brief - instruction - contrAA300 - 600 - 700 - en - копія

Short Instruction
for the development of analytical methods using

the HR-CS Atomic Absorption Spectrometer
®
contrAA 300/600/700
Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 2/ 83
Analytik Jena AG | Konrad-Zuse-Straße 1 | 07745 Jena/Germany | info@analytik-jena.com | www.analytik-jena.com
Index
Index .................................................................................................................................... 3
1 General information ...................................................................................................... 5
2 Flame technique ........................................................................................................... 5
2.1 Start-up of the contrAA 700 for flame-AAS .......................................................... 5
2.2 Creating a simple method ..................................................................................... 7
2.2.1 The cookbook................................................................................................. 7
2.2.2 Processing the method .................................................................................. 9
2.2.2.1 The Lines tab ............................................................................................ 10
2.2.2.2 The Flame tab .......................................................................................... 11
2.2.2.3 The Sample Transport tab ........................................................................ 12
2.2.2.4 Performing automatic flame optimization .................................................. 13
2.2.2.5 The Evaluation tab .................................................................................... 15
2.2.2.6 The Calibration tab ................................................................................... 18
2.2.2.7 Definition of stock and calibration standards ............................................ 19
2.2.2.8 The Statistics tab ...................................................................................... 20
2.2.2.9 The Output tab.......................................................................................... 21
2.3 Creating a measurement sequence .................................................................... 22
2.4 Performing a flame measurement ....................................................................... 24
2.4.1 Results screen ............................................................................................. 26
2.4.2 Verification of the measurement data ........................................................... 27
2.4.2.1 Relative standard deviation ...................................................................... 27
2.4.2.2 Spectrum .................................................................................................. 27
2.4.2.3 Calibration function ................................................................................... 28
2.4.2.4 Recalculation of datasets ......................................................................... 29
2.4.3 Print-out of the measurement protocol ......................................................... 30
2.4.4 Definition of a reslope measurement............................................................ 31
2.4.5 Integration of quality control samples ........................................................... 32
2.4.6 Creating control charts ................................................................................. 33
2.4.7 Performing a standard addition/addition calibration ..................................... 34
2.5 Special applications in Fl-AAS ............................................................................ 36
2.5.1 Optimization of baffle ball (impact bead) and nebulizer ................................ 36
2.5.1.1 Optimization of the nebulizer for the spray chamber from PPS (shipment
since 2010) ............................................................................................................. 38
2.5.1.2 Optimization of impact bead and nebulizer for the PTFE spray chamber
system (Shipment until 2010) ................................................................................. 39
3 Graphite furnace technique ........................................................................................ 40
3.1 Startup of the spectrometer for the graphite tube technique ............................... 40
3.2 Creating a simple method ................................................................................... 41
3.2.1 The cookbook............................................................................................... 41
3.2.2 The Method screen ...................................................................................... 43
3.2.2.1 The Lines tab ............................................................................................ 44
3.2.2.2 The Furnace tab ....................................................................................... 44
3.2.2.3 The Sample transport tab ......................................................................... 46
3.2.2.4 The Evaluation tab .................................................................................... 46
3.2.2.5 The Calib. tab ........................................................................................... 49
3.2.2.6 Definition of stock and calibration standards ............................................ 51
3.2.2.7 The Statistics tab ...................................................................................... 52

3.2.2.8 The Output tab.......................................................................................... 53
3.3 Preoptimizing the temperature-time program ...................................................... 54
3.3.1 Sample drying .............................................................................................. 56
3.3.2 Pyrolysis ....................................................................................................... 57
3.3.3 Atomization .................................................................................................. 57
3.3.4 Clean out ...................................................................................................... 57
3.3.5 Fine optimization of the temperature-time program...................................... 58
3.4 Creating a measurement sequence .................................................................... 60
3.5 Performing a graphite tube measurement ........................................................... 62
3.5.1 The Results screen ...................................................................................... 64
3.5.2 Checking the measurement data ................................................................. 65
3.5.2.1 The Calibration function ............................................................................ 66
3.5.3 Performing an automatic spike recovery test (QC spike) ............................. 67
3.5.4 Programming a standard addition/additions calibration................................ 68
3.6 Special applications in graphite furnace AAS ...................................................... 70
3.6.1 Adjusting the Autosampler MPE 60.............................................................. 70
4 Special methods and techniques in HR-CS-AAS ....................................................... 72
4.1 Background compensation .................................................................................. 72
4.1.1 Compensation of broadband background absorption................................... 72
4.1.2 Compensation of structured background absorption .................................... 74
4.1.2.1 Structured background in the graphite tube technique ............................. 76
4.1.3 Performing a spectrum correction ................................................................ 77
4.1.3.1 Recording the correction spectra .............................................................. 77
4.1.3.2 Creating a correction model...................................................................... 78
4.1.3.3 Integrating the correction model into the method...................................... 80
4.2 Iterative background correction (IBC) .................................................................. 81
4.2.1 General ........................................................................................................ 81
4.2.2 Examples of application of the IBC method ................................................. 81
4.2.2.1 Noisy baseline .......................................................................................... 81
4.2.2.3 Broadband absorption by matrix components .......................................... 82
4.2.3 Programming the IBC method ...................................................................... 83

1 General information
These instructions describe the fast startup of the contrAA 300/ 600/ 700 and provide an
introduction to the use of the AspectCS software for flame and graphite-furnace determination.
Based on cookbook methods, the user should setup simple methods and from this be guided into
the structure of the AspectCS user interface.
 Prerequisite for the startup of the AAS device contrAA 700 is the proper connection to
the electrical power and gas supply, as well as the professional system installation by an
approved AJ service technician. At this installation procedure a first configuration of the
software is already performed.
 The contrAA 700 contains several assemblies:
Radiation source: Xenon short arc lamp

Atomization unit: Flame unit or graphite furnace
Spectrometer: Echelle double monochromator
Detector: CCD array
 Communication between the PC and measuring device is provided by the Aspect CS
application software.
2 Flame technique
2.1 Start-up of the contrAA 300/700 for flame-AAS
 Turn on the PC and printer and wait until the computer has finished booting up
 Activate the AAS device power switch. The contrAA 700 is initialized. This process takes
several minutes, during which the following processes are carried out automatically
o Initialization of wavelength drive
o Initialization of the burner height adjustment
o Ignition of the xenon short arc lamp
o Focusing the lamp focal spot
o Initialization of the accessories (autosampler and/or hydride system)
 The device is ready for measurement when the lamp is ignited and the focal spot is
aligned

Note:
 The contrAA must not be started at the same time as the control computer because this
could cause initialization errors.
 Start the AspectCS® software by double clicking on the AspectCS® icon.

The Main Settings window is displayed.
 For measurements in the flame

technique, activate Flame.
 Activate Initialize, to establish the
connection between software, AAS
device and accessories.
 In the table system configuration all

modules and accessories that have
been recognized by the software are
now displayed.
 In the Task table select Method

Development and confirm by OK.

Note:
 In contrast to Method Development, the Routine option, contains several limitations,
which are defined by the user hierarchy. More details on this can be found in the user
manual or the software help file. The options Data Management or Options take you
directly to the basic software settings where the screen display or data storage can be
configured.
 A basic configuration is performed already by service during system installation.

 The working interface of the

AspectCS® software is displayed.
2.2 Creating a simple method
2.2.1 The cookbook
 The software contains 'cookbook' values for the most important measurement parameters,
such as flame type, fuel gas composition or burner height, for most of the elements to be
determined using the flame AAS. When the elements are selected, these cookbook values
are automatically loaded and a method is created that is used as the starting point for
further method development.
 This cookbook data can be viewed as follows:
 Open Cookbook in the Method Development pull-down menu or
click on the icon .

 The cookbook is opened and a
periodic table is displayed.
 Now select the element to be
determined.
 Under Spectrometer the cookbook

screen contains information on the
recommended measurement
wavelength, alternative wavelengths
and their sensitivity compared to the
primary wavelength
 Under Flame parameters there is

information provided on the
recommended flame type, fuel gas
flow and burner height. Under
Analytical Data you find information
on measurement sensitivity.
 Under Remarks there is also given

information on the preparation of
standard solutions and samples,
required additives, such as ionization
buffers or information on possible
interferences.

Processing the method
 After closing the cookbook, click on the Method icon or select New Method in the File pull-
down menu.
If another method has been loaded previously an additional query is displayed. Here
choose basing on standard methods.
 The empty Method window is

displayed.
 Click on New to add elements.
 Now select one or more

elements from the periodic table
that is displayed and for each
element select the desired
measurement wavelength.
 The most sensitive Line is
indicated by P for primary
wavelength, the secondary line is
indicated by S.
 Close the periodic table with OK.

Note:
 The recommended wavelength for the measurement does not necessarily match with the
primary line. Please refer to the cookbook Remarks.
 Only combine elements in one method that can be determined with the same flame type,
i.e. either elements that can be measured with air/acetylene flame or nitrous oxide/
acetylene flame. For more information refer to the Cookbook, chapter 2.2.1.

 The method window now
contains the list of selected
elements.
 The flame parameters are
loaded from the cookbook.
2.2.1.1 The Lines tab
 The first tab, Lines has different columns with entries that can be edited if necessary.
Type (= measurement type) Typically Absorption; can be changed to

Emission using the pull-down menu.
Wavelength Displays the selected wavelength; can also be freely edited.
Line Line designation is displayed automatically; can be freely edited.
Signal evaluation For flame AAS, typically the ‘mean’ value is calculated. As an
alternative, with the injection technique, the peak area or height
evaluation may be selected.
Measurement time In flame AAS typically 3-5 s; can be freely edited.
Group If the same group is defined for all the elements, then the
elements are measured in fast progression. If you wish to
additionally repeat the measurement delay time prior to the
measurement of a certain element, select a different group
number for this element. This may be advantageous for elements
that require a highly different flame composition.
Order Measurement order of the analysis lines within one group.
Optim. Using this command, the measurement order can be
automatically optimized according to increasing fuel gas flow.

2.2.1.2 The Flame tab
 The Flame tab contains the flame parameters, fuel gas flow rates and burner heights,
which are loaded from the cookbook. These parameters can be manually edited or
determined by an automatic flame optimization (refer to chapter 2.2.2.4).
Flame/Type The displayed flame type corresponds to the last one active. If
necessary, change flame type.
Burner-nebulizer/type Check if the listed burner head is the same as the installed
burner.
Burner angle/Nebulizer The burner angle is generally 0°, but can be changed by
rate manually turning the burner head to reduce the measurement
sensitivity.
Rule of thumb: Rotation by 10°, Sensitivity decreases by a
factor of 2-3. Rotation 90°, Decrease by a factor of 10.
Manual rotation can be entered here for documentation in the
protocol. The nebulizer rate can also be documented in this way.
Both Parameters are not automatically detected by the system.

2.2.1.3 The Sample Transport tab
 The accessories installed on the contrAA are defined on the Sample Transport tab.
 If an autosampler or the injection module is installed (for installation refer to the manual),
activate the corresponding fields.
 The measurement delay time must be adapted depending on the length of the aspiration
capillary. The following delay times are recommended provided if a pre-run measurement is
used in each case under Statistics. If the measurement is performed without a pre-run
measurement, the listed delay times must be increased by approx. 3s.
- Short aspiration capillary, working manually: 8s

- Standard aspiration capillary, working manually: 12s
- Injection module SFS, working manually: 18s
- Autosampler AS 52 S without injection module: 18s
- Autosampler AS 52 S with injection module: 20s
 The Load and Injection time parameters are only active in the injection technique, if peak
area or height is set under Line/Evaluation.

2.2.1.4 Performing automatic flame optimization
 Since the optimum burner height and the gas composition strongly depend on the
respective analyte, the values, preset from the cookbook, should be fine-adjusted once for
each new element. Therefore one or more standard solutions, containing the analyte
elements in a suitable concentration, are needed. The use of commercially available
multielement solutions is recommended.
 The suitable standard concentration can be estimated using the information of the
corresponding cookbook screen. Under test concentration there is an analyte concentration
defined that generates an absorption signal of approx. 0.1A. If this value is multiplied by
factors of 2-3, a standard concentration suitable for the optimization is achieved.
 The optimization is performed using Automatic Optimization. Depending on your
respective device configuration, this optimization can run as a fully automatic or as a semi-
automatic routine.
 Click on the Flame symbol.
 The first page control

indicates whether all
gas pressures are OK
or any of the other
control sensors show
an error. If necessary
rectify the indicated
problem.
 In the Control window ignite the flame applying the Ignite Flame command.
 If a nitrous oxide/acetylene flame is being used for measurement, after ignition of the
air/acetylene flame, the Air N2O button must be used to manually switch to nitrous oxide.

 Open the window Automatic
Optimization and, if an
autosampler is being used, enter
the position of the optimization
standard.
 If all lines need to be optimized,
activate All lines.
 If the lines should be individually
optimized or from different
solutions, select the analyte line
from the pull-down menu and
start the optimization
measurement with Start.
 A query appears asking if the

optimized values should be
directly transferred into the
method and if the optimization
data should be saved
automatically.
 The latter is especially rec-
ommended for documentation
purposes. Start the optimization
with OK. The system performs the
optimization automatically. If no
autosampler is installed, follow the
software instructions.
 The software now starts an

algorithm, which gradually varies
the gas composition and burner
height and calculates the signal.
The system selects the parameter
settings that provide maximum
sensitivity and repeats the
measurement under these
conditions at the end of the
routine.
 The optimized data, if previously
defined, is now transferred
automatically into the method.
 The flame parameters are now optimized. Now using the Opt. command in the Lines
register, the sequence of the measurement can be optimized according to the flame
parameters.
 The method should now be saved to accept the values.

2.2.1.5 The Evaluation tab
 The Evaluation tab contains the line-specific evaluation parameters for determining the
measurement results from the spectra.
 The specifications loaded from the cookbook offer good starting conditions for simple
applications, but can be changed if necessary.
Spectral range  A maximum of 200 pixels of the CCD array can be selected
for evaluation. Considering the spectral range per pixel this
corresponds to a spectral range of approx. 0.4 nm,
depending on the wavelength range chosen. If 200 pixels are
defined for evaluation, this entire range is displayed in the
spectrum window. As not for every application the full
information over such a large wavelength range is needed
the number of evaluation pixels can be reduced. But in any
case, a minimum of approx. 100 pixels must be selected if a
dynamic BGC fit has been selected (see illustrations).

Spectrum with 200 evaluation pixels Spectrum with 100 evaluation pixels

Eval.pixel
 The maximum of the absorption line is expected on pixel no. 101.
Since the absorption profile is larger than the range of an
evaluation pixel, adjacent pixels can also be included for
evaluation, i.e. the absorption signal is integrated over several
measurement pixels. Generally 3 or 5 pixels are used for
evaluation in flame AAS.
Note:
 An increase in evaluation pixels to 5P leads to a better relative standard deviation and to a
higher measurement sensitivity.
 Lowering to 3P mathematically improves the detection limit.
Spectrum with 3 evaluation pixels (orange bar) Spectrum with 3Spectrum

evaluation
with
pixels
5 evaluation
(orange bar)
pixels
Background
 Since the hot flame, and also other atomization units, can emit spectral
correction
emission and absorption spectra that contributes to the analyte signal a
reference measurement with ultrapure water must be performed prior to
measurement of the sample. The spectra recorded in the reference
measurement are then automatically subtracted from the sample
spectrum.
 The reference measurement corresponds to the autozero in the
conventional AAS and should be repeated at regular intervals.
Perm. struct.
 The AspectCS® software contains a mathematical algorithm, eliminating
permanent absorption structures of the flame, such as O-H molecular
bands etc. Activation of this algorithm can be advantageous for
measurements in the low wavelength range or when the nitrous oxide
flame is applied.

GBC fit
 The background correction is performed simultaneously to the
measurement of the analytes from the measured spectrum. Along with
the absorption line, adjacent pixels are selected, which show pure
baseline noise and therefore represent the baseline. The selection of
these connection pixels can be done manually (static) or automatically
(dynamic) via the software. In dynamic mode (basic setting) a special
algorithm calculates the position of suitable correction pixels. If the
correction pixels should be manually defined, in the pull-down menu
select the Static option and in the adjacent field enter the pixel numbers
to be chosen for correction.
Note:
 The columns can be filled and changed by using the autofill function .
Fe spectrum with dynamic Fe spectrum with static

correction correction at pixel 90 and 112
The grey bars represent those correction pixels
the automatic algorithm recognized as showing
pure baseline noise. The second Fe line in the
spectrum is recognized as real absorption
structure and therefore is not included for
correction.

2.2.1.6 The Calibration tab
 To program a calibration, open the Calib. tab.
Calibration Select the desired type of calibration. In flame AAS this typically is the
techniques Standard calibration , applying aqueous calibration solutions.
Std. prod. From the pull-down menu select whether the reference solutions will
be manually prepared or should be automatically diluted by the
autosampler from a standard stock solution. The latter option is only
accessible if an autosampler has been defined.
Volumes Option is only visible/editable, if an autosampler with dilution option

has been defined. Please enter the amount of standard solution to be
prepared in the mixing cup. The required amount depends on the
number of lines (elements) to be measured.
Note:
The default filling volume is 20 mL. It can be reduced if less than 4
elements/lines are measured.
Calib. function Please select the type of calculation for the calibration function.
Linear, Nonlinear or Automatic calculation can be chosen. Details
on the calibration options can be found in the software help function.
Note:
The type of calculation can be changed and the data be recalculated
at any time.
Intercept and If required these parameters can also be changed. In the default
weighting setting allows the intercept is calculated and the calibration data are
not weighted.
Test Optional. Outliers can be recognized and eliminated automatically by
the software. For details please refer to the help function.
Unit Select the unit of the calibration function. For flame AAS this is
generally mg/L.

2.2.1.7 Definition of stock and calibration standards
 If the preparation of standard solutions has been set by autosampler, open the Stocks
window to define the stock solutions.
 An empty screen is displayed. Click on New, to add stock solutions.
 In the selection box that is displayed, choose whether

the stock solution will be loaded from a previously
defined database or if the concentrations will be
entered manually.
 If manual input was selected, the Stock standards

screen is displayed. Open the Concentrations field
and define the corresponding concentrations of the
stock standards.
 The autofill option is also available to fill the table
quickly.
 Confirm the concentrations with OK.
 Now the position of the standards in the autosampler
can be defined on the Stock standards screen.
Note:
 Please select the concentration of the stock solution
about a factor of 4 to 5 higher than the highest
standard solution.
 Return to the Calibration list and

click on Concentrations.
 A screen is displayed in which the number of calibration blank values and calibration
standards can be defined.

 In the same screen the volume of
stock standard can be defined in
% or the standard concentrations
can be defined manually.
 The autosampler position is
automatically applied.
2.2.1.8 The Statistics tab
 In the Statistics page the statistical methods are selected to be used for the calibration and
sample measurement. The settings do not depend onto the selected calibration method and
remain unchanged with anyother changes of the method.
Type of statistics Select the favorized type of statistics. In AAS this typically is the
mean value statistics.
Confidence interval Select the required option. Details on this topic can be found in
calculation/probability the AspectCS® help function.
Number of repeat Define the number of repetitive measurements which should be
measurements performed for each calibration standard, for each quality control
sample or analysis sample.
Note:
In AAS generally 3 - 5 repetitive measurements are used. For

stabilization of the burner/ mixing chamber system, the selection
of a pre-run measurement is recommended. For this a
measurement is performed, but the measurement data is not
included in the averaging calculation.

Grubbs An outlier test is provided in the software, that can be activated for
outlier test 3 replicate measurements or more. Outliers are eliminated and
are not used for the calculation of the statistics. The average
value determined are marked with "!" in the output table.
2.2.1.9 The Output tab
 The options for the automatic saving of Spectra and Methods are already activated under
Output. It is recommended to stay with this setting.
 Then the desired number of decimal places and the printing sequence can be set for each
element.
 A complete flame method has been created, which contains the optimized flame and
calibration parameters. Now the method should be saved under a unique name. For this
click on Save and enter a suitable method name. The method can also include a remark.
Close the window with OK.
Note:
 When storing the methods the method version is automatically indicated with a version
number that automatically increases with every storage process.
 The integration of quality control samples is described in chapter 2.4.5.

2.3 Creating a measurement sequence
 Click on the Sequence icon in the main menu or select New sequence from the File pull-
down menu.
 The empty sequence screen

is displayed.
 Select New.
 Define the sequence of the

measurements from the list
which is displayed. Always
start with a reference
measurement. For this click
on Reference and confirm
with Accept. The reference
measurement is then
included in the work
sequence.
 Select Calibration and
confirm with Accept.
 A typical sequence can be constructed as follows:

- Reference measurement
- Calibration
- Number of samples X
 When the last point for selection is reached, e.g., number x of samples, confirm with OK.
The selection is accepted and the selection window closes.
Note:
 There also can be special actions added to the sequence, such as a shut-down of the
flame at the end of the measurements.

 The sequence now looks as follows:
 Fill out the missing

information for sample
positions for simple,
undiluted samples and
enter the sample
names.
 The Autofill option or
the combination inc.
(increment) + Autofill
are very helpful for
filling in the table.
 If you want to store the samples with information of additional parameters, for example, a
predilution, special weights, filling volumes or calculation into special units, do not enter the
sample names directly into the sequence screen, but select the button Samples.
 This opens an empty

Sample ID screen in
which the individual
samples can be added
using the New function
and then stored with
individual information.
 This table can be saved
under an individual
name and reused or
edited at any time.
 Using the Samples →Sequence command, the sample data are copied into the
corresponding fields of the sequence row. Vice versa the content of the sequence can be
transferred into the sample ID page.
 Now you have created a simple sequence. Confirm it with OK.
 The sequence screen is now displayed.

2.4 Performing a flame measurement
 The measurement is started using the control

symbol beneath the menu bar.
 Starts the complete defined sequence.
 Starts only the marked lines of a sequence. This can

be single lines, connected lines or non-connected
lines. The selection is done using Windows
commands Shift or Control.
Note:
 Even with line by line measurements, the previous
measurement requires a reference value.
 Allows continuation of an interrupted measurement

sequence.
 After starting the measurement

an input box opens
automatically in which the name
of the measurement file can be
entered. If there is no user-
defined name given, the
software assigns a filename,
which is defined by the
measurement date and time.
 For better overview, the data
can be saved directly into a new
user-defined subdirectory
applying the Create new folder
function.
 If manual measurements, follow the software prompts for aspirating reference solution and
standards, etc. or let the autosampler process the started measurement sequence.
 During the measurement, the results screen fills with the measurement values and if not
otherwise set by service the following results windows are displayed,. The results windows
can be adjusted if necessary using the Options icon.

 The Bargraph screen displays
the measurement values as a
bargraph.
 Standard measurements are
displayed in green, sample
measurements in blue.
 The Spectrum display

window shows the absorption
lines of the analytes and the
simultaneously recorded
spectral environment.
 The Sample concentration in

reference curve window
displays in which range of the
calibration function the sample
was measured.

2.4.1 Results screen
 The results screen displays the overview of the measured data in chronological order.
 The data are arranged as follows
Ext /time Absorbance values, corresponding standard deviation, relative standard

deviation, measurement time and individual measurement values.
Absorbance values are given for all solutions.
Conc. 1 Concentration of the aspirated sample solution or the solution in the
measured autosampler cuo with corresponding statistics. A possible dilution
from the autosampler is already considered .
Conc. 2 Concentration relative to the original sample, considers all information on
dilutions, weights, filling volumes and output unit.
QC results Displays results for QC samples, detection limits, etc. if previously defined.
Error Optional, must be activated by service. Provides information on internal
corrections.
Single Single measurement values in absorbance.
values
Sample ID Overview of entries of sample ID, dilutions, weights, etc.

2.4.2 Verification of the measurement data
 After the measurement has been completed, the following parameters in the results screen
should be examined.
2.4.2.1 Relative standard deviation
 For absorbance values higher than 0.05 the RSD values should be below 2.0% for air-
acetylene measurements.
2.4.2.2 Spectrum
 Open the respective measurement row by double-clicking on the line.
 The displayed window shows the

single measurement values in
absorbance and the respective
time-dependent signal curves.
 Click on Display Spectrum.
 The wavelength-resolved spectrum

is displayed.
 The correction pixels are
highlighted in gray.
 Please verify whether the spectrum
of the aqueous standard looks
clean and the evaluation pixels
have been chosen correctly.

2.4.2.3 Calibration function
 To check the calibration function, either open the Calibration icon or double-click
on the Calculate calibration line on the results screen.
 The Calibration window opens.
 The first screen displays the

calibration function and the
average values of the individual
standard measurements.
 Here the type of calculation can be
directly changed (e.g., from linear
to non-linear regression) or
individual calibration points can be
deleted.
 Using Line the individual elements
can be paged through.
 The Parameter screen contains

the specific calibration data, such
as correlation coefficient,
calibration slope, method standard
deviation and the characteristic
concentration.
 For a sample determination with
good measurement accuracy a
correlation coefficient R2 of at least
0.998 should be reached.
 Under Residues the distribution of

the standard values within the
calculated confidence intervals is
displayed.
 In this graphic significant outliers
can easily be recognized.

 If you conclude that the evaluation type for one or more elements needs to be changed or if
you want to eliminate standards, a recalculation of the dataset is necessary.
2.4.2.4 Recalculation of datasets
Note:
 A recalculation of datasets is not only recommended if the calibration parameters have to
be changed, but also if the correction mode (static/dynamic) or the number of evaluation
pixels is to be changed. Prerequisite for such a recalculation is, that the analysis spectra
are saved with the dataset. Refer to chapter 2.2.2.9.
 To recalculate the data set perform the desired modifications in the calibration graph or in
the method and save the method again.
 Click on the control button under the menu bar
 The recalculation window is displayed.

 The name and memory path of the
current dataset are displayed.
 If only measurement data or calibration functions should be recalculated, it is sufficient to

calculate the data from the signals. But if evaluation parameters or correction pixels are
modified, the spectrum is needed. Therefore activate the appropriate options.
 The maximum number of lines to be calculated is already read from the dataset. If desired,
limitate the line numbers for recalculation.
 Also save the spectra together with the recalculated dataset
 If sample data, such as sample weight, filling volume or predilution have been changed,
activate the option modified sample information data.
 Enter a name for the recalculated dataset or append this to the existing one.
 Start the recalculation with OK.
 The system now recalculates the new dataset line by line.
.

2.4.3 Print-out of the measurement protocol
 The print-out of measurement reports can be performed in different manners. The following
description shows one of the possibilities.
 Open the pull-down menu File and

select Print, Report.
 In the appearing window, the

dataset to be printed can be
selected and the printer properties
accessed.
 If the results file from file is
selected, the method parameters
will be printed together with the
data.
 Under Options select data which

should be included into the report.
Confirm the selection with OK.
 Now the report can be loaded as
print preview on the screen or
directly printed.

2.4.4 Definition of a reslope measurement
 A reslope measurement is useful if the complete calibration has been measured some time
ago and the flame conditions have changed meanwhile. Applying a blank value and a
standard measurement, a slope adjustment can be performed.
 First, in the method, define the standard that should be applied as the recalibration standard.
Therfore open the Method screen Calibration, Concentrations.
Using the pull-down menu,

define the blank value and a
standard for recalibration
Note:
 Select a standard from the
upper third of the
calibration range as the
recalibration standard.
 Create a new sequence or insert the recalibration

into the sequence list
 As a simple quality control (QC) action is the measurement of a QC standard. It is

especially irecommended.for drift control. A QC standard is programmed in the same way
as a OC sample, that is described in the following passage

2.4.5 Integration of quality control samples
 Quality control samples (QC samples) are used for evaluation/test of a method and its
stability. Therefore there are samples or reference materials used whose analyte contents
are known and should be determined within specified limits. Optionally the results of such
QC samples can be stored automatically in QC/control charts.
 To define such QC samples, open the Method, QCS window.
 Click on New/Modify
and select QC-Sample
from the pull-down
menu in the Add QC-
Sample type window.
 If there is no database
for QC samples stored,
select enter manually
and confirm with OK.
 Enter a name for the

QC sample and also
enter the element
concentration and the
output unit.
 Define the accepted
tolerance range of the
results in % Deviation.
 Set a + sign under QC-Chart, as long as the measured data should be entered directly into
a QC/control chart.
 Set a + sign under Reaction, if a measured sample, that is outside of the tolerance range,
should lead to the selected reaction.

 Select the reaction from the pull-down menu
 Confirm the entries with OK and resave the method
 Now the QC sample can be defined in the sequence.

 If several QC samples or also QC standards have to be
defined, they can be selected individually from the pull-down
menu.
 QC standards can be defined in the same manner.
2.4.6 Creating control charts
 Prerequisite for creating QC charts is the definition of a QC sample, as described in chapter

2.4.5. In the Method, QCS window, the QC-Chart option must be marked with + and the
method saved.
 Open the QC icon and change to the QC-Chart-Parameters screen.
 Here the number of values of the

pre- and main period and the
design of the QC chart are
defined, as well as the number
of values recorded daily.

 Now the measurements can be
started and the QC charts are
filled with measurement values.
 The part of the chart, marked
yellow, represents the
preperiod.
Note:
 The QC chart is linked to the
method and is automatically
loaded with it.
2.4.7 Performing a standard addition/addition calibration
 An additions calibration is necessary if the sample matrix significantly influences the

sensitivity of the measurement. Therefore a direct measurement against aqueous
calibration standards is not possible.
 In this case a calibration is performed in the sample matrix itself and the sample
concentration is calculated from the slope of the received calibration function.
 There are two additions methods selectable, the standard addition method and the
additions calibration. For details please refer to the help function of the AspectCS® software
or the user manual.
 Open the Method, Calibration window. Under Calibration mode select the Method of
additions or Method of additions calibration respectively.
 The Blank Correction is preset

to Absorbance Corrected. A
more exact explanation of blank
value correction on
Concentration basis can be
found in the manual or using the
help function of the software.
 Under Std. Prep. select
manually (Preparation prep. by
sampler is optional).

 Define a new sequence by integrating the
addition calibration.
Note:
 The addition blank value is automatically set by
the software.
 Now start the measurement.

 You receive the typical calibration function of a standard addition.
 The Y-axis intercept of the calibration function is

thus shifted by the absorbance value of the
sample.
 The content of the sample is computed by the
software from the slope of the received
calibration line.

2.5 Special applications in Fl-AAS
2.5.1 Optimization of baffle ball (impact bead) and nebulizer
 An optimization of the baffle ball and nebulizer is necessary if the mixing chamber has been
removed and disassembled, for example, for cleaning purposes.
 The optimization is performed manually, i.e. without any autosampler.
!! Note:
 Always turn off the contrAA before the autosampler is removed. If the autosampler cable is
removed when the device is still turned on or the connection of the autosampler to the
device is interrupted, the electronics can be damaged.
 Before you start the optimization procedure, please make sur that the nebulizer has well
been fixed in the mixing chamber.
 Prepare a solution of 2 mg/L Cu for flame optimization.
 Open the Icon Method and

activate New/ Attach.
 Select Cu from the periodic table

and activate the primary
wavelength at 324.8 nm. Confirm
the selection with OK.

 The recommended conditions are
now loaded from the cookbook.
 Using this method, the flame
optimization can be performed.
 The capillary for manual
aspiration is used, the injection
module is not activated.
 Open the Flame window using the
corresponding icon
 Activate the Test Air function

without aspirating a liquid. The
compressed air is activated.
 Now hold the aspiration hose briefly in pure water and check if water is aspirated or if air
bubbles occur in the water container.
 For the following description of the flame optimization, a differentiation between two
possible nebulizer/spray chamber systems is necessary.
The currently shipped nebulizer /spray chamber system is built from brown or black poly
propylene sulfide and uses a plastic nebulizer. Flame optimization for this system is
described in the next chapter 2.5.1.1
 Chapter2.5.1.2 describes the optimization for the whitespray chambers (teflon with stainless
steel nebulizer) that have been shipped until 2010.

2.5.1.1 Optimization of the nebulizer for the spray chamber from PPS (shipment since
2010)
 If bubbles occur, open the fixing screw

of the nebulizer (behind nebulizer
screw (6) and turn the nebulizer screw
(6) clockwise until no more air bubbles
occur.
 Activate Test Fuel to fill the gas line
with fuel gas.
 Activate End Test to stop the gas
supply.
Note:
 It takes a few seconds to stop the gas
supply
 Ignite the flame using the Ingnite Flame.button.

 Let the flame stabilize for a few minutes.
 Change to the tab Manual

Optimization and activate Set.
For the Cu line. The spectrometer
now moves to the Cu wavelength.
 Aspirate demineralized water and
activate Start.
 The actual measurement value can
now be seen in the continuous
graph window. It should be close to
zero.
 Aspirate the Cu test solution and observe the sensitivity display.

 Optimize the nebulizer by opening the fixing screw and turning the nebulizer screw (6) until
a maximum signal is reached (also refer to User's Manual).
 Now fix the nebulizer using the fixing screw.
 Please verify the aspiration rate of the nebulizer by means of a graduated flask and a stop
watch. The aspiration rate for this spray-chamber/nebulizer system should be within 3-6mL
per minute.

2.5.1.2 Optimization of impact bead and nebulizer for the PTFE spray chamber system
(Shipment until 2010)
 If bubbles occur, open the fixing screw (6) of the

nebulizer and turn the nebulizer screw (4) counter
clockwise until no more air bubbles occur.
 Activate Test Fuel to fill the gas line with fuel gas.
 Activate End Test to stop the gas supply.
Note:
It takes a few seconds to stop the gas supply
 Ignite the flame using the Ingnite Flame.button.

 Let the flame stabilize for a few minutes.
 Change to the tab Manual

Optimization and activate Set.
For the Cu line. The spectrometer
now moves to the Cu wavelength.
 Aspirate demineralized water and
activate Start.
 The actual measurement value can
now be seen in the continuous
graph window. It should be close to
zero.
 Aspirate the Cu test solution and observe the sensitivity display.

 Now optimize the baffle ball by turning the horizontal and vertical screws on the baffle ball
holder (7) until a maximum signal in the absorbance display is obtained (also refer to User's
Manual).
 Then optimize the nebulizer. To do this, open the fixing screw (6) and turn the nebulizer
screw until a maximum signal is reached (refer to User's Manual).
 There should be a signal of at least 0.2 A for the solution of 2 ppm Cu.
 Now fix the nebulizer using the fixing screw.
 Check the aspiration rate of the nebulizer using a stop watch and a measuring cylinder. The
aspiration rate for this mixing chamber/nebulizer system should be 6–10 mL per minute.

3 Graphite furnace technique
3.1 Startup of the spectrometer for the graphite tube technique
Switching on the device
Start the PC as described in chapter 2.1. and then the contrAA 600/700.
 Start the AspectCS® software by double-clicking on the AspectCS®

icon. The Main Settings window is displayed.
 For measurements in the graphite

tfurnace technique, activate Graphite
furnace.
 The sample state for liquid samples is

already preset. Under Tube type select
whether you want to work with wall-type
tubes or platform tubes.
 Activate Initialize to establish the

connection between software, AAS
device and accessories.
 The table Available accessories shows which device

parts and accessories have been recognized by the
software
 In the Task table select Method development and

confirm with OK.

Note:
 The Routine option, in contrast to Method development, contains several limitations,
which are defined via the user hierarchies. More details on this can be found in the user
manual or the software help file. The options Data management or Options take you
directly to the basic software settings where the screen display or data storage can be
configured.
 A basic configuration has already been performed by service during device installation.
 The working screen of the

AspectCS® software is
displayed.
3.2 Creating a simple method
3.2.1 The cookbook
 For most of the elements that are determined by graphite furnace AAS the software
contains 'cookbook' values for the most important method parameters, such as matrix
modifiers, pyrolysis or atomization temperature,. When the elements to be measured are
selected, these cookbook values are automatically called up and a method is created that is
used as the starting point for further method development.
 This cookbook data can be viewed as follows:
 In the Method Development pull-down menu, open Cookbook or
click on the icon.

 The cookbook is opened and a
periodic table is displayed.
 Now select the element to be
determined.
 Under Spectrometer the cookbook

page contains information on the
recommended measurement wave-
length, alternative wavelengths and
their relative sensitivity compared
to the primary wavelength.
 Under Furnace parameters you

will find the recommended pyrolysis
and atomization temperatures,and
the recommended matrix modifier.
Under Analytical parameters
information on measurement
sensitivity is provided.
 Under Comments you will find

information onto the preparation of
standard solutions and samples,
required additives or notes on
possible interferences.

3.2.2 The Method screen
 After closing the cookbook, click on the Method icon or alternatively open the File pull-
down menu and select the New Method command.
 If a different method was already previously loaded, an additional query appears. Select
Based on default parameters.
 The empty method window appears.

 Click on Append to add elements.
 Now select one or more elements

from the periodic table that is
displayed and for each element select
the desired measurement wavelength.
 Close the periodic table with OK.
 The method window now contains the

list of selected elements.
 At the same time the furnace
parameters are loaded from the
cookbook.

3.2.2.1 The Lines tab
 The first tab, Lines has different columns with entries that can be edited if necessary.
Type (= measurement type) In graphite furnace technique only

absorption can be selected here.
Wavelength Displays the selected wavelength; can also be freely edited.
Line Line designation, is displayed automatically; can be freely edited.

Signal evaluation With graphite tube AAS, typically peak area measurement;
alternatively peak height measurement may be selected.
Test time With graphite tube AAS, typically 3-8s; can be freely edited.
Order Order of the sequential measurement of the analysis lines.
3.2.2.2 The Furnace tab
 The Furnace tab contains the graphite furnace parameters that were loaded from the
cookbook.
 The tab shows the most important parameters of the graphite furnace program, as well as
the matrix modifier to be used.

 The detailed graphite furnace program can be loaded either by double-clicking on the
appropriate line in the element list or simply marking the line and clicking on the Edit
furnace program command.
 The first column shows the name of each temperature step. This can be edited if required.
 Column 2 shows the actual temperature, column 3 shows the respective ramp rate in
°C/sec and column 4 the respective temperature hold time.
 The program includes three drying steps, in which the sample is slowly evaporated. The
internal gas flow (Purge gas) is set to a maximum, thereby ensuring a controlled transport
of the resulting water and solvent vapor out of the graphite tube..
 In a first pyrolysis step at 350°C, any remaining amounts of moisture are removed of the
graphite furnace. This generally prolongs the life-time of the graphite tube.
 In the second pyrolysis step, the sample is decomposed and interfering sample matrix is
partially evaporated. Directly before atomization, an additional program step is carried out
at a constant pyrolysis temperature. In this step the internal gas flow is stopped in order to
create good conditions for the subsequent atomization. This program step is set by the
software itself and cannot be edited.
 In the atomization step, the analyte is then evaporated at high ramp rates and high
temperature and is thus able to absorb the radiated light. This step triggers the start of the
actual absorption measurement.
 In the cleaning step, the graphite tube is finally heated-out at high temperatures in order to
eliminate any residual sample matrix and to prepare the graphite tube for the next injection.
 During the subsequent cool-down of the graphite tube, the system independently performs
a reference measurement.
 If the program was edited, you can click on the Check program button to activate a
program logic check. A green LED next to the button indicates that the program does not
contain any inconsistencies.
Note:
 The temperature program loaded from the cookbook is based on the physiochemical
properties of the analyte and follows empirical values. It offers a good starting program for
further method development, but must be further optimized based on a standard solution
and the sample to be determined.

3.2.2.3 The Sample transport tab
 The Sample transport tab is used to define the accessories installed with the contrAA.
 The graphite furnace is equipped with the autosampler MPE60. This is already activated in
the method.
 After each measurement, 2 wash cycles are preset for the autosampler capillary. This can
be changed if required.
 Under Dilution you can define whether samples whose measured absorbance values are
calculated above the calibrated range are to be diluted in the graphite tube. With this option,
the sample volume is reduced, but the total volume is kept by the addition of an appropriate
amount of blank solution. Alternatively, the volume can be reduced without the addition of a
blank.
3.2.2.4 The Evaluation tab
 The Evaluation tab contains the line-specific evaluation parameters for the calculation of
the measurement results from the spectrum.
 The specifications loaded from the cookbook offer good starting conditions for simple
applications in graphite furnsce AAS, but can be changed if necessary.

Spectr.range A maximum of 200 pixels of the CCD array can be selected for
evaluation. Considering the spectral band width per pixel this
corresponds to a spectral range of approx. 0.4 nm, depending on the
wavelength range chosen. If 200 pixels are defined for evaluation, this
entire range is displayed in the spectrum window. As not every
application requires information over the full wavelength range the
number of evaluation pixels can be reduced. However, a minimum of
approx. 100 pixels is needed, if a dynamic BGC fit has been selected
(see illustrations).
Eval.Pixels The maximum of the absorption line is expected on pixel no. 101. Since the
absorption profile is larger than the range of an evaluation pixel, adjacent
pixels can also be included for evaluation, i.e. the absorption signal is
integrated over several measurement pixels. Generally, 3 or 5 pixels are
used for evaluation in graphite tube AAS.
Note:
An increase in evaluation pixels to 5P leads to a better relative standard
deviation and to a higher measurement sensitivity.
Lowering to 3P improves the calculation of the detection limit.

(orange bar)

Background Since the atomization unit - in graphite furnace technique the graphite
correction tube itself, emits spectral light that adds to the analyte signal, a
reference measurement has to be performed before sample
measurement. In the graphite furnace program, this reference
measurement is automatically performed during the cool-down phase,
with the exception of the first replicate measurement. Alternatively, the
IBC mode can be selected here. More information on IBC can be found
in chapter 4.2. under ‘Special applications in the HR-CS-AAS‘.
Perm. Struct. The AspectCS® software contains a mathematical algorithm eliminating

permanently occurring structures, e.g. caused by O2 molecule absorption.
This may be especially advantageous, for measurements in the
wavelength range below 250nm.
For the determination of arsenic or selenium it is already preset by the
software.
BGC fit The background correction is performed simultaneously to the

measurement of the analyte from the measured spectrum. Here, along
with the absorption line, adjacent pixels are selected, which represent the
baseline. These connection pixels can be selected manually (static) or
automatically (dynamic) via the software.
With dynamic correction (default setting), a special algorithm calculates
the position of suitable correction pixels. If the correction pixels should be
manually defined, in the pull-down menu select the Static option and in
the adjacent field enter the pixel numbers to be chosen for correction.
If the special IBC application is selected, these connection options are
disabled.

Fe spectrum with dynamic Fe spectrum with static
connection connection at pixel 90 and 112
The grey bars represent the correction pixels,
which the automatic algorithm recognized as
pure baseline noise. The second Fe-line in the
spectrum is recognized as a real absorption
structure and therefore is not included for
correction.
 Before processing the next Calibration tab, it is recommended to optimize the time-
temperature program of the graphite furnace. A corresponding description can be found in
chapter 3.3.
3.2.2.5 The Calib. tab
 To program a calibration, open the Calib. tab.

Calibration modes Select the desired type of calibration. In graphite furnace AAS, for
most applications this is the Standard calibration, using aqueous
reference solutions.
Std. prep. From the pull-down menu select whether the reference solutions were
prepared manually or should be automatically diluted by the
autosampler from a standard stock solution. In this case, a defined
aliquot of the standard stock solution is pipetted into the graphite tube,
together with the volume of a diluent needed to make up the entire
volume. This usually is the blank solution.
If by variation of volume is selected, the addition of a diluent solution
is omitted.
Volumes The sample and calibration volume used for determination. The
default setting is 20µL. The sample volume can be changed if
required.
Note:
Increasing the pipetting volume will significantly lengthen the required
drying time, i.e., the time-temperature program will have to be
adjusted accordingly (see also chapter 3.3). For platform tubes the
maximum total pipetting volume is 40µL, for wall-type tubes it is 50µL.
Calib. func. Select the calculation type of the calibration function. Select between
linear, non-linear or automatic calculation. Details can be found in
the software help function.
Note:
The calculation type can be changed and the data can be recalculated
later at any time.
Intercept These parameters can be changed if required. With the basic setting,
and Weighting the intercept is calculated and the calibration data is not weighted.
Check Optional! Significant outliers can be automatically detected and

eliminated by the software. Details can be found in the software help
function.
Unit Select the unit of the calibration function In graphite furnace AAS this
generally is µg/L.
.

3.2.2.6 Definition of stock and calibration standards
 If the preparation of the standard solutions was defined by autosampler, open the Stocks
window to define the prepared stock solutions.
 An empty screen is displayed. Click on New to add stock solutions.
 In the selection box that is displayed, choose whether

the stock solution should be selected from a
previously defined database or whether the
concentrations should be entered manually.
 If Enter manually was selected, the Stock

standards screen is displayed.
 Open the Concentrations field and enter the
corresponding concentrations of the stock standard.
 The Auto Fill option is also available here for filling
the table quickly.
 Confirm the input with OK.
 Now a name and the position of the stock standard in
the autosampler can be defined on the Stock
standards screen.
 Return to the Calib. tab and then click

on Concentrations.
 A screen is displayed in which the
number of calibration blanks and
calibration standards to be measured
can be defined.

 Define the volume which is to be
pipetted from the stock solution for
each standard.
 The autosampler position is auto-
matically applied.
 Check the position of the Cal Zero
value and adjust it if necessary.
 Under Diluent position enter the
position of the Cal Zero value.
Note:
 For the calibration standards, a pipetting volume of less than 4µL is not recommended.
3.2.2.7 The Statistics tab
 On the Statistics tab select the statistical methods to be used for calibration and sample
measurement. The settings are independent of the selected calibration mode and remain
unchanged with any other change of the method.
Statistics Select the desired type of statistics. In AAS this is generally the
mean value statistics.
Confidence Select the desired option here. Details can be found in the
interval AspectCS® help function.
calc./Confidence
level

Replicates Enter the number of replicate measurements which should be
performed for each calibration standard, quality control sample or
analysis sample.
Note:
In graphite furnace AAS, generally 2–3 replicate measurements
are used. For the measurement of highly refractory elements
such as vanadium or boron, it is recommended to select a Pre-
run. Then an initial measurement is performed, but the measured
value is not used for calculation of the mean value. Thus memory
effects can be reduced.
Grubbs An outlier test is defined in the software, which can be activated

outlier test for 3 replicate measurements or more. Outliers are eliminated
and not used for the calculation of the statistics. The average
values then are marked with "!" in the output table.
3.2.2.8 The Output tab
 Under Output, some options for the automatical storage of Spectra and Methods are
already activated. It is recommended to keep these settings.
 The desired number of decimal places and the printing sequence can now be defined for
each element.

3.3 Preoptimizing the temperature-time program
 First check the drying based on an aqueous standard as well as the sensitivity of the
measurement. For this, prepare a test standard. For the optimum test concentration, refer
to the cookbook.
 To open the cookbook, open the Method Development pull-

down menu and select the Cookbook command or click on the
icon.
 If the use of a matrix modifier is recommended in the cookbook, then prepare the modifier
as described in the appendix.
 Set the matrix modifier, as specified in the method, to position 89 or change the modifier
position in the method.
 Set the test standard to any desired autosampler position.
 Now program a simple measurement sequence.
 To do so, click on the Sequence icon in the main menu or open the File pull-down menu
and select the New Sequence command.
 The empty sequence screen

is displayed.
 Select Append.

 Define the sequence of the
measurements from the list
which is displayed.
 Select samples and set the
sample number to 1.
 Confirm the selection with
OK.
 In the sequence, set the

sample position to the
position of your choice and
confirm with OK.
 The measurement is started using the control symbols

beneath the menu bar.
 Starts only the marked lines of a sequence. This can be

single lines, connected lines or non-connected lines.
The selection is done using the Windows commands
Shift or Control.
 Both starting options can be used for method development.

3.3.1 Sample drying
 The placement of the drop in the graphite tube can be observed using the furnace camera.
During the drying phase control the evaporation of the solvent.
 Now optimize the sample drying in accordance with the following points:
 The drop should spread out in the first two drying steps in the platform/on the tube wall and
slowly evaporate, without reaching boiling point. This can be achieved by optimizing the
temperatures, ramp and hold times.
Note:
 Too rapid drying will lead to condensation of water vapor in the graphite contacts and the
furnace shroud, which on further heating can lead to corrosion and thus reduces the life-
time of the graphite parts.
Step Observation Action
At the beginning of the graphite tube

program the pipetted sample drop Increase the
No
spreads in the platform or on the tube temperature by 5°C
wall
The drop ebbs down slowly without

First drying step Yes No action required
boiling
The drop immediately starts to

Reduce the
evaporate or boil and dries quickly Yes
temperature by 5°C
within the first temperature step
The drop continues to slowly

evaporate. At the end of the second No reaction
Second drying step Yes
drying step the solvent has fully necessary
evaporated
Liquid is still visible during the last 5-10

Last drying step Yes Extend the hold time
seconds

3.3.2 Pyrolysis
 The first pyrolysis step at 350°C serves to eliminate any residual water vapor from the
graphite tube before higher temperatures are reached. This step requires no further
optimization.
 The pyrolysis temperature, which is loaded from the cookbook, is the maximum
temperature for the analyte when using the specified matrix modifier. If necessary, this
specified pyrolysis temperature must be lowered significantly.
 If no matrix modifier is used, apply the maximum pyrolysis temperatures specified in the
cookbook under Remarks.
 Optimization is based on the following points:

Pyrolysis Sensitivity is too low Reduce the pyrolysis temperature, for
example, in 100°C increments
Note:
 For the measurement of real samples, the pyrolysis temperature, ramp rate and hold time
are very important. Therefore, the ramp and hold times specified by the cookbook often
have to be adjusted to the samples. However, they are sufficient for a preoptimization of the
temperature program based on a simple aqueous standard.
3.3.3 Atomization
 The atomization temperature is mainly optimized using the received signal profile. The
following points should be used for orientation:
Increase the temperature or

Signal does not return to the lengthen the hold time of the
baseline during the measurement step. In the latter case, under
time Method, Line , also increase the
Measurement time
Atomization
Signal is very narrow and sensitivity
Reduce the temperature
is too low
3.3.4 Clean out
 The clean out temperature is preset from the cookbook so that the analyte is completely
evaporated out of the graphite tube. With high analyte contents or low volatile sample
matrix it may, however, be necessary to increase this temperature.

Clean out Significant carry-over effects from Increase the temperature or
measurement to measurement lengthen the hold time of the step
Note:
 Avoid clean-out temperatures of over 2500°C
.Exception: the determination of highly refractory elements, such as V, Ti, Mo.
 After this preoptimization of the temperature program, check the precision of the
determination for three replicate measurements. Ideally, this should not exceed a value of
3% for a signal of 0.1 A*s.
3.3.5 Fine optimization of the time-temperature program
 The actual optimization of the graphite furnace method is performed using a characteristic
sample.
 Depending on the sample composition/sample matrix, the graphite furnace program has to
be modified. A high acid concentration of the sample can lead to a significantly different
drying behavior than an aqueous standard or also matrix components of the sample may
affect the volatility of the analyte.
 The aim of the method development is to eliminate the sample matrix as well as possible,
before atomization is performed, however without evaporating the analyte itself. The
automatic optimization routine therfore provides good assistance.
 For such an automated optimization, open the Furnace, Optimization screen.
 Now select the temperature step which

should be optimized and enter the
temperature limits and the step size. It is
recommended to vary the specified
pyrolysis temperature by +/- 300°C.
 Under Sampler pos. enter the position
of the test solution.
 Start the optimization by activating
Start.
Note:
 Before starting the optimization, the method should be given a name and stored.
 It is recommended to run the optimization applying a characteristic sample. If the analyte
content is very low (absorbance < 0.05),however, you should spike some standard to the
sample in order to obtain a reasonable signal value for optimization
 After completion of the optimization run, a graph is shown which displays the analyte signal
as a function of the applied temperature.

 By also selecting y-scale, the display is scaled to the received background signal.
 Using the arrow keys, the cursor can be moved and the temperature offering the best
possible conditions for the analysis can be chosen The selected temperature is applied to
the time-temperature program using Save.
 Then check measurement precision and the stability of the method. by measuring several
replicate measurements
 Now a complete graphite furnace method has been created, which contains an optimized
time-temperature program and calibration parameters. The method should be saved again
under a unique name. To do this, click on Save and enter a suitable method name. The
method can also include a remark. Close the window with OK.
Note:
 The integration of quality control samples is described in chapter 2.4.5.

3.4 Creating a measurement sequence
 In the main menu click on the Sequence icon or open File from the pull-down menu and
select the New sequence command.
 The empty sequence screen is

displayed.
 Select Append.
 In the list that is displayed,

select Calibration and confirm
with Accept.
Note:
 In graphite furnace technique a
reference measurement does
not need to be programmed. In
this technique it is auto-
matically performed by the
system.
 A typical sequence can be programmed as follows:

- Calibration
- Number of samples X
- Measurement of a spike recovery , QC sample or standard (optional)
 When the selection has been performed, e.g., the number x of samples, confirm with OK.
The selection is accepted and the window closes.
 The sequence is now displayed as follows:

 For simple, undiluted
samples complete the
missing information on
sample positions and
sample names.
 The Auto Fill option or the
combination inc.
(=increment) + Autofill help
to complete the table.
 If you like to store the samples with any corresponding information such as a predilution
factor, special weights and filling volumes or a certain sample unit do not enter the sample
name directly in the sequence screen, but use the Samples command in the window..
Alternatively you also may click on the ID samples button in the main menu.
 This opens an empty Sample ID screen. Using the New/Append function individual
samples can be added and be stored with individual information.
 This table can be saved

under an individual name
and re-used or edited at
any time.
 Using the Samples →Sequence command, the sample data is stored or updated from the
specified sequence row in the sequence. Conversely, you can also load the content of the
sequence into the sample table.
 Now you have created a simple sequence. Confirm it with OK.
 The sequence screen is now displayed.

3.5 Performing a graphite furnace measurement
 The measurement is started using the control symbols

beneath the menu bar.
 Starts only the marked lines of a sequence. This can be

single lines, connected lines or non-connected lines.
The selection is performed applying the Windows
commands Shift or Control.
 Allows an interrupted measurement sequence to be

continued.
 After the start of the measurement, an input box opens

automatically, in which the name of the measurement
file must be entered. If there is no self-defined name
given, the software will assign a filename, which is
defined by the sequence name, the measurement date
and the time of the start of measurement.
 For a better overview, the data can be saved directly in
a new self-defined subdirectory using the Create new
folder function.
 The autosampler now starts the measurement sequence. During this process, the results
screen is filled with the measurement values and the following results windows are
displayed, if not otherwise defined. Report window, spectra display, signal plot, bargraph
window and the image of the furnace camera.
 The display of the signal plot is especially important.
 If necessary the results windows can be adjusted via the Options, Analysis sequence
button.

 The Bargraph screen displays
the measurement values as a
bars
 Standard measurements are
displayed in green, sample
measurements in blue.
 The spectrum plot displays the

absorption line of the analyte and
the simultaneously recorded
spectral environment.
 The display can also be
represented as a three-
dimensional plot.
 The signal plot shows the time –

resolved atomization process. .

3.5.1 The Results screen
 The Results screen displays the overview of the measured data in chronological order.
 The result window is arranged as follows:
Abs./Time Absorbance values, the corresponding absolute standard deviation, relative

standard deviation, measurement time and individual measurement values.
Conc. 1 Concentration of the pipetted solution with the corresponding statistics. A

possible dilution performed by the autosampler is already considered as an
autosampler dilution factor (AS-VF).
Conc. 2 Concentration of the original sample, considering all information on dilutions,

weights, filling volumes and output unit.
QC Res. Displays the results for QC samples, recovery rates, detection limits etc. if
previously defined.
Error Provides information on any error messages that occurred during

measurement. (Rinse water, gas pressure error etc.)
Single val. Measured values of the individual measurement in absorbance.

Sample ID Overview on the entries for sample ID, dilutions, weights, etc.

3.5.2 Checking the measurement data
After the measurement is completed, the following parameters in the results screen should be
checked:
 Relative standard deviation
For absorbances above 0.1 the RSD values should be below 5.0%.
 Spectrum
Did you get a clear spectrum with an appropriatel selection of evaluation pixels for standard
solutions?
To check this, open the respective measurement row with a double-click on the line.
 The displayed window

shows the single
measurement values in
absorbance and the
associated time-resolved
signal plots.
 Click on Show spectrum.
 The wavelength-resolved
spectrum is displayed.
 The connection pixels are
highlighted in grey.

3.5.2.1 The Calibration function
 To check the calibration function, double-click on the Calculate calibration line on the
results screen.
 The Calibration window appears.
 The first screen displays the

calibration function and the
average values of the individual
standard measurements.
 The type of calculation can be
directly changed (e.g., from linear
to non-linear regression) or
individual calibration points can be
deleted.
 Under Line you can scroll through
the individual elements.
 The Parameters screen contains

the specific calibration data, such
as the correlation, the slope of the
calibration function, the method
standard deviation and the
characteristic concentration.
 The correlation R2 should raech at
least 0.998 to ensure a
determination with sufficient
accuracy.
 Under Residuals the distribution

of the standard values within the
calculated confidence intervals is
displayed.
 Significant outliers can be easily
recognized.
 If you find that the type of calculation of one or more elements has to be changed or you
want to eliminate standards, the dataset will have to be recalculated.

3.5.3 Performing an automatic spike recovery test (QC spike)
 Open the Method, QCS. New/Modify window
 Select QC spike and set Prepare QC

spike in tube to active.
 Select a spike volume and specify the
sequential number of the spike solution
(e.g., 5µL of the spike solution 1).
 The system will calculate the spike
concentration from your input.
 The overview field shows the calculated, expected increase.

 Now define the lower and upper limits of the tolerable range in percent. Use +/- to select
whether the result of the spike should be entered into a control chart and whether
measurements outside of the tolerance range should trigger a subsequent reaction.
Note:
 In graphite furnace technique a spike recovery rate of 90-110% is considered to be ideal
but recovery rates of 85-115% are still acceptable.
 Poorer recovery rates indicate the existence of a non-spectral interferences. This normally
cannot be corrected by repeating the measurement, but requires a standard addition
calibration to be performed (see chapter 3.5.4).
 To add the spike to the sequence, select Sequence, Append, QC samples then add the
previously defined spike (refer to the figure on the following page))
 The system always relates the measurement of the spike to the previously measured
sample and shows the result of the spike on the results screen under QC Res.

3.5.4 Programming a standard addition/additions calibration
 To program a standard addition, open

the Method, Calibration window.
 On the Calibration mode screen,
choose in between the Method of
additions and the Method of
additions calib.
 On the same screen you can define whether you want to prepare the addition standards
manually or use the automatic dilution option of the autosampler.
 The Blank correction is preset to Absorbance corrected. More information on blank
correction set to Concentration corrected can be found in the Manual or the help function
in the AspectCS® software.
 In the table, define the sample volume and the addition volume of the addition standards.

 If the preparation of the standard solutions was defined by the autosampler, open the
Stocks window to define the stock solutions to be applied.
 An empty screen is displayed. Click on New to add stock solutions.
 In the selection box that is displayed, select whether

the stock solution shouldl be selected from a previously
defined database or if the concentrations shall be
entered manually.
 If Enter manually was selected, the Stock standards

screen is displayed.
 Open the Concentrations field and enter the
corresponding concentrations of the stock standard.
 The Auto Fill option is also available here to fill the
table quickly.
 Confirm the input with OK.
 Now the position of the standard in the autosampler
and optinally a stock name can be defined in the Stock
standards window.
 Return to the Calib. tab and

then click on Concentrations.
 A screen is displayed in which
the number of addition
standards can be defined.
Note:
 The blank is not defined in this screen. It is automatically inserted in the sequence (see
flame technique, chapter 2.4.7).
 An addition calibration must be performed within the linear working range, since a non-
linear calculation is not possible. Exceeding the linear working range would result in large
measurement errors.
 Typically, 3-4 addition standards should be used.
 Now create a measurement sequence, as already described for the standard calibration.
 After calibration has been performed, the typical calibration function of an addition will be
available (see chapter 2.4.7.)

3.6 Special applications in graphite furnace AAS
3.6.1 Adjusting the Autosampler MPE 60
 To adjust the autosampler, first open the Autosampler symbol and go to the
Technical parameters screen.
 Click on the Align MPE to furnace field.
1 Adjusting screw 1
2 Lock nut
3 Adjusting screw 2
4 Adjusting aid
5 Clamp nut
6 Adjusting screw 3
7 Lock nut
 The screens that are now displayed contain an assistant function that will guide you through
the complete adjustment procedure. Carry out the following adjustment steps:
- Open the clamp-nut and push-out the dosing tube by approx. 8 mm from the canula
of the autosampler arm.
- Replace the dosing funnel in the graphite furnace by the adjusting aid with crosshair.
- Lower the autosampler arm via the software to the adjusting aid.
- Use the adjustment screws 2 or 3 as necessary to perform minor readjustment of x-
direction.
- Note:
Only adjust the x direction using the arrow keys when the autosampler capillary is
very far from the target position. In most cases, the fine adjustment described above
is sufficient.
- Adjust the y direction using adjusting screw 1.
- Readjust the x direction using adjusting screws 2 and 3.
- Check the adjustment by lowering the autosampler arm via the software. The dosing
tube must dip into the whole of the adjusting aid without any contact.
- Adjust the z direction via the software:
Lower the autosampler arm to the upper edge of the adjusting aid and then lower it
by two steps more (approx. 0.5 mm).
- The adjustments for the x and z direction are saved internally.
- Secure the positions of the adjusting screws with the lock nuts (2 and 7).
- Remove the adjusting aid and insert the funnel.

- Lower the autosampler arm via the software. The dosing tube dips into the graphite
tube.
- Loosen the clamp nut, push the dosing tube onto the tube bottom and fasten the
clamp nut.
- Move the autosampler arm via the software to the optimal dispensing depth (approx.
- 0.8 mm for a sample volume of 20 µL).
 Note:
The dispensing depth is set depending on the sample volume to be pipetted and saved in
the method. For special applications, such as the measurement of blood or serum samples,
it may be advantageous to select a lower dispensing depth, e.g., 0.3-0.5 mm, as such
medical samples tend to coat the dosing capillary with a lipid film to which the sample may
adhere..

4 Special methods and techniques in HR-CS-AAS
4.1 Background compensation
 In high-resolution AAS, background correction differs significantly from classical line-source

AAS. With line-source systems, the total and the background signal are alternately
measured and the difference between the measured values results in the specific signal.
High-resolution AAS, in contrast, applies a CCD line detector, detecting the absorption
signal and the spectral environment simultaneously and uses this information for
compensation purposes.
 Generally, in HR-CS_AAS a differentiation must be made between the compensation of
broadband background, as caused by light scattering of particles, and structured
background resulting from molecular or element absorption.
4.1.1 Compensation of broadband background absorption
 Generally, before each sample measurement, a reference measurement must be

performed. This records the absorption or emission structures of the atomization unit, which
is then subtracted from the measured sample spectrum.
 In flame technique, this reference measurement is performed at the start of the
measurement series with pure water. In all other techniques, it is part of the measurement
program and is carried out automatically by the system.
Energy spectrum of the reference measurement Energy spectrum of the sample measurement
 The illustration shows the energy distribution of the reference and sample measurement
over the 200 measurement pixels of the detector.
 In the sample spectrum, besides the energy drop on the central measurement pixel, which
is caused by the absorption of the analyte, a general energy decrease over the entire
wavelength range can be observed. This is caused by a broadband background absorption,
such as light scattering, or by a fluctuation of the lamp intensity.

 The obtained spectra are now converted
to absorption and subtracted from each
other, This results in a spectrum whose
baseline is shifted by an off-set value to
a higher absorbance. This off-set
represents the broadband background
absorption
 By selecting connection pixels (dynamic or static), the detectable baseline is set to zero.
Then, the difference between baseline and the absorption maximum is calculated, which
provides a simultaneous and automatic compensation of the broadband background.
Since especially in graphite furnace technique it is important to know whether any high
broadband background is present, the amount of broadband background is calculated from the
reference and sample spectrum and shown as a red line in the signal plot.

 Typical graphite graphit furnace
signal.
 The red line represents the
broadband background absorption,
the blue line the specific analyte
signal.
 Note:
This broadband background is calculated very roughly as the exact background absorption
value is not applied to calculate the specific signal. For this reason, the red line may show
very large differences between individual replicate measurements and a background signal
of less than 0.1A and below the baseline can therefore generally be neglected. The latter is
mainly caused by a fluctuation of the lamp intensity.
 In flame and hydride techniques, the the broadband background absorption is not displayed
in the spectrum plot..
4.1.2 Compensation of structured background absorption
 Structured background absorption is caused by molecules or matrix atoms that also absorb
within the considered spectral wavelength range.
 If there is no direct overlay of this external absorption with the actual measurement
wavelength, this has no effect on the measured value of the analyte. It is recognized by the
dynamic correction algorithm as a real spectral structure and not included into the
calculation of the baseline.
 Example: The absorption of nickel in the vicinity of the bismuth absorption line
Spectra display 3D spectrum plot
 The nickel line is clearly separated from the analysis wavelength and is recognized by the
dynamic background correction as a real absorption structure.

 For the identification of structured background absorption, the software offers a spectra
database containing the most common element and molecular bands.
 For this, open the sample spectrum and go to the Line identification screen.
 Now select the line to be identified by a mouse click. The spectra screen and the line table
now display the respective interfering element or molecule.
Note:
 If there is no direct overlay of element lines or molecular structures with the analysis
wavelength, the interference line in the spectrum is automatically corrected, i.e., it is not
included in the calculation of the baseline. A User action is not necessary.

4.1.2.1 Structured background in the graphite furnace technique
 In graphite furnace technique, yellow to orange-red bars in the signal plot indicate the
presence of structured background absorption. For such signals, check whether there is a
direct overlay of these structures with the measurement wavelength or whether they are
clearly separated from the analyte line.
 In the signal plots, the red line indicates the presence of broadband background absorption,
the yellow and orange bars indicate structured background absorption.
 In the right signal plot, an incorrect compensation is also visible. In this case, it is absolutely
necessary that the sample spectrum is checked for interferences.
 Therefore, various auxiliary tools are offered in the spectra display.
 Open the signal window of the measurement by means of a double-click on the result line
and select Spectrum. The time-averaged spectrum is shown.
Spectrum 3D spectrum plot
 While it is not directly possible to evaluate the interference in the averaged spectrum, the
three-dimensional spectrum plot indicates that the interference only occurs at the end of the
graphite furnace measurement.

 Under Plot deactivate the averaging option and you will
be able to view the development of the measurement
spectrum by spectrum and check if and when an overlay
of the spectra has occurred.
 For the identification of interfering spectra, the spectra database can be used as described
above.
 The list offers molecule and element spectra, which can be simply selected and compared
with the structures in the spectrum. In the example a direct overlay of the Zn line by NO
molecule bands is shown, caused by a high concentration of nitric acid. In a similar manner,
a high content of iron will interfere by an overlaying iron line.
 To compensate for the direct overlay of element and molecule absorption lines, it is
necessary to perform a spectrum correction. This is described in the following chapter.
4.1.3 Performing a spectrum correction
4.1.3.1 Recording the correction spectra
 First measure the individual matrix components that were found to cause the spectral
overlay.
Note:
 The concentrations of the matrix components do not have to exactly match the
concentration in the samples. However, the concentrations should be high enough to
generate clear absorbance values and, if possible, be in a similar concentration range than
in the sample.

 A precondition for a correct spectrum correction is that only one matrix component is
measured at a time as a pure substance. No contamination with the analyte itself or another
interfering components should be present.
 If no pure substances for the record of correction spectra are available, the contaminated
correction spectra will first need to be corrected with the correction spectrum of the
contaminating element itself..
 Example:
For the overlay of the zinc line by HNO3, a nitric acid solution with a higher concentration
(e.g., 5%) is measured as a sample.
 After the measurements, open the measurement line with a double-click and open the
spectrum display via the Show spectrum button.
 Save the spectrum of the matrix component as a correction spectrum by using the Corr.
spectrum button. Define a spectrum name and close the process with Save.
 Repeat these steps for each interfering matrix component.
4.1.3.2 Creating a correction model
 Now open again the measurement values and the spectrum display of the sample via the
Show spectrum button.
 Activate the Model button. Using the New/modify model option open the Spectral
corrections window. The sample spectrum is displayed.

 Open the selection of the already saved correction spectra using the Add button. Select the
correction spectrum with a mouse click and close the process with Load. Repeat the steps
for each individual correction spectrum.
 Activate the Highlight corrected spectrum button to check if the resulting sample
spectrum is free of direct overlays (refer to the figure on the following page).
 Open the window for storing the correction model using the Save button. Enter a model
name and close the process with Save.
Note:
 Using the Mask. button and holding down the left mouse button, certain ranges in the
spectrum can be masked that should not be included into the calculation of the correction
model. The range of the analyte line (pixel 92-110) is already masked by default. Masking
of more ranges can be necessary if no correction spectrum was recorded for individual
components of the sample or if additional permanent structures exist.

4.1.3.3 Integrating the correction model into the method
 Open the current method and the Evaluation tab.

 Open the associated window using the Spectral corrections button.
 Select the corresponding model in the dialog field for the analyte line and exit the window
with OK.
 After the method has been saved, the future measurements with this method will be
performed with the created correction model. Measurements already completed can also be
recalculated with this method, so that a new measurement is not necessary.

4.2 Iterative background correction (IBC)
4.2.1 General
 IBC stands for Iterative Background Correction. It was developed and patented by the
Institute for Analytical Spectroscopy (ISAS) in Berlin.
The method is similar to using a high-pass filter in electronics. Here, lower frequencies are
attenuated or eliminated completely, but high frequencies are not affected. This results in a
reduction of noise or a smoothing of the baseline.
 Using this method is advantageous
- for measurements in the lower wavelength range (<200nm)
- with the presence of strong molecule bands within the detected range
- and with broadband background absorption which is directly overlays the
measurement wavelength.
4.2.2 Examples of application of the IBC method
4.2.2.1 Noisy baseline
 A noisy baseline can be observed especially in the wavelength range below 200 nm caused
by the absorption. This complicates the selection of suitable connection pixels for baseline
correction. The IBC algorithm can be used here to obtain a smoothened baseline (refer to
the figure).
Dynamic
mode
Ideal baseline Noisy baseline

IBC
mode
The IBC mode results in a smoothened baseline

4.2.2.2 Broadband absorption by matrix components
 The IBC option is also advantageous if the broadband absorption of a matrix component is
directly overaying the analysis line and the dynamic background compensation cannot
calculate any suitable connection pixels.
 This occurs, for example, through the broadband absorption of aluminum in the wavelength
range of 193 nm. The arsenic line is located directly in the flank of aluminum absorption.
While the dynamic background compensation fails here, the IBC option results in an
evaluable spectrum.
Broadband absorption of aluminum at 193 nm:
Dynamic mode IBC mode
In this case, no connection pixels can be

In IBC mode, the baseline automatically detected
calculated for compensation

4.2.3 Programming the IBC method
 In the Method, Evaluation window, under Background correction activate the IBC
option.
 This deactivates the BGC fit column.
Notes:
 When using the IBC mode, measurement sensitivity is decreased by about 30%. However,
depending on the application, improved detection limits can be achieved.
 When using spectrum corrections, the spectrum to be corrected and the correction spectra
must be recorded with the same correction method (IBC or reference).
 It is recommended to test by means of recalculations whether or not the IBC method is
advantageous for the respective application.


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Short Instruction

for the development of analytical methods using

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 3/ 83

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 4/ 83

 The contrAA 700 contains several assemblies:

Radiation source: Xenon short arc lamp

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 5/ 83

 Start the AspectCS® software by double clicking on the AspectCS® icon.

 For measurements in the flame

 In the table system configuration all

 In the Task table select Method

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 6/ 83

 The working interface of the

2.2 Creating a simple method

2.2.1 The cookbook

 Open Cookbook in the Method Development pull-down menu or

click on the icon .

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 7/ 83

 Under Spectrometer the cookbook

 Under Flame parameters there is

 Under Remarks there is also given

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 8/ 83

 The empty Method window is

 Now select one or more

 Close the periodic table with OK.

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 9/ 83

2.2.1.1 The Lines tab

Type (= measurement type) Typically Absorption; can be changed to

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 10/ 83

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 11/ 83

- Short aspiration capillary, working manually: 8s

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 12/ 83

 Click on the Flame symbol.

 The first page control

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 13/ 83

 A query appears asking if the

 The software now starts an

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 14/ 83

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 15/ 83

Spectrum with 3 evaluation pixels (orange bar) Spectrum with 3Spectrum

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 16/ 83

Fe spectrum with dynamic Fe spectrum with static

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 17/ 83

 To program a calibration, open the Calib. tab.

Volumes Option is only visible/editable, if an autosampler with dilution option

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 18/ 83

 In the selection box that is displayed, choose whether

 If manual input was selected, the Stock standards

 Return to the Calibration list and

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 19/ 83

2.2.1.8 The Statistics tab

In AAS generally 3 - 5 repetitive measurements are used. For

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 20/ 83

2.2.1.9 The Output tab

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 21/ 83

 The empty sequence screen

 Define the sequence of the

 A typical sequence can be constructed as follows:

Short instruction contrAA® 300/600/700 | update 09.08.2011/ Po 22/ 83

 Fill out the missing

 This opens an empty

 Now you have created a simple sequence. Confirm it with OK.

 The sequence screen is now displayed.