Analytik Jena Contraa 700 Labrecycling
Analytik Jena Contraa 700 Labrecycling
Analytik Jena Contraa 700 Labrecycling
User Manual
Service: Analytik Jena AG
Kundendienst
Konrad-Zuse-Str. 1
07745 Jena
Germany
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!
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
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
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
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.
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.
IMPORTANT
Indicates application hints and other especially useful information without any resulting
hazardous or damaging situations.
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.
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.
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.
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.
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.
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.
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
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
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.
Furnace fuse
Type Protected current circuit
TR5-T 100 mA Graphite tube furnace
Ambient conditions
acc. to DIN ISO 90022-2:2003 / 01
Autosampler AS-GF
Autosampler with Dilution Function, complete PC Control
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.
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
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)
Autosampler AS-FD
Autosampler with dilution function, completely PC-controlled
Injection Module
PC-controlled
Scraper
PC-controlled
Hg/Hydride Systems
HS 60 modular; HS 55 modular; HS 50
Refer to Hg/Hydride Systems user manual.
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)
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.
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!
Table 1 Dimensions and weights of the contrAA 700 and its system components
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
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.
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.
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
Absorption(Flame) Absorption(Flame)
Monochromator Monochromator
(low resolution) (high resolution)
Detector Detector
(Photomultiplier) (CCD line)
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:
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.
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.
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.
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.
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.
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.
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.
IMPORTANT
Manual pipetting is not recommended because of the poor reproducibility rate.
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).
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.
SSA 600 with liquid dispensing SSA 6z for manual sample supply
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.
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.
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
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.
Fig. 22 Main power switch and connector strip terminals for utility supplies and controls
on the right-hand side of the contrAA 700
Fig. 24 Rear panel view of contrAA 700 with ports and terminals for gas and electric
power supply, including fuse holders
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!
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.
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.
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.
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.
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
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.
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
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.
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
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
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).
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
IMPORTANT
For further configurations of the autosampler see the instruction manual "Aspect CS" /
section "Technical autosampler parameters".
IMPORTANT
The population of the sample tray must match the software configuration in the method or in
the sample ID.
Fig. 33 Terminals at the burner-nebulizer system unit available for flame technique
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)
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.
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
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.
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
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.
Fig. 39 SFS 6 installed at the contrAA 700 for manual sample delivery
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.
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. 41 Fixing rail with burner mounted / knurled thumb screws at scraper
CAUTION!
The HPT burner head can only be used for the air-acetylene flame up to a fuel gas-air ratio
of 0.16.
The AAS system is operational now and you may proceed to actual work (for
preparation of analytical jobs and measurement).
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.
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.
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!
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.
IMPORTANT
After cleaning the sample chamber window with alcohol, it takes approx. 1 h until the
complete UV transmission has been restored.
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.
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. 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.
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.
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.
1. Switch on the contrAA 700 and start the ASpect CS software (the movable furnace
part must be pressurized to be opened/closed).
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.
1 Burner jaw
2 Spacers
3 Burner jaw
4 Burner body
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.
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.
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.)
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).
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.
1. In the software ASpect CS use to open the FLAME window and ignite the flame.
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.
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.
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.
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.
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
11 EC Declaration of Conformity