Getting Started with the Integrated ESI prepFAST II on

the Thermo Scientific iCAP 7400 ICP-OES

Introduction The goal of this Getting Started Guide is to explain the basic steps needed to set up your prepFAST II
autodilution system inside the Thermo Scientific™ Qtegra™ ISDS software. It additionally provides a brief
overview of how to use the different features of the prepFAST II system, i.e. prescriptive and intelligent
autodilution inside a LabBook.
NOTICE The following instructions describe a configuration consisting of a Thermo Scientific iCAP™ 7400
ICP-OES with an SC-2DX prepFAST II system as an example. However, all steps can be adapted to other
DX-based autosamplers used in combination with the prepFAST II system. The installation of the prepFAST II
system is outlined in Installation of the integrated ESI prepFAST II on the Thermo Scientific iCAP 7400 ICP-OES
manual. ▲

Creating a The first step after the installation of the prepFAST II system is to create a new configuration, to define the
configuration hardware, which is used. This hardware configuration is then the basis for the creation of Templates and
LabBooks.

❖ To create a new experiment configuration

1. Open the Configurator (START > Thermo Qtegra > Configurator) and select the Experiment
configurator applet.
2. Click New to create a new experiment configuration, see Figure 1.
3. Enter a name for the new configuration, for example, iCAP 7400 and prepFAST II.

Figure 1. Creating a new experiment configuration

❖ To assign the instruments

1. Assign the instruments to the new experiment configuration by dragging & dropping them from the list of
Available Items on the right of the window to the newly created configuration on the left of the window. The
configuration should include the Thermo Scientific iCAP 7400 ICP-OES as well as the ESI autosampler
equipped with the prepFAST II system, for example, the ESI SC-2DX.

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© 2015 Thermo Fisher Scientific Inc.
All rights reserved.
 2. Right-click the autosampler entry in the new configuration and select Edit settings… (see Figure 2).

Figure 2. Selecting the menu of the autosampler

❖ To select the FAST system

1. In the Settings window, select the ESI SC-2DX tab and then the FAST Setup tab in the bottom of the
window.
2. Select the Enable prepFAST Dilution check box and choose prepFAST II from the FAST System dropdown
menu, see Figure 3.

Figure 3. Enabling and selecting the prepFAST II system

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 3. Select the Autosampler tab and Settings > Racks to set the layout of the trays, the region, type and probe
depth of the racks to reflect your autosampler rack setup, see Figure 4.

Figure 4. Selecting the rack settings

4. Click OK to close the window and then click the Save button of the Experiment configurator toolbar, see
Figure 5, to save the configuration.

Figure 5. Saving your configuration settings

NOTICE All other instrument settings of the Thermo Scientific iCAP 7400 ICP-OES and the ESI autosampler
provided inside the Experiment configurator can be adjusted according to the demands of your analysis.
However, the options Optimization and Optimization Uptake Delay should be disabled for the ESI
autosampler in combination with the prepFAST II. ▲

prepFAST: Five solutions are needed to operate the prepFAST II system, while each of them can have a different
Solution composition. These solutions are:
Preparation 1. prepFAST Carrier/Diluent
It is used to push the sample from the P7+ valve (valve 2) to the P6 valve (valve 1) using syringe 2. It is also
used to dilute the sample when it is transferred to the P6 valve using syringe 3.
2. prepFAST Internal Standard
The internal standard is added to the P7+ valve and transferred together with the diluted sample to the P6
valve using syringe 4.

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 3. prepFAST Rinse
The rinse solution is used to clean the sample loop of the P6 valve after the analysis using syringe 1.
4. Carrier
The carrier solution is needed to push the diluted sample mixed with the internal standard from the P6 valve
to the instrument. It is delivered via the instrument's peristaltic pump.
5. Rinse
This solution is used to clean the sample probe and the loop of the P7+ valve after the P6 valve has switched
to the Inject position.
All solutions should be prepared in order to meet the requirements of your analysis. For simple matrices and
analytes with a good washout behavior, the following solutions might be taken as an example.

❖ To prepare the prepFAST Carrier/Diluent solution

1. Prepare the prepFAST Carrier/Diluent solution by filling the appropriately labeled bottle with nitric acid at a
concentration that matches the matrix of your samples. Make the solution from acid and ultrapure water,
which are suitable for trace elemental analysis by ICP-OES.
2. Place the tubing labeled prepFAST Carrier/Diluent in the bottle.

❖ To prepare the prepFAST Internal Standard solution

1. Prepare the prepFAST Internal Standard solution by filling the appropriately labeled bottle with nitric acid at
a concentration that matches the matrix of your samples. Make the solution from acid and ultrapure water,
which are suitable for trace elemental analysis by ICP-OES.
2. Place the tubing labeled prepFAST Internal Standard in the bottle.
3. Keep in mind that the internal standard is also diluted by a factor of 6, if the FAST methods are used, which
were provided with the instrument, see Table 1.
NOTICE For the Operational Qualification no internal standard solution is needed. Use the prepFAST
Carrier/Diluent solution for this procedure. ▲

❖ To prepare the prepFAST Rinse solution

1. Prepare the prepFAST Rinse solution by filling the appropriately labeled bottle with nitric acid at a
concentration that matches the matrix of your samples. Make the solution from acid and ultrapure water,
which are suitable for trace elemental analysis by ICP-OES.
2. Place the tubing labeled prepFAST Rinse in the bottle.
3. In this case, also the prepFAST Carrier/Diluent solution can be used.

❖ To prepare the Carrier solution

1. Prepare the Carrier solution by filling the appropriately labeled bottle with nitric acid at a concentration that
matches the matrix of your samples. Make the solution from acid and ultrapure water, which are suitable for
trace elemental analysis by ICP-OES.
2. Place the bottle with the Carrier solution in the FAST bottle holder.
3. In case of the Carrier, also the prepFAST Carrier/Diluent solution can be used.

❖ To prepare the Rinse solution

1. Prepare the Rinse solution by filling the appropriately labeled bottle with nitric acid at a concentration that
matches the matrix of your samples. Make the solution from acid and ultrapure water, which are suitable for
trace elemental analysis by ICP-OES.
2. Place both tubings labeled Rinse (1+2) into the bottle. Note that two different solutions can be used to rinse
the probe and the sample lines.

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 3. In this case, also the prepFAST Carrier/Diluent solution can be used.

Table 1. Exemplary solution flow rates during autodilution procedure

Internal
Sample Flow Diluent Flow Diluent + Sample Standard Flow Loop Fill Total
(μL/min) (μL/min) Flow (μL/min) (μL/min) Flow (μL/min)
1× (Undiluted) 10000 0 10000 2000 12000
2× Dilution 5000 5000 10000 2000 12000
20× Dilution 500 9500 10000 2000 12000
200× Dilution 50 9950 10000 2000 12000

Preparing the It is recommended to prime the complete prepFAST II system before first use in order to remove air bubbles
System for from the sample lines and the syringes. This ensures reproducible results as well as a good washout behavior.
the First Use ❖ To run the priming procedure
1. Start Qtegra ISDS and load the prepFAST II configuration created in “Creating a configuration” on page 1.
2. From the Dashboard, open the autosampler display by clicking the headline, see Figure 6.

Figure 6. Opening the autosampler view

3. If the autosampler does not already display Connected and Initialized in the Dashboard (see Figure 7), select
Tools > Initialize. If the autosampler is connected properly and all drivers are installed, the state should
change after a couple of seconds. Otherwise, please power cycle the complete autosampler and the
prepFAST II system, reload the Qtegra configuration and try again.

Figure 7. Connection status of the autosampler

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 4. The autosampler probe should be located at the Home Position above the first rinse station. If this is not the
case, select Tools > Calibrate. A wizard will guide you through the calibration procedure. If the rinse station
position was not located correctly upon initialization and calibration was required, it is recommended to
check if the vial positions are located correctly. This can be checked using the same calibration procedure.
Alternatively, this step can be repeated if the autosampler does not go into the vials properly during the
acquisition of a LabBook.

❖ To prime the rinse station

1. In order to initially prime the rinse station with rinse solution, select Settings > Rinse to open the Rinse
control window (see Figure 9).
2. Turn on both rinse pumps by clicking On for both pumps. As soon as you see that there is solution at the top
of the rinse station(s), switch the pumps Off again.
3. When the Rinse solution matrix is changed, this procedure should be repeated in order to flush the tubings
off the previous Rinse solution.

Figure 8. Settings menu and rinse pump switches of the autosampler

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 ❖ To select the FAST method
1. On the Dashboard, select the FAST Method tab in the lower ribbon and, from the New user method from
a template, select the supplied prepFAST2_Prime.fast from the Browse for FAST Methods dialog, see
Figure 9.

Figure 9. Selecting the prepFAST II method

2. The selected method is shown on the Dashboard, see Figure 10.

Figure 10. Selected prepFAST II method on the Dashboard with dropdown menu of the Save button

3. To save the selected prepFAST II method, click the Save button. Select Save As from the dropdown menu.
The method is saved as a user method.

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 4. On the Dashboard, select the FAST Method tab in the lower ribbon and, from the Open a user method,
select the supplied prepFAST2_Prime.fast from the Browse for FAST Methods dialog, see Figure 11.

Figure 11. Opening a user method

The method is shown on the Dashboard page.

❖ To start the prepFAST II method

1. Click the green Play button to start the method, see Figure 12.
2. Repeat this prepFAST II method triggering until all syringes are filled completely with solution.
3. This procedure will have to be repeated each time the composition of the prepFAST Carrier/Diluent, the
prepFAST Internal Standard or the prepFAST Rinse solutions are changed.
4. Once the rinse stations and all syringes are filled the prepFAST II system is ready for use.

Figure 12. Play button to start the method

Get Ready As the prepFAST II-based system is a discrete sample introduction system that provides steady signals over a
Operation fixed time period, the Get Ready process for the prepFAST II is different to that for a continuous sample
introduction system such as a traditional autosampler.

❖ To use Get Ready

1. From the Qtegra ISDS Dashboard, click the Get Ready button, which opens a dialog for the startup of the
instrument, see Figure 13.

Figure 13. Get Ready button

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 2. Enter the Warm up time (if required), the Wash time and the Uptake time (for the supplied tubing, 30 s
should be sufficient) you want to use for the analysis, see Figure 14.
3. Select Spectrometer Optimization or Nebulizer Optimization if you want them to be performed
automatically after the Warm Up.
4. Select the Use Manual Sampling checkbox as Performance Checks conducted by the software require a
stable signal, which is longer than the one the prepFAST II system can provide.

Figure 14. Get Ready dialog

❖ To run the Get Ready process

1. Make sure that the prepFAST II sample out line is connected to the nebulizer and that all waste tubings are
fitted to an appropriate waste bottle.
2. Make sure that the carrier and the spray chamber drain pump tubing are aligned correctly on the peristaltic
pump.
3. Click OK.
4. The plasma will be started and, after any defined warm up time and optimization procedures, the
performance checks will be acquired. During these actions, you will be asked to provide the corresponding
solutions for each step, see Figure 15. Use the carrier tubing, which goes from the peristaltic pump through
the first prepFAST II valve into the iCAP 7400 ICP-OES to supply these solutions.

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 5. Once the performance checks are finished, the state of the instrument should be Ready and the analysis can
be started.

Figure 15. Getting Ready process

Performing Since Qtegra 2.4 SP2 the following options are fully supported:
an Analysis • Prescriptive dilution
using the • Intelligent dilution for an analyte above the calibration range
prepFAST II • Intelligent dilution when one or more of the internal standards show an unacceptable recovery due to matrix
System effects

General adjustments
After you have created a LabBook based on the configuration including the prepFAST II system, the
corresponding tabs will be shown inside the menu of the LabBook, see Figure 16. All parameters of the
autosampler can be set using these tabs.

Figure 16. Menu of ESI SC-2DX inside the LabBook

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 One of the most important settings is the definition of the rack sizes and the probe depth. To change them, go to
Method Settings >Racks and adjust them according to the configuration of the ESI autosampler using the
dropdown menu, see Figure 17.

Figure 17. Settings menu of the Methods Settings window

The Analysis tab is used to define the Uptake Time as well as the Wash Time. As the dilution procedure is part
of the Uptake time, typically 25-35 s are needed to get a stable signal. The Wash Time can be set to a smaller
value as it is already part of the FAST method (4-10 s are recommended) and needed in order to make sure the
autosampler is ready to start with the aspiration of the next sample. If the displayed window does not look like
the one shown in Figure 18, the reason is that no prepFAST II method has been selected. As soon as this is done,
the window will change accordingly.

Figure 18. Sample settings in the Methods Settings window

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 The FAST Methods tab allows setting for the selection of the method used for the analysis. If you click it, you
can either load the methods supplied with the system or ones you have created. The browser can be opened by
clicking the Browse button, see Figure 19.

Figure 19. Opening a FAST Method from the FAST Methods tab

NOTICE Different FAST methods are supplied with the system for the different available sample loop volumes.
Please make sure that the duration of the acquisition corresponds to the flow rate of the sample introduction, i.e.,
the speed of the peristaltic pump, and the volume of the FAST loop to ensure a stable signal during the
acquisition. Please also make sure that the chosen method matches the configuration of your system. For further
information regarding the setup of a method, please refer to the Qtegra for iCAP 7000 Series ICP-OES
Software-Manual. ▲

Prescriptive dilution
Prescriptive dilutions can be used whenever it is known that a dilution is needed prior to the analysis. This can
either be the case for samples, which are known to have a high concentration of analytes or high matrix content
or to generate calibration curves from one or more stock solutions.
The prepFAST II system is able to dilute the sample up to a factor of 400, whereas the internal standard is
additionally added to all samples. In any configuration including a prepFAST II system, the prepFAST dilution
factor (DF) can be adjusted inside the Sample List of a LabBook, see Figure 20.
In order to correct for dilutions done prior to placing the sample in the autosampler, the Dilution Factor is used.
The Total Dilution Factor is the product of the prepFAST DF and the adjustable Dilution Factor.

Figure 20. prepFAST Dilution Factor inside the Sample List of a LabBook

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 Intelligent dilution
The intelligent dilution can be adjusted by opening the corresponding tab in the LabBook, see Figure 21.

Figure 21. Opening the Intelligent Dilution tab

You have the possibility to activate an automated dilution in case the internal standard does not meet the set
criteria or an automated dilution in case the concentration of an analyte is not within the calibration range, see
Figure 22.
For the Internal Standard an Upper and a Lower Limit can be defined, between which the recovery of the
internal standard has to lie. If the recovery rate of any internal standard within the LabBook does not meet this
criterion, the sample will be diluted according to the set Autodilution Factor, e.g. 10. If the recovery of at least
one internal standard is still not within the defined limits, the prepFAST II system will try to dilute it further,
e.g. by a factor of 20, until the Maximum Number of Autodilutions has been reached. In this case, the action
defined by the Action on Failure dropdown menu will be performed.
For the Calibration Range a Limit can be set. If at least one of the investigated analytes shows a concentration
above this limit, the sample will be autodiluted. This value is the percentage of the highest calibration standard
(STD sample) for any measured analyte. If for example, the highest calibration point is 1 ppm and the limit was
set to 120%, each sample with an analyte concentration above 1.2 ppm will be autodiluted to the Target value. If
more than one analyte is out of the calibration range, the highest dilution factor will be applied automatically.
This value is again a percentage of the highest calibration point. With the aforementioned example this would
mean that the 1.2 ppm sample is diluted by a factor of 2 to achieve a concentration of 0.6 ppm (60% of the
highest calibration point).

Figure 22. Enabling the Autodilution for Internal Standard and Calibration Range

NOTICE Both checks apply to all internal standards or all measured wavelengths, respectively. There is no
possibility to exclude designated sample analyses within a LabBook from these checks. ▲
If a sample line was added into the LabBook’s Sample List by the prepFAST II system, it will be
marked with a plus to indicate that this sample line was automatically added during the runtime of
the LabBook.

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 You also have the possibility to review the results of the prepFAST II Intelligent Dilution Checks by opening the
Comments inside Evaluation Results > Concentration after the analysis. An example is shown in Figure 23.

Figure 23. Results view of autodiluted sample line

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