mixing chamber tube and turn against the 0° stop. Clamp with
stud bolt.
11. Screw the tube for fuel gas (red marking) on the connector.
12. Screw the tube for oxidant (1 blue mark) on the connector.
13. Connect the tube for oxidant (2 blue marks) to the nebulizer connector.

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Sensitivity control / adjustment


1. Select the FLAME window of ASpect CS software.
2. Open the CONTROL tab and set oxidant-to-fuel-gas ratio.
3. Align burner head in relation to the optical axis in terms of height, depth and parallelism
(beam passage of xenon lamp).
4. Open the MANUAL OPTIMIZATION tab.
5. Let the nebulizer draw in test solution, for example, Cu / 2 mg/L, then trigger continuous
display mode of measured values. Evaluate the signal.
6. If the sensitivity is not reached, readjust the nebulizer:
Loosen the lock nut (3 in Fig. 55).
Adjust the depth of the canula (4 in Fig. 55) with the adjustment nut.
7. After completing the adjustment, secure the adjustment with lock nut (3 in Fig. 55).
1 Baffle ball
2 Connection for oxidant
3 Lock nut
4 Adjustment nut for canula
5 Inner canula

Fig. 55 Components of the nebulizer

7.4.7 Cleaning the sensor of the burner


The sensor monitors if the burner is mounted correctly before igniting the flame. Clean the
sensor of the burner if
• there are deposits (for example salt incrustations) on the openings of the sensor
• the inserted burner cannot be detected (shown by an error message in the software).
1. Remove the burner-nebulizer-system by loosening the knurled head screw on the
holding bow (10 in Fig. 49).
2. Clean the sensor cautiously with the help of a little brush, for example a toothbrush,
using alcohol, for example Isopropanol.
3. Reinstall the burner-nebulizer-system on the holding bow.

Fig. 56 Sensor of the burner

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7.5 Autosampler AS-GF


The following maintenance work must be performed on the AS-GF:
 Remove any contamination from the sample tray and the casing with a dry cloth on a
daily basis.
 Wash, service, replace the dosing tube.
 Clean, after a wash or mixing cup has overflowed.

7.5.1 Washing the dosing tube


The dosing tube must be washed prior to and after work. Washing solution is taken from the
storage bottle, pumped via the dosing syringe into the dosing tube and dispensed into the
wash cup.
1. Switch on the contrAA 700 and start the ASpect CS software.

2. In ASpect CS open the window AUTOSAMPLER with .


3. Use the [W ASH] button to start the wash cycle.
Note: If the dosing tube is not immersed properly into the wash cup during washing, the
autosampler must be realigned in the wash position.
4. In the window FUNCTION TESTS enable the button [ADJUST AUTOSAMPLER].
In the area ALIGNMENT POSITION enable the option W ASH POSITION. In the area
ALIGNMENT W ASH POSITION enter the immersion depth in the list field (approx. 40 mm).
Correct the alignment of the swivel arm with the arrow keys. Save the configurations
and exit the window.
Caution: When opening the window [ADJUST SAMPLER] again, a value of 13 MM is shown
under DEPTH, not the stored value.
5. The wash cycle can be repeated several times if required.
The wash cycle can be defined in the method and thus performed automatically prior to
and after the measurement.

IMPORTANT
If a method is active, pressing the [W ASH] button in the AUTOSAMPLER window results in the
processing of the number of Wash cycles set the method.

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Fig. 57 Window "Autosampler / Function tests" in the ASpect CS software

7.5.2 Servicing the dosing tube


A defective or kinked dosing tube or one with sediment deposits can be the cause of
distorted measurement results.
Maintenance work is:
 Cleaning the dosing tube
 Shorten the dosing tube
 Replace the dosing tube
1 Tube holder
2 Dosing tube
3 Tube holder
4 Screw top at the dosing unit
5 Tube guide lock screw
6 Tube guide clamp nut

Fig. 58 Dosing tube at the AS-GF

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Cleaning the dosing tube


The dosing tube requires cleaning, dependent on the sample material, when:
 The pH levels of the sample, the wash liquid and the air bubble are blurred, or if the
bubble is segmented.
 The sample is spread out in the tube (tube is contaminated on the inside).
An 8 to 13% sodium hypochlorite solution (NaOCl) is recommended as a cleaning solution.
The following cleaning procedure should be repeated as often as is necessary.
1. Fill the sodium hypochlorite solution into a 5 mL special cup and mount tray position 101
with it.
2. Switch on the contrAA 700 and start the ASpect CS software.

3. In ASpect CS open the window AUTOSAMPLER with . Change to the tab FUNCTION
TESTS (Fig. 57 p. 93).

4. In the area TRACKER/ROTATOR enter "101" into the list field and enable the option CUP
NO. The autosampler arm moves to position "101".

5. In the area DIPPING ARM in the list field DEPTH lower the autosampler arm into the
special cup with the arrow keys (approx. 50 mm).
Note: The autosampler is only lowered if the arrow keys are used. After entering the
value directly into the list field, click the arrow keys once again!
6. In the area PIPETTER, in the list field VOLUME [µL], use the arrow keys to set the volume
to be picked up (approx. 100 - 200 µL). The volume can be set in steps of 50 µL.
7. Press the button [TAKE UP]. The autosampler fills the dosing tube with the cleaning
liquid.
8. Allow the cleaning liquid to work for approx. 20 min.
9. In the area TRACKER/ROTATOR enable the option W ASH POSITION.
10. The autosampler arm moves to the wash position.
11. In the area DIPPING ARM in the list field DEPTH lower the autosampler arm into the wash
cup with the arrow keys (approx. 40 mm). When entering the value directly into the list
field, click the arrow keys once again!
12. Use the [DISPENSE] button to empty the dosing tube into the wash cup.
13. Start 5 wash cycles. (Click the [W ASH] button 5 times.)

Shortening the dosing tube of the AS-GF


1. Loosen the clamp nut at the tube guide (6 in Fig. 58) and remove the dosing tube by
pulling upwards.
2. Cut the dosing tube with a razor blade or a scalpel at an angle of 10° to 15°.
3. Push the dosing tube as far as possible into the tube guide until the dosing tube
protrudes by approx. 8 mm at the bottom.
4. Lock the dosing tube with the clamp nut.
5. Readjust the injection depth of the sample (→ section "Adjusting the AS-GF" p. 56).

Replacing the dosing tube of the AS-GF


1. Loosen the clamp nut at the tube guide (6 in ) and pull out the tube. Remove the tube
from the tube holders at the sample arm and the back of the autosampler (1 and 3 in
Fig. 58).

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2. Detach the screw top from the T valve of the dosing unit (4 in Fig. 58).
3. Screw the new dosing tube to the valve and feed it through the tube holders.
4. Push the dosing tube into the tube guide until it protrudes 8 mm at the bottom, lock with
the clamp nut.
5. Readjust the injection depth of the sample (→ section "Adjusting the AS-GF" p. 56).

7.5.3 Replacing the metering syringe


The details below apply to the samplers AS-GF (graphite tube) and AS-FD (flame). The
dosing units only differ in the size of the dosing syringe (500 or 5000 µL).
1 Valve
2 Dosing syringe, consisting of piston and glass cylinder
3 Attachment screw
4 Drive rod

Fig. 59 Dosing unit at AS-GF and AS-FD

1. Switch on the contrAA 700 and start the ASpect CS software. In the window MAIN
SETTINGS Select technique: GRAPHITE FURNACE (AS-GF) or FLAME (AS-FD).

2. Use to open the AUTOSAMPLER window. Change to the tab FUNCTION TESTS.
3. In the PIPETTER area, in the list field VOLUME [µL] , use the arrow keys to set the volume
to be picked up (AS-GF: 500 µL; AS-FD 5000 µL). Increase the speed to 6-7.
4. Press the button [TAKE UP].
The piston of the dosing syringe moves down.
5. Unscrew the fixing screw (3 in Fig. 59).
6. Unscrew and remove the dosing syringe (2 in Fig. 59).
7. Screw the new dosing syringe to the valve.
8. Carefully pull the piston down until the eyelet at the piston end is aligned with the hole in
the drive rod.
9. Screw the piston with the attachment screw finger-tight to the drive rod.
Caution: Excessive force can lead to material damage! Do not tighten the screw too
much.
10. In the window AUTOSAMPLER click on the [INITIALIZE] button.
The piston of the dosing unit moves back to the original position.

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Care and maintenance

7.5.4 Clean-up after cup overflow


If during the process a wash cup has overflowed, immediately interrupt the process and
clean the device.
1. Stop the process immediately.
2. Take up the liquid with cellulose wadding or cloth. Wipe the surface dry.
3. Ensure that the outlet can be drained, i.e., remove any sharp bends in the draining tube
or make sure that the draining tube does not dip into the liquid in the waste bottle.

7.6 Automatic samplers AS-F, AS-FD


Contamination on the tray and the casing can be removed with a dry cloth on a daily basis
as required. In addition according to conditions:
 Washing the sample paths
 Wash the mixing cup
 Replace the canula(s) at the autosampler arm
 Replace the aspiration tube and dosing tube
 Replace the dosage syringe, as for AS-GF (→ Section "Replacing the metering
syringe" p. 95)
 Clean, after a wash or mixing cup has overflowed

7.6.1 Washing the sample paths

1. In the software ASpect CS use to open the FLAME window and ignite the flame.

2. Use to open the AUTOSAMPLER window.


3. In the tab TECHN. PARAMETERS set approx. 60 s in the input field W ASH TINE W ASH CUP.
4. Use the [W ASH] button to start the wash cycle.
The canula of the autosampler dips into the wash cup. The wash liquid is aspirated through
the system.

7.6.2 Washing the mixing cup of the AS-FD


The mixing cup must be washed before and after the operation to prevent adhesion and
scaling. Before preparing the first standard / first sample the mixing cup is washed
automatically. Further washing processes might be useful during continuous operation.

Washing the mixing cup prior to and after the measurement

1. In ASpect CS open the window AUTOSAMPLER with .


2. In the tab TECHN. PARAMETERS enter a volume of 25 mL in the group W ASH MIX CUP.

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Care and maintenance

3. Use the [START] button to start the wash cycle.


4. The wash cycle can be repeated several times if required.
25 mL of washing liquid is dispensed from the storage bottle into the mixing cup and
automatically drained off afterwards.

Washing the system prior to an extended period of decommissioning


If salts were added to the diluent (bidistilled or acidic bidistilled water), the dosing unit and
valve must be washed with methanol or ethanol prior to extended periods of
decommissioning. Otherwise scaling and blocking may also occur.
1. Fill the storage bottle for the diluent with methanol or ethanol.
2. Perform the wash cycle as described in Section "Washing the system prior to and after
the measurement". Repeat the washing process several times.

7.6.3 Replacing the canulas and guide on the autosampler arm of


the AS-FD
The canulas and guide must be replaced if there is a significant contamination or mechanical
damage (detectable by large standard deviations in the measurements).
1. Pull off the hoses from the canulas.
2. Loosen the fixing screw on the autosampler arm.
3. Pull the canula guide with canulas upwards and out.
4. Fit the guide with the new canulas into the autosampler arm and fix in place with the
locking screw.

CAUTION! RISK OF FRACTURE!


Set the canula height for them to terminate 1-2 mm above the block with the wash and
mixing cup.
5. Plug the sample intake tube onto the thinner canula. Plug the dosing tube for the diluent
onto the thicker canula.

7.6.4 Replacing the canula on the autosampler arm of the AS-F


The canula for picking up the sample (thin canula) must be replaced if there is a significant
contamination or mechanical damage (detectable by large standard deviations in the
measurements).
1. Pull the intake tube off the canula.
2. Loosen the lock screw at the autosampler arm and pull out the canula.
3. Insert the new canula and fix with the clamp nut.

CAUTION! RISK OF FRACTURE!


Set the canula height for it to terminate 1-2 mm above the washing cup.

4. Plug the intake tube onto the new canula.

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Care and maintenance

7.6.5 Replacing the intake tube


If the intake tube is contaminated, it must be replaced.
1. Pull off the intake tube from the thinner canula at the autosampler arm and then from
the nebulizer canula.
2. Cut a new tube to the required size and attach it on both canulas.

7.6.6 Replacing the tube set for diluent and washing liquid at the
AS-FD
1. Pull the dosing tube for diluent off the thicker canula at the autosampler arm and feed it
through the tube guide (8 in Fig. 36 p. 63).
2. Detach the tube for the washing liquid at the rear of the autosampler (5 in Fig. 37 p. 65).
3. Pull the encased tubes out of the attachment lug at the rear of the autosampler.
4. Pull the tube for the washing liquid off the storage bottle.
5. Unscrew the dosing tube from the change-over valve (3 in Fig. 38 p. 65).
6. Screw the new tube set with dosing tube (marking "1") to the change-over valve and
attach the encased tubes with the attachment lug to the rear of the autosampler.
7. Insert the tube with the marking "2" into the storage bottle for the washing liquid.
8. Screw the tube for the washing liquid to the rear of the autosampler.
9. Slide the other end of the dosing tube through the tube guide onto the thicker canula of
the autosampler arm.

7.6.7 Clean-up after cup overflow


If during the process the washing cup or mixing cup (with AS-FD) has overflowed,
immediately interrupt the process and clean the device.
1. Stop the measuring process immediately.
2. Take up the liquid with cellulose wadding or cloth. Wipe the surface dry.
3. Washing cup: Ensure that the outlet can be drained, i.e., remove any sharp bends in the
draining tube or make sure that the draining tube does not dip into the liquid in the
waste bottle.
Mixing cup (only for AS-FD):
Use to open the AUTOSAMPLER window. Change to the tab FUNCTION TESTS.
In the area PUMPS enable the checkbox MIX CUP PUMP to start the pump.
Run the pump until the liquid has been drained off.
Disable the checkbox MIX CUP PUMP, to stop the pump

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Care and maintenance

7.7 Compressor JUN-AIR 6/S


IMPORTANT
Observe the maintenance and care instructions in the separate instruction manual
"Compressor JUN-AIR 6/S".

Maintenance work
1. Drain the water separator at the filter and the pressure cylinder:
Drain off the oily condensation water every one to three months by opening the drainage
tap.

CAUTION!
Condensation water sprays out when released under pressure.
Open the drainage tap carefully. Drain off the oily condensation water into a narrow necked
bottle with a tube.

2. Clean the aspirating filter:


A dirty aspirating filter impairs compressor performance. Clean or replace the filter at
least every six months.
3. Refill/change oil:
Note: Only use the special oil SJ 27!
Check the oil level in the gauge regularly. Refill the oil at the oil screw if necessary.
Change the oil every 12 months. To do this, unscrew the gauge glass and tilt the
compressor enough so that the used oil can drain off completely. Screw the gauge back
on and refill with approx. 0.75 liter of oil at the oil screw. Check the oil level.
4. Check the safety valve:
Allow air to escape from time to time by turning the knurled nut. The valve position is
thus prevented from sticking and the functioning is guaranteed.
Note: Do not damage the seal and do not alter the setting of the safety valve!

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Transportation of the contrAA 700

8 Transportation of the contrAA 700


Auxiliary tooling
 4 carrying handles
 19 mm W/F open-end wrench (included in delivery)
 17 mm W/F open-end wrench (included in delivery)

Working steps
CAUTION! RISK OF INJURY!
 Handles which are screwed in too loosely may give rise to damage during transport.
Screw in the handles up to the end stop.
 The device must be transported by at least 4 persons using the fixed screw-in
carrying handles (included in scope of supply).
The contrAA 700 is too heavy for two persons (→ Section "Technical data of
contrAA 700" p. 13). In addition, it is not possible to get an adequate grip for
transport without the screw-in handles. There is a risk of injury if transport is
attempted without using the handles or by too few people.

1. Deinstall all components (refer to chapter "Installation and start-up" p.45. Make sure
that drain tube was removed from sample compartment.
2. Unscrew door before flame sample compartment.
3. Break gas supply up-line of all gas inlet ports.
4. Detach gas supply tubing on the back of the contrAA 700:
− Detach argon tube from tube clip.
− Use 17 mm W/F open-end wrench for air supply port.
− Use 19 mm W/F open-end wrench for acetylene gas port.
Left-hand threading!
− Use 19 mm W/F open-end wrench for nitrous oxide supply port.
5. Use 19 mm W/F open-end wrench for acetylene gas supply port. Left-hand threading!
6. Detach electrical cables.
7. Remove four seal plugs from the mounting holes for carrying handles on both sides of
the contrAA 700 and keep them in a safe place.
8. Screw all four carrying handles fully in until they are firmly seated in mechanical stop
position.

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Disposal

9 Disposal
Typically, atom absorption spectrometry generates only liquid waste which, besides metal or
heavy metal ions, mainly contains various mineral acids that are involved in sample
preparation procedures. For safe removal, such resulting waste solutions must be
neutralized, using, for example, diluted sodium hydroxide solution.
Once neutralized, such waste must be made available for proper disposal in accordance with
currently valid rules of law.
Under currently binding legislation, the contrAA 700, including its electronic components,
must be disposed as electronic waste on expiry of the rated service life.
You are requested to dispose of the xenon lamp in accordance with local rules or contact the
Customer Service of Analytik Jena AG for this purpose.

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Abbreviations / terms

10 Abbreviations / terms
EA Electrothermal atomizer
TTP Temperature-time programming / furnace program
EA operation Operation with electrothermal atomizer
Analysis line A spectral line defined by an analyzing instruction
Analyte Element to be analyzed
Atomizing Sample is vaporized to produce atoms
Clean-out Clean-out of the graphite tube furnace to a temperature at which all
sample residues in the furnace have been evaporated (i.e. furnace
cleaning).
AZ Autozero for the analysis
Determination limit The minimum weight (concentration) of the element to be analyzed
that can be determined with a defined precision. Also see detection
limit.
Reference solution Solution which can contain the analyte in a known concentration,
and according to requirements, the chemicals used for creating the
sample solution. It may also contain the matrix components which
influence the measurements and which are also contained in the
sample solution.
Blank value solution Solution which contains the chemicals which are used for creating
the sample solution but does not contain the sample matrix.
Characteristic mass Mass of the element to be analyzed which yields an absorbance of
A = 0.0044 (corresponds to 1 % absorption); analog: "characteristic
concentration").
Formatting Heating the graphite tube furnace via several predefined
temperature set-points to the maximum temperature. The actual
temperatures are measured and by comparing rated and actual
temperatures, a correction factor for controlling the specific graphite
tube is calculated. A new graphite tube is "burned in" during this
process.
ID/Wt Identity and weight. Identity data and weight/mass of a sample.
Continuum source Radiator, the radiation of which is continually distributed over a
large wavelength range. The contrAA 700 uses a xenon lamp as an
excitation source.
Neutral value solution Solution which contains the chemicals used for creating the sample
solution and also the components which influence the measurement
in the same or similar concentration as the sample to be analyzed.
No analyte is added to this solution.
Methods A method includes all data required for the analysis of samples of a
specific element, i.e. the spectrometer, atomizer, calibration,
sample, autosampler and QC settings, if necessary also the
settings for the QC charts and the results windows (if these
parameters have been included in the method).
Methods can be saved and reloaded. When changing from one
method to another, all ASpect CS settings are transferred to the
new analysis task.
Measurement solution Any solution that is measured directly.
Measuring program A collection of methods which requires compatible analysis

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Abbreviations / terms

conditions (i.e., the same analysis technique, the same


autosampler, etc.) and which has been put together in a specific
order. A measurement program is used to analyze a sample
sequence (semi)automatically for different elements "at the same
time". ("At the same time” means that all samples are analyzed first
for one element and then for the next element).
A measurement program can also consist of only one method.
Modifier Addition for changing the physical and chemical characteristics of
samples.
Detection limit The weight (concentration) of the element to be analyzed that can
be detected with a defined statistical certainty. Also see
determination limit.
Zero solution Solution which is used to set the zero point. This can be the solvent
or the blank value solution or neutral value solution.
Precision Measure of the statistical deviation of the measurement values from
a mean value (standard deviation, relative standard deviation)
Sample solution Solution which originates after treating the sample to be analyzed
according to the analysis instructions. If no additional processing
steps are required, this is the measuring solution.
Pyrolysis Most effective removal of incidental substances from the sample by
heating in the graphite tube furnace, without vaporizing any part of
the analytes.
QC Quality control. Concerned with samples and processes for
monitoring the quality of the analysis over time.
Serial precision Precision of several measurements over several days (e.g., 20-fold
determination in medicine: 20 days, each with 20 measurements)
Statistical series For calculating the statistical accuracy of an analysis, the individual
sample is analyzed for the current element several times in a row.
This sample analysis series is defined as a statistical series in this
manual.
Stock solution Solution of a suitable composition (diluent, acid type, acidic content,
etc.) which contains the analytes in high and known concentrations.
The stock solution is used for making reference solutions.
Background Evaluation of measurement value with no background. The
compensation background compensation occurs simultaneously.
Background Measurement of the spectral background in the environment or
measurement under the analysis line.

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EC Declaration of Conformity

11 EC Declaration of Conformity

104 Issue 01/2014 contrAA 700

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