Setup the Sequence and QCs

The Sequence page of the worksheet is where you:

Some features on the Sequence tab will only be available while in the ICP Expert view and some are available in both the ICP Expert and ICP Applet view.

Some features are only available when using ICP Expert Pro and are indicated below.

Setup Recurring Standard Recalibrations

Use to setup a recurring interval to recalibrate standards. This is not available if 'Enable reslope' is selected on the Standards page.

Click Standards.
Setup all calibration standards.
Click Sequence.
Select Calibrate every (samples) to enable the recalibration feature in the software.
Enter the recalibration rate.

The standards populate at the specified interval in the Sequence table.

Setup a Calibration Curve Reslope Rate

Reslope your calibration curve using a subset of standards. Appears only if 'Enable reslope' is selected on the Standards page.

Click Standards.
Setup all calibration standards.
Select Enable Reslope.
All standards to reslope with are selected by default. Deselect the standards that will not be used during calibration curve reslope.
Click Sequence.
Select Reslope rate.
Enter the number of solutions that can be run before a reslope is performed.

The reslope standards populate at the specified interval in the Sequence table.

Enable and Configure Displayed Sample Information

Setup and configure which information is displayed in the Sequence table and in the report.

Click Sequence.
Click Enable sample information.
Click Columns above the Sequence table.
Select or deselect the available options to customize the Sequence table display.
Click in the relevant cell under the column for each sample and then enter the required information.

Label

Description

Notes

Solution Label

Assign a unique name to each solution in the Solution Label column. This Label will be used in the Analysis page to identify the solution.

QC solution names are edited on the QC page.

Solution Type

Assign the solution as either a sample or as one of the previously set up QC solutions. If you assign it as a QC solution the solution label will be changed to reflect the QC label created in the QC page.

There is a recommended order for QC tests.

QC solutions added this way are considered non-rate driven. They occur only in the selected position and are not automatically repeated.

QC solutions can also be added to the sequence by right clicking on a row and using the ‘Insert solution below’ option. Select the required solution from the list. Once a new sample or QC solution is inserted, if needed you can select a different QC type and edit the Solution label (on inserted samples only). QC solutions and samples can be deleted by right-clicking on selected solutions and then selecting 'Delete Selected Solutions'.

Because you can only add a sample related QC solution after a sample or another sample related QC solution, the drop-down list may be filtered, depending on where you are in the sequence.

Dilution List

Enter the Dilution List name to enable reactive dilutions for a specified list of wavelengths. The Dilution List must be entered for each solution.

Dilution List are created on the Elements page after enabling the ADS 2 or PrepFAST on the Configuration page.

Measurement Selection

The drop-down menus in this column display the repeated measurements that have been generated for each solution that required dilution.

Double-click in the column to view the repeated measurements and then select the desired iteration, if required.

Weight/Volume/Dilution

Enter any factors used to create the solution. These factors will be used to calculate the final concentration shown on the Analysis page.

Autodilution

To use prescriptive dilution values, enter a dilution value that will be used for each sample or QC solution.

A dash "-" in an Autodilution cell means that no autodilution will be applied to that solution. To remove an entered value, type -, 1, or 0 in the cell.

This column appears when ADS 2 or ESI PrepFAST is selected in the Autosampler drop-down menu on the Configuration page. The 'Autodilution' field is available for all solution types that accept a prescriptive dilution value.

If reactive dilution is used instead of prescriptive dilution, ICP Expert will enter the dilution factor for all solutions requiring reactive dilution into this column.

Rinse

Available only with the Agilent SPS 4 autosampler with dual rinse mode enabled. Specify the rinse port to use for each sample or solution. Method (x), where x is the method rinse position selected on the Conditions page, is the default position. To customize rinse positions for each sample or solution, select from rinse port 1 or 2 or a combination of both. Rinse 1+2 will use both rinse ports, starting with rinse port 1. Rinse 2+1 starts with rinse port 2 and then rinse port 1.

MDD (g/day)

MDD is the maximum daily dose for the specific drug preparation being analyzed and is defined by USP <232> and ICH Q3D guidelines.

This appears only when Expanded QC is enabled in the Configuration tab.

Sample Type

For expanded QC, select the QC sample(s) created on the File > Expanded QC page. When USP <232/233> and ICH Q3D enabled, select the route of administration of drug products or LSpikes from the drop-down list. It is important to note that the MDD changes based on how the drug is administered.

This appears only when Expanded QC is enabled in the Configuration tab.

This is not an editable field. The hover tip displays the expected concentration in µg/L of each element in the sample at 1.00 x J.

J is the concentration (w/w) of the elements of interest at the target limit, appropriately diluted to the working range of the instrument.

This appears only when Expanded QC is enabled in the Configuration tab and if a PDE (permissible daily exposure) sample type (Oral, Parenteral, or Inhalation) is selected.

LIMS ID, Customer, Customer Ref., Sample Site, Sample Date, Description

All of these are additional sample information fields that can be used to customize sample information. They can be exported into the report if selected in Options > Export Preferences.

Displays a unique solution ID when CFR mode is enabled.

QC Tests

This section describes individual actions that can be performed on the Sequence page to add QC solutions to the sequence. For a full description of how to add QCs to a sequence click here and view the video.

To access the rate driven QC feature and this table, you must have the ICP Expert Pro Feature Pack installed. Otherwise, all QC solutions are non-rate driven.

Subtract preparation blank from samples and sample QCs

Select to subtract the results of the preparation blank from the samples and sample related QC tests. This will only appear if Preparation Blank is selected from the QC test list.

Adding QC tests to the sequence

Select, drag and drop single or multiple QC solutions from the QC Solutions table onto the Sequence table to add a QC solution or block. If it is a rate driven QC block, the automatically calculated rate (how often the block is inserted into the rest of the sequence) is equal to the number of samples preceding the original inserted QC block.

Inserted blocks will automatically appear as a single line until expanded by clicking the + to the left of the line.

To insert multiple tests in one block press CTRL and select all required tests. Drag the block into the appropriate location in the Sequence table.

The Rate QC preferences dialog appears the first time any QC solution is dragged into the Sequence table. Alternatively, to access this dialog box, right-click on the inserted QC solution and then select Rate QC preferences.

The QC solutions listed in this table are selected on the QC tab.

Count as sample when manually inserted

Select to include these solutions as samples when they are not inserted as a rate driven QC test. The ICP Expert software calculates the number of samples between rate driven blocks.

It is important to note that once results are collected, all 'Count as sample' check boxes become read-only. The only exception to this is when there are IEC only results collected (IEC standards, etc.) such as when creating a template with IEC factors and QC enabled.

Tell me more about Rate Driven QC.

Enable reactive dilution

Select to enable reactive dilution for each QC type.

Count reactive dilutions as samples

Select to count reactive dilutions as samples. This only applies to QCs with 'Count as sample when manually inserted' is also selected.

Adding or changing a non-rate driven QC solution or block

Non-rate driven QC solutions can be added or changed by selecting the solution from the drop-down menu on the Solution Type column, added via the right-click context menu or dragged and dropped (function only available with ICP Expert Pro) from the QC solutions table onto the Sequence table the Sequence page.

Because you can only add a sample related QC solution after a sample or another sample related QC solution, the drop-down list may be filtered, depending on where you are in the sequence.

Deleting a non-rate driven QC solution

Select and then right-click the QC solution(s) then select Delete Selected Solutions in the context menu or select the desired solution and then press Delete on the keyboard.

Adding a rate driven QC solution or block

Rate driven solutions or blocks can be added via the right-click context menu or dragged and dropped after a sample or another rate driven block on the Sequence page. A summary row with + on the left side will indicate the block is rate driven.

Adding or deleting QC solutions in a rate driven QC block

To add or change QC solutions in a rate driven QC block, right-click any of the tests in the block or the solution to open the Rate QC Parameters dialog box and then insert via the drop-down menu or delete the required solutions by clicking the red X .

Deleting a rate driven QC solution or block

Right-click the test (or press CTRL and then select multiple tests and then right-click) and then select Delete selected solutions for all occurrences. This will delete all occurrences of the rate driven test or block.

Edit Rate QC Preferences

This dialog box only appears if the ICP Expert Pro Feature Pack is installed.

This dialog automatically appears the first time any QC solution is dragged into the Sequence table. Alternatively, access this dialog box by right-clicking on the inserted QC solution.

Select where you would like the QC solution inserted:
- After 'Sample x' - where 'Sample x' is the selected solution label. This is automatically populated and selected if it is a non-rate driven solution or block.
- Number of samples between QC tests - the number of samples to be run between QC solutions. This is automatically populated and selected if it is a rate driven solution or block. Editing this value will change where the rate driven solution or block appears in the Sequence table.
- Insert after calibrations - QC solutions inserted at the end of every calibration.
Select the error action to occur for the selected QC solution or block. Changing error actions for that solution or block will only apply to that QC solution or block. Other QC solutions or blocks added, even those that include the same solution(s), will have their own error action and will not be affected by changes to that solution or block.
Select the test and then use the arrows to rearrange the order in which the tests will be performed.

Deleting tests

Select the rate driven QC solution and then the red X .

Edit the Rack and Tube Locations

Shows the current location of the sample in the autosampler rack. This is not visible if the sample introduction is set to Manual.

Click the Rack:Tube cell and select the values from the drop-down menus to change the position of the tube.
To automatically change the layout of the subsequent samples, select ‘auto increment down’ to reassign the rack tube location of the subsequent samples.

Lock Autosampler Rack:Tube Positions

Adding or removing solutions from the sequence table can change the rack location of the remaining solutions. To prevent this, you can lock the Rack:Tube solution location so that it remains in the same position regardless of other sequence changes.

To lock the autosampler tube position you can either:

Click the Rack:Tube cell and then click the open lock icon (or closed lock icon if you are unlocking a cell).
Highlight a cell or group of cells and then right-click them. Select 'Lock solution position' or 'Unlock solution position' if you want to unlock a Rack:Tube position.

Setup Start of Run Actions

If you are using an ADS 2, select ADS 2 flush cycles and then enter the number of syringe flush cycles required before analysis starts.

Setup End of Run Actions

Select the end of run actions for the instrument to perform after finishing the analysis.

Option	Action
Set pump speed	Set a low pump speed to conserve rinse solution at the end of a run.
Turn plasma and pump off	Choose this to turn off the plasma and peristaltic pump at the end of a run.
Turn plasma off and reduce pump speed	Choose this to make the plasma turn off at the end of a run, and have the peristaltic pump slow down to 1 rpm. This helps to prevent tubing wear. Once the plasma is turned off, the autosampler will raise its probe and no solution will run through the system. In Manual mode, since the peristaltic pump is turning slowly, the last solution will slowly go through the system.
Disable polychromator boost purge after run	Select to turn off the polychromator boost purge at the end of the run. Typically used when analyzing UV wavelengths below 189 nm.
Disable snout purge after run	Select turn off the snout purge at the end of the run. Typically used when analyzing UV wavelengths below 189 nm.
Rinse system	Continue pumping rinse solution for the specified time at the end of a run. This is in addition to any allocated method rinse times.
Park autosampler	Moves the autosampler probe to the Park position at the end of the run.
End of run rinse port	Available when using the Agilent SPS 4 autosampler with Dual Rinse selected in File > Options > General. Select the rinse port(s) to use for the end of run rinse when 'Rinse system' is selected.