ICP-MS Operation Procedure - users.4dlabs.ca · solution pushes the sample out of the sample loop...

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ICP-MS Operation Procedure

Standard Operating Procedure

4D Labs Confidential

Revision: 1.0 — Last Updated: October 24, 2016

Revision History

# Revised by: Date Modification

1.0 Philip Kubik 2016/10/24 Original version.

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Table of Contents

1 Purpose ........................................................................................................................................... 6

2 Definitions ....................................................................................................................................... 6

3 Conventions .................................................................................................................................... 7

4 References ....................................................................................................................................... 7

5 Contact ........................................................................................................................................... 8

6 Instrument Overview ........................................................................................................................ 8

6.1 iCAP Q ..................................................................................................................................... 8

6.2 Autosampler ............................................................................................................................. 8

6.3 Software ................................................................................................................................. 10

6.3.1 Instrument Control & Qtegra ........................................................................................... 10

6.3.2 Auxiliary Computer .......................................................................................................... 10

7 Measurement Overview ................................................................................................................. 11

7.1 Manual Sampling versus Autosampling ................................................................................... 11

7.2 Measurement Recipes ............................................................................................................. 11

7.2.1 LabBooks ........................................................................................................................ 11

7.2.2 Templates ....................................................................................................................... 12

7.2.3 Evaluation Methods......................................................................................................... 12

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7.3 Measurement Modes .............................................................................................................. 13

7.4 Quantification ......................................................................................................................... 14

7.4.1 Why are Standards Needed for Quantification? ................................................................ 14

7.4.2 External Standards .......................................................................................................... 15

7.4.3 Internal Standards ........................................................................................................... 16

7.4.4 Isotopic Standards ........................................................................................................... 17

7.5 Quality Control ....................................................................................................................... 17

7.6 Analytical Methods ................................................................................................................. 18

7.6.1 External Standardization .................................................................................................. 18

7.6.2 Standard Additions .......................................................................................................... 18

7.6.3 Isotope Dilution ............................................................................................................... 18

7.6.4 Isotope Ratios ................................................................................................................. 19

7.6.4.1 Measurement Parameters ........................................................................................ 19

7.6.4.2 Corrections .............................................................................................................. 19

7.6.5 Standard Additions .......................................................................................................... 21

8 Sample Preparation ........................................................................................................................ 21

9 ICP-MS Operation Procedure .......................................................................................................... 22

9.1 Personal Protective Equipment ................................................................................................ 22

9.2 Log-in ..................................................................................................................................... 23

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9.3 Plasma Ignition ....................................................................................................................... 23

9.4 Performance Report ................................................................................................................ 28

9.5 Autotuning ............................................................................................................................. 30

9.5.1 Tuning Methods .............................................................................................................. 30

9.5.2 Source Autotune ............................................................................................................. 31

9.5.3 Other Autotune Routines ................................................................................................. 32

9.5.4 Mass Calibration ............................................................................................................. 33

9.6 Measurements ........................................................................................................................ 34

9.6.1 Create a LabBook ............................................................................................................ 34

9.6.2 Method Parameters ......................................................................................................... 36

9.6.2.1 Analytes .................................................................................................................. 36

9.6.2.2 Acquisition Parameters ............................................................................................ 37

9.6.2.3 Monitor Analytes ..................................................................................................... 40

9.6.2.4 Survey Scan Settings ................................................................................................ 41

9.6.2.5 Interference Correction ............................................................................................ 43

9.6.2.6 Standards ................................................................................................................ 45

9.6.2.7 Quantification .......................................................................................................... 48

9.6.2.8 Regions ................................................................................................................... 51

9.6.2.9 Ratios ...................................................................................................................... 51

9.6.3 Sample Introduction ........................................................................................................ 52

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9.6.3.1 Manual Sampling..................................................................................................... 52

9.6.3.2 Autosampler ............................................................................................................ 53

9.6.4 Sample List ..................................................................................................................... 58

9.6.5 Running a LabBook ......................................................................................................... 60

9.6.5.1 Autosampler ............................................................................................................ 60

9.6.5.2 Manual Sampling..................................................................................................... 64

9.7 Wrapping Up Measurements ................................................................................................... 64

9.8 Evaluation Results ................................................................................................................... 65

9.8.1 Intensities, Concentrations, and Ratios ............................................................................ 65

9.8.2 Surveys ........................................................................................................................... 66

9.8.3 Spectra View ................................................................................................................... 66

9.9 Reports ................................................................................................................................... 66

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1 Purpose

This document describes the procedure for operating the 4D Labs ThermoScientific iCAP Q Inductively Cou-

pled Plasma Mass Spectrometer (ICP-MS) with aqueous liquid sample introduction. The laser ablation

module is not included. This procedure is intended to be a reference for users of the 4D Labs Nanofabrica-

tion Facility and is not a substitute for training by the tool owner. Users of the ICP-MS are expected to have

independent knowledge of chemical safety and the techniques of ICP-MS and analytical chemistry. Apart

from a few guidelines, sample preparation is outside the scope of this document.

2 Definitions

Carrier: A rinse solution, which is used to flush the system between samples.

CCT: Collision Cell Technology, which refers to the collision/reaction cell.

CRM: Certified Reference Material

c/s: counts per second

DIW: Deionized Water.1

ICP-MS: Inductively Coupled Mass Plasma Mass Spectrometer.

IR: Isotope Ratio

LA: Laser Ablation.

LabBook: Initially, a recipe in Qtegra for a series of mass spectra measurements. As the recipe is run, data

are added to the LabBook.

Measurement: In this document, a measurement corresponds to a row in the Sample List of a Qtegra Lab-

Book.

QC: Quality Control

Q-cell: Collision/reaction cell between the QID and quadrupole detector.

QID: Quadrupole ion deflector. Downstream from the cones.

Qtegra: ThermoScientific ICP-MS software.

1 Deionized water should have a resistivity ≥ 18.1 MΩ-cm. Distilled water has a lower resistivity, typically ~ 1 – 3 MΩ-cm.

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Semi-quantification: An approximate calibration method which may be used when there is no standard

corresponding to an analyte. Concentrations of selected analytes are plotted as a function of mass. Provid-

ed that the mass of the unknown analyte lies between the masses of two analytes selected for the semi-

quantification curve, its concentration may be estimated.

SRM: Standard Reference Material

TDS: Total Dissolved Solids

3 Conventions

In this document, the following items are italicized.

Hardware units

Software menu items

Software windows and panels

Software box names

The following items are underlined.

Hardware buttons and switches

Software buttons

Software checkboxes.

Special keyboard keys, e.g., Enter.

Text to be typed is shown inside double quotation marks.

Hazard conventions:

CAUTION indicates a hazard which may cause damage to equipment.

WARNING indicates a hazard which may cause injury to personnel. It may cause damage to equipment

as well.

4 References

Elemental Scientific, FAST Method Guide - iCAP Q, Document M-FMG-73.

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Thermo Fisher Scientific, Qtegra for iCAP Q ICP-MS Software Manual Qtegra 2.6, Document no.

1288010, Rev. J (September 2015).

Thermo Fisher Scientific, iCAP Q Operating Manual, Document no. 1288090, Rev. C (August 2013)

Paul R. Gaines, ICP Operations Guide: A Guide for using ICP-OES and ICP-MS, Inorganic Ventures

(2011). https://www.inorganicventures.com/icp-operations-guide

Paul R. Gaines, Sample Preparation, Inorganic Ventures. https://www.inorganicventures.com/sample-

preparation

Paul R. Gaines, Trace Analysis Guide, Inorganic Ventures. https://www.inorganicventures.com/trace-

analysis-guide

Additional reference material is available in the Training and Reference folders on the ICP-MS computers.

5 Contact

Questions or comments concerning this document or operation of the system should be directed to the cur-

rent tool owner at 4D Labs Nanofabrication Facility, Simon Fraser University, Burnaby, BC, Canada. The

current tool owner is listed on the web page for the tool on the 4D Labs Nanofabrication Facility web site.

6 Instrument Overview

6.1 iCAP Q

For a description of the iCAP Q hardware, refer to Chapter 3 of the CAP Q Operating Manual. 2

6.2 Autosampler

The autosampler FAST valve has two operating states: Load (Figure 6-1) and Inject (Figure 6-2).

2 Thermo Fisher Scientific, iCAP Q Operating Manual, Document no. 1288090, Rev. C (August 2013).

https://www.inorganicventures.com/icp-operations-guide

https://www.inorganicventures.com/sample-preparation


https://www.inorganicventures.com/trace-analysis-guide


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Figure 6-1: FAST valve configured to load loop and rinse nebulizer.

In Load mode, the autosampler probe moves into the sample vial and sample is sucked into the sample

loop by a vacuum pump while the carrier and internal standard solutions are pumped into the nebulizer by

the peristaltic pump.

Figure 6-2: FAST valve configured to rinse the autosampler probe and inject the sample into the nebulizer.

In Inject mode, the autosampler probe moves into the autosampler rinse solution. Suction from the vacuum

pump flushes the autosampler probe with the rinse solution. Meanwhile, one end of the sample loop is

connected to the nebulizer and the other to the carrier solution through the peristaltic pump. The carrier

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solution pushes the sample out of the sample loop into the nebulizer and then rinses the sample loop.

Simultaneously, the internal standard is also pumped into the nebulizer by the peristaltic pump.

6.3 Software

6.3.1 Instrument Control & Qtegra

The ThermoScientific software for the operation of the iCAP Q ICP-MS is called Qtegra. It has two compo-

nents:

Instrument Control

Qtegra

Note that there may be some confusion because the name of one of the components is the same as that of

the two components together. In this document, Qtegra means the component, unless otherwise noted.

Instrument Control should be used to ignite the plasma, run performance tests, and tune the system. Qte-

gra must be used to acquire mass spectra. Qtegra may also be used to ignite the plasma, run performance

tests, and tune the system but for those applications it is not as versatile and gives less information than

Instrument Control. Consequently, the latter is preferred for those applications and those features of Qte-

gra are not discussed in this procedure.

Mass spectra are measured and the results are displayed in a LabBook in Qtegra. Initially, a LabBook is

essentially a complete recipe for a set of measurements. When a LabBook is run, the measured data are

added to it. Once measured data are added, they cannot be deleted from the LabBook.

6.3.2 Auxiliary Computer

There is an auxiliary computer in the 4D Labs Instrument space room (TASC 2, room 7076) on which Qte-

gra is installed. On this computer, Qtegra LabBooks may be created and modified, acquired data may be

viewed, and reports may be created. There is no charge for the use of this computer. Users are encouraged

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to use the auxiliary computer for these purposes in order to avoid tying up the instrument computer unnec-

essarily.

The instrument computer may also be used to create and modify LabBooks, view acquired data, and create

reports but the usual tool charges will apply if the ICP-MS is reserved for those purposes.

7 Measurement Overview

7.1 Manual Sampling versus Autosampling

Except, perhaps, when only making a few quick measurements, autosampling is preferred to manual sam-

ple loading. The advantages of autosampling are:

LabBooks may be run unattended.

Loading incorrect samples is less likely because the operator has the opportunity to check (and even re-

check) that the actual sample vial positions match the positions in the measurement recipe.

If the wrong sample is loaded by mistake, it may be discovered by reviewing the measurement recipe.

When present while the LabBook is running, the operator can focus on examining the results, instead

of moving the sample probes to different solutions.

Be cautious about running samples unattended. Except, perhaps, when measurements are routine, it is

important to check from time to time that the measured signal intensities make sense, especially for the

first few measurements. Otherwise, a lot of time may be wasted.

7.2 Measurement Recipes

7.2.1 LabBooks

Measurements and analysis methods are created and run from a Qtegra LabBook. A LabBook consists of a

recipe for the measurement, a vessel for the data which are acquired when the LabBook is run, and a

method of analysis of the data. Once data are acquired, they cannot be deleted from the LabBook, alt-

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hough the entire LabBook with all of its data can be deleted. By the same token, once a measurement in a

LabBook has been run, it cannot be run again because it has data associated with it. On the other hand, a

new LabBook can be created from an existing LabBook, which has data in it.3 The new LabBook will have

the same measurement recipe as the original LabBook but no measured data.

7.2.2 Templates

A Template is a file which contains a measurement method and an analysis method. When a specific

measurement and analysis method is to be run repeatedly, it is useful to create a Template. Although a

Template cannot be run, a LabBook with the same measurement and analysis methods can be created

from the Template. Then, the Sample List in the LabBook can be populated and the LabBook can be run. It

is preferable to create a LabBook from a Template, rather than a LabBook, because a LabBook may be-

come corrupted when it is run.

7.2.3 Evaluation Methods

Each Template is based on an evaluation method. The primary evaluation methods relevant to the 4D Labs

iCAP Q ICP-MS are:

eQuant: External standards are used to quantify measurements of analyte concentrations in unknown

sample solutions. See Section 7.4.2.

trQuant: For laser ablated solid samples. See ICP-MS Laser Ablation Module Operation Procedure.

rQuant: For isotope dilution. See Section 7.6.1.

Other evaluation methods, which may be used with the 4D Labs iCAP Q ICP-MS but are less useful, are:4

3 Although a new LabBook can be created from an existing LabBook, it is preferable to create a new LabBook from a template

(see below).

4 Another evaluation method, tQuant, is for ICP-MS systems with an interface to a chromatograph. The 4D Labs iCAP Q does not

have this option.

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aQuant: For standard addition analysis; however, eQuant can also be used for standard addition analy-

sis and is more versatile so, usually, eQuant is preferred.

Raw Date: No analysis is performed on the measured data.

7.3 Measurement Modes

The 4D Labs iCAP Q has two basic measurement modes, STD (standard) and KED (Kinetic Energy Discrimi-

nation). KED mode can be subdivided further into two cell modes, depending upon the type of gas flowing

into the collision/reaction cell.5 Two ports CCT1 and CCT2 feed gas directly into the collision/reaction cell.

Currently, He gas is connected to CCT1 and H2 gas is connected to CCT2. KED mode can be configured in

the software to use either port. If the collision/reaction cell is configured to use He (an inert gas), then the

cell operates in collision mode. If the cell is configured to use a reactive gas, e.g., H2, O2, or NH3, then the

cell operates in reaction mode.6 The KED cell modes are summarized in Table 7-1.

Table 7-1: KED cell modes.

Gas Port Cell Mode

He CCT1 Collision (KED)

H2 CCT2 Reaction

The basic STD and KED measurement modes have a number of variants, which require different hardware

than the basic configuration. The modes are listed in Table 7-2.7

5 ThermoScientific's trade name for the collision/reaction cell is the Qcell.

6 Kinetic energy discrimination only occurs in collision mode. When the collision/reaction cell operates in reaction mode, the term

KED is not actually applicable, but, nevertheless it is used in the software.

7 There are additional modes listed in the software but they are not recommended, e.g., because the required hardware is not

installed.

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Table 7-2: iCAP Q measurement modes.

Basic High Sensitivity

Argon Gas Dilution

Laser

STD STDS STD AGD Laser STD

KED KEDS KED AGC Laser KED

The basic modes (STD & KED) use the standard interface cones.

The high sensitivity modes use high sensitivity cones. Sensitivity is about a factor of two higher. The high

sensitivity cones are recommended for laser ablation and for trace element analysis of low matrix, i.e.,

clean, solutions. The high sensitivity cones will be rapidly degraded by high matrix, i.e., dirty, solutions.

Argon gas dilution involves injecting an additional Ar gas flow directly into the injector, while reducing the

Ar flow into the nebulizer. Reducing the nebulizer flow reduces the sample uptake, effectively diluting the

sample. The effect is similar to liquid dilution of the sample.

In the laser modes, the liquid sample introduction system is replaced by the laser ablation cell, which is

connected directly to the injector.

7.4 Quantification

7.4.1 Why are Standards Needed for Quantification?

ICP-MS measurements are inherently qualitative. In addition to depending upon the analyte concentration,

the measured intensity at the analyte mass depends upon:

Instrumental parameters, some of which are well controlled and relatively constant but others of which

are poorly controlled and vary with time even in the short term.

Interfering ions, which may consist of single species, dimers, trimers, etc.

The matrix containing the analyte.

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ICP-MS measurements of an analyte may be made semi-quantitative by the measurement of various types

of standards. In all cases, the matrix of the standard should be similar to that of the samples since the ma-

trix is one of the factors that affects the measured intensities. Three types of standards are discussed in the

following sections.

External standard: Contains the analyte of interest in a known concentration.

Internal standard: Must not contain the analyte of interest but does contain a different analyte with a

similar mass, e.g., within 50 amu.

Isotopic standard: Contains the isotopes of interest in known concentrations.

7.4.2 External Standards

External standards are a valuable tool to help quantify analyte concentrations. Typically, a series of external

standards, each of which contains the analytes of interest in known concentrations, are measured immedi-

ately before all of the samples. External standards may be single element standards or multi-element

standards. In the latter case, one must avoid introducing interferences.

The range of the analyte concentrations in the external standards should extend below and above the ana-

lyte concentrations in the samples and must include a calibration blank, which is a standard in which the

analyte concentration is insignificant, ideally zero.8 When using multi-element external standards, a wide

range of concentrations may be required if different analytes have a widely different concentrations in a

sample. The matrices of all of the standards, including the blank, should be identical and as close to those

of the samples as possible.

The analyte concentrations in each external standard are defined in a LabBook under Method Parameters:

Standards (see Section 9.6.2.6). ICP-MS measurements of the external standards are specified in Sample

List (see Section 9.6.3).

8 Qtegra requires that a blank be specified in order to generate a calibration curve. In principle, an operator could measure a

series of external standards without a blank and generate a calibration curve manually but this is not recommended.

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When a LabBook, which includes measurements of a set of external standards, is run, Qtegra quantifies

analyte concentrations and generates a calibration curve of intensity vs. concentration for each analyte.

7.4.3 Internal Standards

Internal standards are intended to compensate for drift due to poorly controlled measurement parameters.

They are added to all samples but do not contain the analytes of interest.9 Although internal standards are

a valuable tool when measuring analyte concentrations, they may do more harm than good when measur-

ing isotope ratios. This is result of the timing difference between concentration measurements and isotope

ratio measurements. The time difference between measurements of external standards and samples is typi-

cally a few minutes so drift is likely to be significant. On the other hand, the time difference between

measurements of the isotopes of an element depends only on the dwell times and is normally a small frac-

tion of a second. Drift in isotope ratio measurements should be insignificant. Attempts to correct for insig-

nificant drift will only introduce errors related to the imprecision of the measurements.

When a LabBook is run, the internal standard solution flows into the ICP-MS continuously, in conjunction

with the sample during measurements and with the carrier solution between measurements. The intensity

of a single mass in the internal standard solution is monitored during sample measurements and, as the

internal standard mass intensity changes, the intensities of the analytes are corrected accordingly. The in-

ternal standard solution must not contain any analyte of interest but it should contain an element with a

mass and ionization potential near that of the analyte of interest. Preferably, the mass should be within 50

amu. Concentration of the internal standard should be selected to give a signal intensity ~ 1 x 105 c/s. If

unsure, try 5 ppb – 10 ppb initially.

Since the response of the ICP-MS is mass dependent, the accuracy of the correction provided by the inter-

nal standard will decrease as the difference between the analyte mass and the internal standard mass in-

creases. Consequently, when there are multiple analytes which differ significantly in mass or ionization po-

tential, it may be beneficial to specify more than one element as an internal standard.

9 The method of isotope dilution is an exception. See Section 7.6.3.

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7.4.4 Isotopic Standards

Isotope ratio measurements require correction for dead-time and mass bias (see Section 7.6.1). In order to

make these corrections, one requires a set of isotopic standards, which contain the isotopes of interest in

known concentrations. Isotopic standards are employed in a similar manner to external standards. Typical-

ly, a series of isotopic standards are measured immediately before all of the samples. The range of the iso-

tope concentrations in the isotopic standards should extend below and above the analyte concentrations in

the samples. No calibration blank is required. The matrices of all of the standards should be identical and

as close to those of the samples as possible.

The isotope concentrations in each isotopic standard are defined in a LabBook under Method Parameters:

Standards (see Section 9.6.2.6). ICP-MS measurements of the isotopic standards are specified in Sample

List (see Section 9.6.3).

7.5 Quality Control

For quality control, it is recommended to additionally re-measure the blank and one of the standards im-

mediately after the set of standards and after each sample or a subset of samples. Commonly, these meas-

urements are labelled the "QC Blank" and the "QC standard" in the Sample List. The resulting measure-

ments are not used for calibration. Instead, they should be used to assess the quality of the measurements,

specifically, to determine whether the original intensities are recovered. In the original intensities are not

recovered, appropriate steps should be taken to ensure that they are.

In addition, Qtegra has a quality control feature for templates based on eQuant, which may be activated in

the Quantification window. This feature allows the operator to trigger warnings or errors when user-

specified parameter values exceed tolerances set by the user. This feature is outside the scope of this pro-

cedure. For additional information, refer to the Qtegra for iCAP Q ICP-MS Software Manual.

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7.6 Analytical Methods

7.6.1 External Standardization

External standardization is an analytical method in which solutions are prepared in several known concen-

trations from a standard reference material containing the analytes of interest. Typically, the external

standard solutions are measured before the samples and, for each analyte, a calibration curve of intensity

vs. concentration is generated. See Section 7.6.1.

7.6.2 Standard Additions

The method of standard additions is an analytical method in which a standard reference material contain-

ing the analytes of interest is added in known concentrations to identical samples. A calibration curve is

constructed from ICP-MS measurements of the spiked solutions. Since the matrix of the spiked samples is

essentially identical, this method is less prone to matrix induced errors than external standardization. How-

ever, since every sample is spiked with several concentrations of the SRM, sample preparation is much

longer than for external standardization.

7.6.3 Isotope Dilution

Isotope dilution is a quantification technique in which a known concentration (usually enriched) of the iso-

tope of interest in a standard is added to a sample containing an unknown concentration of that isotope.

Dilution refers to the fact that the enriched standard is diluted by mixing with the sample. Since the stand-

ard is added to the sample, it is a method of internal standardization. Relying on measurement of isotope

ratios, rather than concentrations, it avoids some the stability issues associated with concentration meas-

urements.

First, a set of at least three unknown samples are prepared in the same concentration. Then, all but one of

the unknown samples are spiked with different, known concentrations of the isotope of interest. The con-

centration of the isotope in the unknown sample is determined from the intercept of the intensity vs.

spiked concentration of the samples.

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7.6.4 Isotope Ratios

7.6.4.1 Measurement Parameters

Usually, very high precision (low RSD) is required for isotope ratios but some isotopes may have low abun-

dance. Precision can be improved by increasing the dwell time, number of sweeps, and number of repeti-

tions (main runs), e.g.,

Dwell time = 50 ms for low abundance isotopes.

Number of sweeps = 200 to start. For high precision more may be required, e.g., 500.

Number of main runs = 10.

All of these increases mean that larger volumes of solutions are usually required for isotope ratio meas-

urements as compared to other types of ICP-MS measurements. Consequently, it is important for the oper-

ator to estimate the amount of solution required for each measurement and for the entire LabBook. It may

be necessary to use a large autosampler loop volume and to prepare relatively large volumes of the blank,

rinse, external standards, and samples. In particular, repeated QC blank and QC standard measurements

will increase the demand for those solutions substantially.

It may be that even the largest autosampler loop volume does not provide enough solution to give the re-

quired precision. In that case, it may be desirable to perform repeated measurements of the sample be-

cause the loop will be refilled for each measurement.

235U/238U is a commonly used certified reference material for isotope ratios.

235U/238U = 0.01 in certified reference material.

235U dwell time = 50 ms, 238U dwell time = 10 ms.

7.6.4.2 Corrections

Two important corrections are required for the calculation of isotope ratios.

Dead time correction, if using pulse count mode

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Mass bias correction

In pulse counting mode, dead time due to the finite response time of the electronics reduces the measured

intensity. If the interval between pulses is much greater than the dead time, the effect of the dead time on

the intensity (i.e., pulse count rate) is insignificant; however, as the intensity increases, the time between

pulses becomes comparable to or even less than the dead time so the electronics is unable to count all of

the pulses. It is important to correct for this error in pulse count mode. In analogue mode, there is no dead

time so correction is unnecessary.

Dead time can be corrected for by measurements of a standard reference material (SRM), which contains

the isotope of interest and for which the isotope ratios are known. It should be prepared in a series of ana-

lyte concentrations both greater and less than the analyte concentrations of each unknown samples. Pro-

vided that all of the data are acquired in pulse count mode, by plotting the intensity vs. concentration curve

for each isotope of the SRM and comparing with the intensities of the unknown isotopes, the concentra-

tions of the unknown isotopes can be calculated with the dead time correction. The calibration curve gen-

erated from the measurements in a LabBook may be helpful in this regard; however, the linear fit generat-

ed does not take into account mass bias and it is only applicable if all of the measurements are in pulse

count mode or all are in analogue mode.

The need for mass bias correction stems from the fact that the sensitivity of the ICP-MS depends on the

mass detected. In other words, the ICP-MS sensitivity will be different for different isotopes.

After making the dead time correction, one can correct for mass bias using the following equation, where

IR = Isotope Ratio and Standard IR of SRM means the specified value of the isotope ratio of the SRM.

(Corrected IR of sample) = (Measured IR of sample) x (Standard IR of SRM) / (Measured IR of SRM)

Actually, since the SRM was prepared in several concentrations, there will be a measured IR of the SRM for

each concentration. All should be similar in value. One may wish to take a weighted average of those val-

ues.

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7.6.5 Standard Additions

Use at least 3 standard addition spikes.

8 Sample Preparation

Sample preparation is largely beyond the scope of this document but a few guidelines will be presented

here. It is important that the matrices of all samples, standards, and blanks be as similar as possible. Alt-

hough deionized water may be used as a solvent, better results will usually be achieved by using an acidic

matrix. The presence of an acid helps to avoid precipitation, which, of course, would change the analyte

concentration.

Nitric acid is a good general purpose acid because it dissolves a wide range of materials and the ions that

it contains will already be present. Thus, it should not create additional interferences. On the other hand,

some elements do not have sufficiently high solubility in nitric acid and some elements (e.g., Os) react to

form hazardous compounds so other acids must be used.

Hydrochloric acid is the next most commonly used acid for ICP-MS but chlorine ions may generate prob-

lematic interferences.

Hydrofluoric acid is required for some elements but the 4D Labs ICP-MS is not compatible with solutions

containing > 0.1% HF. Furthermore, the 4D Labs ICP-MS does not have suitable exhaust for the handling

of HF solutions.

Samples in solutions with low acid concentrations, e.g., 2% HNO3, can usually be kept for 1-3 months

without degradation. Ag and Hg are exceptions, which should be analyzed within 1 week.

Ag solutions should be kept in the dark to mitigate photo-reduction.

Hg is absorbed into sample containers.

Samples in deionized water are typically only stable for a few days.

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The use of high purity reagents, deionized water with resistivity 18 MOhm-cm, and clean labware is es-

sential for the preparation of ICP-MS samples. For ppb level analysis, reagents should be trace metal grade.

Glass labware is acceptable. Labware, including sample vials, should be cleaned and rinsed with deionized

water. Soaking for a day in 20% high purity nitric acid would be beneficial at the low end of the ppb scale.

For ppt level analysis, reagents should be ultra-trace metal grade. Labware should be cleaned and samples

prepared in a cleanroom. Fluoropolymer labware is preferred. Labware should be cleaned, soaked for 1 – 7

days in 20% trace metal grade nitric acid, and rinsed with deionized water.

More detailed information about sample preparation for ICP-MS may be found in the following documents.

Paul R. Gaines, ICP Operations Guide: A Guide for using ICP-OES and ICP-MS, Inorganic Ventures

(2011). https://www.inorganicventures.com/icp-operations-guide

Paul R. Gaines, Sample Preparation, Inorganic Ventures. https://www.inorganicventures.com/sample-

preparation

Paul R. Gaines, Trace Analysis Guide, Inorganic Ventures. https://www.inorganicventures.com/trace-

analysis-guide

9 ICP-MS Operation Procedure

9.1 Personal Protective Equipment

Safety glasses should be worn at all times in the vicinity of the ICP-MS, including near the computer.

Appropriate chemical-resistant gloves should be worn at all times when in contact with equipment in-

side the mini-environment.10

10 For low concentration nitric acid solutions, nitrile gloves are acceptable.

https://www.inorganicventures.com/icp-operations-guide





23



9.2 Log-in

1) Observe whether the LEDs on the front panel of the ICP-MS are in the following states. If not, do not

proceed. Instead, contact the tool owner.

a) Power: green.

b) Vacuum: green.

c) System: flashing blue.

2) Create a ticket on the 4D Labs User web site. List any supplies, which you are purchasing.

3) Start a record in the ICP-MS user log book.

9.3 Plasma Ignition

1) Check that the 10 L waste container is less than 75% full. When the peristaltic pump is on, solutions

flow at 24 mL/h. If the capacity is insufficient, ask the tool owner to empty the waste container.

2) Ensure that there is sufficient autosampler rinse solution. Typically, the container should be no less

than 25% full.

3) Ensure that the cylinder valves and pressure regulator outlet valves for all required gasses are open,

there is sufficient pressure in the cylinder, and that the pressure regulator is set correctly.

a) Argon: Always required. T-cylinder. 100 psi. When the plasma is ignited, the cylinder pressure will

drop about 200 psi/h.

b) LA Helium: Required for laser ablation. T-cylinder. 15 psi.

c) Oxygen: Required for organic solvent-based solutions. 25 psi.

d) CCT2 reaction gas (e.g., Hydrogen): Required for ICP-MS reaction mode. 15 psi.11

e) CCT1 Helium: Required for ICP-MS KED mode. 15 psi. 12

4) Ensure that the mini-environment fans are on.13

5) Switch on the mini-environment lights. The switch is at the left rear of the mini-environment.

11 Both the cylinder valve and pressure regulator outlet valve for CCT2 reaction gas should normally be left open at all times.

12 Both the cylinder valve and pressure regulator outlet valve for CCT1 He should normally be left open at all times.

13 The mini-environment fans should normally be left on at all times.

24



6) On the ICP-MS chiller:

a) Ensure that the coolant level is in the correct range.

b) Switch on the chiller pump, using the button on the front of the chiller.14

Figure 9-1: Chiller pump switch.

7) Check the condition of the peristaltic pump tubing. If the section which is stretched over the pump is

flattened, try the adjacent section. If both sections are flattened, replace the tubing.15

8) Stretch the peristaltic pump tubing (sample, internal standard, and waste) over the peristaltic pump but

don't clamp it with the collar.

9) Ensure that the tubing is placed over the pump drum in the correct direction.16

14 The power switch at the rear of the chiller is normally left on at all times.

15 The peristaltic pump tubing is colour coded by three plastic stops: orange – yellow - orange. One can place either the section

of tubing between the first (orange) and second (yellow) stops or that between the second (yellow) and third (orange) stops over

the pump drum. The lifetime of the tubing can be extended by using one section and then the other. For new tubing, start with

the first (orange) and second (yellow).

16 The pump should be set to rotate clockwise in the software, in which case the solution should enter the pump from the left

and exit from the right.

25



10) Ensure that there is sufficient rinse solution.17

11) Place the two manual probes (sample and internal standard) into the rinse solution.

Figure 9-2: Manual probes in rinse solution.

12) If the autosampler will be required, switch on the power to the autosampler.18 The autosampler probe

should move to its home position above the rinse tank.

13) Log on to the ICP-MS computer as 4DLabs.

14) Run Instrument Control.

15) In Instrument Control, go to the Control Panel, on the left side.

a) Select the Main panel and set the torch horizontal and vertical positions to 0.

i) Type "0".

ii) Press Enter.

b) Select the Plasma panel and check whether the Plasma Exhaust pressure is in the range 0.4 – 0.6

mbar. If it is not, do not proceed. Instead contact the tool owner.

c) Select the Inlet panel.

i) Ensure that the Peristaltic Pump Speed is set to 20 rpm.

ii) Press the Peristaltic Pump On button.

17 Normally, the rinse solution is 2% nitric acid in deionized water (DIW).

18 Rocker switch on the left side of the autosampler.

26



iii) Wait 20 s.

iv) Press the Peristaltic Pump Off button.

16) Clamp each peristaltic pump tube to the pump drum by pressing down firmly on its collar and rotating

its lock pin onto the collar.19 Do not clamp any collar without tubing underneath.

17) Click on Experiment Configuration in the Instrument Control menu bar and select the desired configu-

ration from the scroll-down list.

a) iCAP: for solution-based ICP-MS with samples introduced from the manual sample probes.

b) iCAP with DX FAST: solution-based ICP-MS with samples introduced from the autosampler.

c) iCAP with Laser: ICP-MS with sample introduction by laser ablation.

18) If iCAP with DX FAST is selected as the Experiment Configuration:

a) Select the ESI SC-4DX tab, which should appear to the right of the iCAP tab.

b) Select Tools: Initialize and wait for initialization to complete.20

c) The centre of the autosampler should display "Connected and initialized".

d) Confirm that the autosampler was initialized successfully by right clicking on any position and se-

lecting Move to. The autosampler should move to the position.

e) Right click on the current position and select Move home.

19) Ensure that the chiller temperature is 20°C.

20) Ignite the plasma as follows.

a) Click on iCAP in the Instrument Control menu bar. The iCAP ribbon should open.

b) Press the On button in the Control group on the iCAP ribbon.

c) At the prompt, confirm that you wish to ignite the plasma. The plasma ignition process should

commence. Its progress may be observed in the log window.

d) Observe the plasma as it ignites; ignition should occur about 30 s after starting the process. In the

following the plasma may be extinguished rapidly by opening the door to the interface region

(cones) at the front of the iCAP. Then, inform the tool owner.

19 It is important to press down on the collar in order to avoid applying excessive force to the lock pins. They are not very strong.

20 The autosampler should be initialized even if the display states that it is already.

27



i) Flickering once or twice during the first second or two is normal. If flickering continues for

more than 5 s, extinguish the plasma rapidly. 21

ii) When viewed through the window to the interface region, the plasma should appear green. If

it is orange, extinguish it rapidly.

e) Wait for the message "Operate" to appear in the Log View window, indicating that the start-up

procedure has completed successfully.

21) Make a note of the time at which the plasma ignition process was completed.

22) Make a quick check of the flow through the manual probes by simultaneously lifting both of them out

of the solutions for about 2 s. Then, return them to the solutions. An air bubble should appear in the

transparent section of each tube about 6 s after the probe was removed. If not, resolve the issue be-

fore proceeding.22

23) Press the Run button in the Control group on the iCAP ribbon.

24) Open the Data Display window to display the real-time measurements. In the display, the following

notation is used:

Doubly charged = 137Ba++:137Ba+ ratio.

Oxides = 140CeO+:140Ce+

KED = 59Co+:35Cl 16O+ ratio. It is desirable for it to be high.

25) In the iCAP ribbon, go to the Measurement mode group, and select the desired mode in the Select

scroll box.

26) Measure the sample flow as follows.

a) Record the volume of the rinse solution in its vial in mL.

b) Start a timer.

c) Wait at least 10 min in order to get an accurate measurement.

d) Record the volume of the rinse solution in its vial in mL.

21 The torch may be damaged by excessive flickering.

22 Flicking the tubing with your finger may help.

28



e) Stop the timer.

f) Calculate the flow. It should be 0.40 mL/min. If it is significantly different, check the sample intro-

duction system.

27) Before running performance tests, autotuning, or making measurements:

a) Ensure that the sample flow is correct, i.e., 0.40 mL/min.

b) Wait 30 min to allow the system to stabilize and, if required, the collision/reaction cell gas lines to

be purged.23

Note that:

For a clean system with 2% HNO3 flowing, the 238U intensity should be ~ 20 c/s.24

RSDs in the real-time display are typically higher than in measurements because only 10 sweeps

are used. RSD ≤ 5% is good.

After the system has stabilized, if the plasma is extinguished for more than 1 h, after re-igniting the plas-

ma, wait 30 min for stabilization. If the plasma is extinguished for < 1 h, the wait time for stabilization

may be shorter.

9.4 Performance Report

A built-in set of performance tests allows one to check whether the iCAP Q meets specifications for a spe-

cific measurement mode. Each day, you should ensure that the iCAP passes the performance tests for the

measurement mode you wish to use prior to measuring reference materials or samples. Furthermore, after

switching measurement modes, the performance tests for the new mode should be run.

23 Heavy masses take longer to equilibrate than light masses. Full warm-up reduces 137Ba++ : 137Ba+ ratio and sensitivity im-

proves.

24 With DIW flowing, the 238U intensity should be ~ 200 c/s.

29



This section describes how to run the performance tests. It is assumed that the plasma has been ignited,

the manual sample probes are in the rinse solution, and the system has stabilized (15-30 min after igni-

tion).

1) Ensure that the iCAP ribbon is open. If it is not, click on iCAP in the Instrument Control menu bar. The

iCAP ribbon should open.

2) In the iCAP ribbon, go to the Measurement mode group, and select the desired mode in the Select

scroll box.

3) Ensure that the system has warmed up.

a) For all measurement modes, wait 30 min after the plasma has ignited.

b) In KED mode, wait 30 min after activation of KED mode to insure that the collision/reaction cell is

purged. May be concurrent with plasma warm-up.

4) Place both manual sample probes in the iCAP Q Tune B solution.

5) Observe the Data Display window.

6) After 80 s, the intensities of the selected analytes should rise sharply and continue to increase over 20

s.

7) Wait for the analyte intensities to stabilize.25

8) In the Wizards group, select Performance Report. The Performance Report Wizard window should

open.

9) Select Run Performance Report from active Measurement mode.

10) Press Next.

11) You will be asked to confirm that the measurement probes are in the "1 ppb Tune B in 2% HNO3 and

0.5% HCl" solution. Click Next to confirm. Performance tests should begin. About 10 min is required

to complete the tests. When the tests a completed, a summary of the results of the tests will be dis-

played in the Performance Report Wizard window.

12) After reviewing the results, click Next. The final Performance Report Wizard window should display

"Completing the Performance report run wizard".

25 In STD mode, intensities should be ~ 105 c/s. If the intensities are low, the cones may need to be cleaned.

30



13) If desired, check Open Report.

14) Press Finish. The Performance Report should open.

15) In the Performance Report, observe whether all tests were passed.

a) If all tests were passed, move the manual probes to the rinse solution and proceed to making

measurements.

b) If any test failed, carry out tuning, as described in Section 9.5. If Source Tune will be performed

promptly, the manual probes may be left in the tuning solution because it will be required for auto-

tuning. Otherwise, move the probes to the rinse solution.

Performance Reports may by clicking Performance Report in the Views group of the iCAP ribbon.

9.5 Autotuning

9.5.1 Tuning Methods

Tuning should be performed if one or more performance tests are failed. If all performance tests are

passed, tuning is unnecessary. Instrument Control provides several automated tuning routines, which are

listed in the Wizards group of the iCAP ribbon.

Autotune

Mass Calibration

Detector Setup

If a mass calibration test fails, the Mass Calibration wizard should be run. For other modes of failure, the

Autotune wizard should be run. Users should not need to run the Detector Setup wizard.

The Autotune wizard contains a number of tuning routines each of which is specific to a particular meas-

urement mode. In addition, it includes a global tuning routine called Source Tune, which tunes parameters

common to all measurement modes. If autotuning is required, it is recommended to run Source Tune first.

Afterwards, repeat the performance tests. If one or more performance tests still fails, run the autotuning

routine for the active measurement mode (unless the problem is mass calibration).

31



If autotuning fails repeatedly, contact the tool owner.

9.5.2 Source Autotune

Source Autotune tunes the parameters which are common to all measurement modes. It should be run

when using the standard interface cones. When using the high sensitivity cones, see Section 9.5.3.

Run the Source Autotune routine as follows.

1) Ensure that both manual sample probes are in the iCAP Q Tune B solution.



4) Click the Autotune button in the Wizards group of the iCAP ribbon.

5) In the drop-down list, select Source Autotune. The Autotune Wizard [SourceTune High Matrix] Load

the sample window should open. If the measurement mode was not STD, it should change to STD.

6) Click Next. The Tune Data View window should open.

7) Wait for tuning to be completed. When tuning is completed, you may view the results graphically by

clicking the left and right arrows at the top left of the Tune Data View window.

8) Click Next. The Acquisition status window should open. It lists the effect of tuning on analyte intensi-

ties.

9) Click Next. The autotune completion window should open.

a) You have the option to save or discard the results of tuning. Usually, you should save the results by

selecting Yes.

b) Optional: Check Open Report, if you wish to view the tuning report after the next step.

10) Press Finish.27 The measurement mode should return to its original state (before running Source Auto-

tune).


27 If you fail to press Finish, the new tuning parameters will not be saved and the iCAP Q will revert to the values prior to auto-

tuning.

32



11) Run the Performance Report wizard again (see Section 9.4).

9.5.3 Other Autotune Routines

Other Autotune routines include:

!CaliTune KEDS line 1: For KED mode using He gas. Uses CCT gas line 1. Tunes the parameters specific

to KED & KEDS modes.

!CaliTune KEDS line 2: For KED mode using H2 gas. Uses CCT gas line 2. Tunes the parameters specific

to KED & KEDS modes.

SourceTune High Sensitivity : To be run when using high sensitivity interface cones. Tunes the parame-

ters which are common to all measurement modes.

In general, if a performance test fails, one of the SourceTune routines, which tunes the parameters com-

mon to all modes, should be run before tuning the parameters specific to the desired mode. In other

words, run SourceTune High Matrix or SourceTune High Sensitivity first, depending upon the type of inter-

face cones installed.

1) Ensure that both manual sample probes are in the iCAP Q Tune B solution.



4) Click the Autotune button in the Wizards group of the iCAP ribbon.

5) In the drop-down list, select Autotune Wizard. The autotune welcome window should open.

6) Select Run an existing Autotune sequence.

7) Click Next. The Select an autotune sequence window should open.

8) Select the desired autotuning sequence in the left pane, e.g.,

!CaliTune KEDS line 1

!CaliTune KEDS line 2


33



SourceTune High Sensitivity

9) Click Next. The Load the sample window should open.

10) Click Next. The Tune Data View window should open.

11) Wait for tuning to be completed. When tuning is completed, you may view the results graphically by

clicking the left and right arrows at the top left of the Tune Data View window.

12) Click Next. The Acquisition status window should open. It lists the effect of tuning on analyte intensi-

ties.

13) Click Next. The autotune completion window should open.

a) You have the option to save or discard the results of tuning. Usually, you should save the results by

selecting Yes.

b) Optional: Check Open Report, if you wish to view the tuning report after the next step.

14) Press Finish.29


9.5.4 Mass Calibration

The Performance Report wizard measures the centre and width of selected mass peaks. If any of these val-

ues are outside the specified tolerance, the mass calibration test fails and the Mass Calibration wizard

should be run as follows.

1) Ensure that both manual sample probes are in the iCAP Q Setup solution.



4) Click the Mass Calibration button in the Wizards group of the iCAP ribbon. The mass calibration wel-

come window should open.

5) Click Next. The Coarse Mass Calibration window should open.

29 If you fail to press Finish, the new tuning parameters will not be saved and the iCAP Q will revert to the values prior to auto-

tuning.


34



6) Ensure that the Execute a Coarse Mass Calibration first checkbox is not checked.

7) Click Next. The Load the Sample window should open.

8) Click Next. The Waiting for sample uptake window should open.

9) Click Next.31 Mass calibration should commence.

10) Optional: Real-time data acquired for mass calibration may be displayed graphically by clicking the Da-

ta Display tab.

11) Wait for calibration to be completed. When calibration is completed, the Acquisition status window

should open. It lists the calibration results.

12) Click Next. The mass calibration completion window should open.

13) Optional: Check Show Mass Calibration to view a report of the results after the next step.

14) Press Finish.32


9.6 Measurements

9.6.1 Create a LabBook

1) Open Qtegra. Normally, the Dashboard will be displayed. If not, select Home Page: Dashboard.

2) Observe the colour of the Get Ready button.

a) If it is green, proceed to the next step.

b) If it is red, move the cursor over it.

i) If the cursor is a hand, click the Get Ready button. It should turn green.

ii) If the cursor remains an arrow, close Qtegra, restart the computer, open Qtegra, and try again.

3) On the left pane, select LabBooks. The LabBooks window should open, as shown in Figure 9-3.

31 There should be no need to wait for uptake because you should have already waited for the signal intensities to stabilize.

32 If you fail to press Finish, the new mass calibration parameters will not be saved and the iCAP Q will revert to the values prior

to running the mass calibration wizard.

35



Figure 9-3: Qtegra LabBooks window.

4) In the LabBooks window, do the following.

a) Name: Type the filename of your new LabBook. The filename should begin with your initials so

that your LabBooks can easily be identified.

b) Location: It is recommended that you keep your LabBooks in the LabBooks folder but you may

browse to a different folder.

c) Select one of the three methods of creating a LabBook. It is recommended that you either create

your new LabBook from an existing template or from a blank template (eQuant for solutions, ex-

36



cept rQuant for isotope dilution, or trQuant for laser ablation).33 Creation from an existing LabBook

is not recommended because the LabBook may have errors.

d) Click Create LabBook. A new tab for the LabBook should open.

9.6.2 Method Parameters

9.6.2.1 Analytes

1) In the left pane of the LabBook, select Method Parameters: Analytes. The Analytes window should

open, as shown in Figure 9-4.

33 If your LabBook is created from a blank template, the sample introduction method will correspond to the method in the cur-

rent Experiment Configuration.

37



Figure 9-4: Method Parameters: Analytes window.

2) Select the desired analytes as follows.

a) Left click an element to select the most abundant isotope.

b) Right click an element to open the isotopes window for the element. Check the checkboxes of the

desired isotopes in the first column.

9.6.2.2 Acquisition Parameters

1) In the left pane of the LabBook, select Method Parameters: Acquisition Parameters. The Acquisition

Parameters window should open, as shown in Figure 9-5.

38



Figure 9-5: Method Parameters: Acquisition Parameters window.

2) Enter the Acquisition Parameters for each analyte as follows.

a) Dwell time: Use the following guidelines.

i) In general, 5 ms ≤ Dwell time ≤ 200 ms. Default is 10 ms.

ii) STD mode: Typically, 10 ms ≤ Dwell time ≤ 20 ms.

iii) KED: Typically, 30 ms ≤ Dwell time ≤ 50 ms.34

iv) Laser ablation: Typically, 20 ms ≤ Dwell time ≤ 100 ms. Try 50 ms to start.

v) Use longer dwell times for analytes with low intensities, e.g., due to low concentration or high

mass.

b) Channels:35 Use the default value, i.e., 1.

c) Spacing:36 Use the default value, i.e., 0.1.

34 Intensities are suppressed in KED mode so longer dwell times are needed than for STD mode.

35 Number of channels used for each mass peak.

36 Spacing between channels in atomic mass units.

39



d) Measurement mode: Set as desired.37 Stability may be compromised if more than one mode is se-

lected.38

e) Resolution: Usually, should be set to Normal; however, if intensities are expected to be excessive,

they can be reduced by setting Resolution to High.39

3) Enter the Advanced Parameters for each analyte as follows.

a) Number of sweeps: Use the following guidelines.40

i) In general, 10 ≤ Number of sweeps ≤ 50, except for isotope ratios. Default is 10 sweeps.

ii) STD mode:

(1) Concentrations ≥ 10 ppb, try 10 sweeps.

(2) Concentrations ≤ 10 ppb, try 20 sweeps.

iii) KED mode: try 20 sweeps.

iv) Isotope ratios: try 200 sweeps. For high precision, more may be required.

b) Measurement order: Drag the mode to the desired position.

c) External Input Trigger: Not applicable.

d) External Output Trigger: Not applicable.

A measurement time ("runtime") estimate is displayed above the table. It is given by:

𝑅𝑢𝑛𝑡𝑖𝑚𝑒 = (𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑠𝑤𝑒𝑒𝑝𝑠) ∑ (𝐷𝑤𝑒𝑙𝑙 𝑡𝑖𝑚𝑒)

𝐴𝑛𝑎𝑙𝑦𝑡𝑒𝑠

37 See Section 7.2.

38 Although the Acquisition Parameters window allows the operator to measure different analytes in different measurement

modes, bear in mind that the measurement stability may be compromised when the mode changes. For example, when switch-

ing from STD mode to KED mode, the CCT1 gas is switched on and it may take up to 30 min for the instrument to stabilize.

39 In general, the Resolution setting should be used for control of intensity rather than resolution.

40 Not applicable for LabBooks based on tQuant & trQuant templates.

40



9.6.2.3 Monitor Analytes

Monitor Analytes is an optional feature (except for tQuant and trQuant), which allows one to modify the

uptake and wash, depending on the signal intensity and stability of one or more user-specified monitored

analytes. Uptake starts when the monitored analyte signal meets the user-specified stability value. If the

stability falls below the user-specified value after the measurement, the wash starts.

1) In the left pane of the LabBook, select Method Parameters: Monitor Analytes. The Monitored Analytes

window should open, as shown in Figure 9-6.

Figure 9-6: Method Parameters: Monitor Analytes window.

2) Set the ranges for the uptake and wash delays.

3) To add a monitored analyte, click Monitored Analyte. An empty row will be added to the table

4) In the Analyte column, type the mass and chemical symbol of the monitored analyte, e.g., 115In.

5) To enable the uptake settings:

41



a) Check the checkbox in the Uptake column.

b) Type the desired Signal Above (cps) threshold.

c) Type the desired Stability (%RSD) threshold.

d) In the On Failure column, select the desired outcome on failure from the dropdown list.

6) To enable the wash settings:

a) Check the checkbox in the Wash column.

b) Type the desired Signal Above (cps) threshold.

c) Type the desired Stability (%RSD) threshold.

d) In the On Failure column, select the desired outcome on failure from the dropdown list.

9.6.2.4 Survey Scan Settings

1) In the left pane of the LabBook, select Method Parameters: Survey scan settings. The Survey scan set-

tings window should open, as shown in Figure 9-7.41

41 Not applicable for LabBooks based on tQuant & trQuant templates.

42



Figure 9-7: Method Parameters: Survey Scan Settings window.

2) Set the parameters for the survey scan region, as desired.

3) Additional scan regions may be added by placing the cursor near the right edge of the graph, right

clicking, and selecting Add new range.42

Regions shaded in pink are protected and will not omitted from the scan.

The estimated runtime for the survey scan is displayed above the table. It is given by:

𝑅𝑢𝑛𝑡𝑖𝑚𝑒 =(𝐸𝑛𝑑 𝑚𝑎𝑠𝑠 − 𝑆𝑡𝑎𝑟𝑡 𝑚𝑎𝑠𝑠)(𝐷𝑤𝑒𝑙𝑙 𝑡𝑖𝑚𝑒)

𝑆𝑝𝑎𝑐𝑖𝑛𝑔 (𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑠𝑤𝑒𝑒𝑝𝑠)

42 Multiple scan regions may be desired if, e.g., different dwell times are desired in different regions.

43



Samples with very high concentrations of some masses may overload the detector and cause the intensities

in following main runs to be suppressed. If this occurs, omit those masses from the survey, reduce the

dwell time, or run the survey in a separate measurement from the main runs.

9.6.2.5 Interference Correction

The Interference Correction window allows one to correct for interference by subtracting the signal at a

specified mass multiplied by a correction factor depending on the relative abundances and relative instru-

ment sensitivities. Interference corrections may be turned on or off before and after the LabBook is run;

however, in order to apply an interference correction, the correcting analyte must be measured using the

same mode as the corrected analyte. Ensure that any correcting analytes, which may be desired, are select-

ed in the Analytes window and that the correct measurement mode is selected in the Acquisition Parame-

ters window before running the LabBook! Interference corrections may do more harm than good if they are

applied injudiciously.

1) In the left pane of the LabBook, select Method Parameters: Interference correction. The Interference

Correction window should open, as shown in Figure 9-8. It contains a table of analytes and isotopic in-

terference corrections. By default, no corrections are active.

44



Figure 9-8: Method Parameters: Interference Correction window.

2) For each analyte for which interference correction is desired:

a) Check the Measure and Apply checkbox to activate the correction.

b) Enter the desired correction formula in the Correction column. The default correction may be se-

lected by right clicking and selecting Default interference correction from the menu.

3) If any correcting analytes are missing from the analytes list, click the Select missing analytes button in

the Qtegra toolbar.43

43 The correcting analyte is added to the Quality Control window but not enabled in any tests. It is added to the Quantification

window but Quantify is set to No. It is added to the Acquisition Parameters window with the same parameters as the corrected

analyte but these parameters may be changed.

45



Interference corrections applied during an acquisition may be removed later by unchecking the Measure

and Apply checkbox.

9.6.2.6 Standards

As described in Section 7.4, ICP-MS measurements are inherently qualitative but the use of standards can

make them quantitative. External and isotopic standards are defined in the Standards window of a Lab-

Book. One can either define a new standard or load a standard from the global standards database.

9.6.2.6.1 Defining a New Standard

1) In the left pane of the LabBook, select Method Parameters: Standards. The Standards window should


Figure 9-9: Method Parameters: Standards window.

46



2) (Optional) Set the default concentration, which will be used for each analyte added to the Elements

list of each standard solution.

a) Click in the Standard(s) toolbar. The Set Default Concentration dialogue box should open.

b) Type the value of the default concentration and select the units.

c) Click OK.

3) Create a new standard solution by clicking + New in the Standard(s) toolbar and select the type of

standard from the dropdown list. For LabBooks based on the eQuant template, the choices are: 44

a) Elemental

b) Internal (Isotopic)

c) Isotopic

The Add New Standard dialogue box should open.

4) Elemental standards

a) Type the Standard Name and Standard Description (optional) in the dialogue box.

b) All of the elements defined in the Analytes window (Section 9.6.2.1) may be added to the Selected

Elements list by checking the checkbox. The elements will be added to the Selected Elements list

with the default concentration.

c) Click OK.

d) Add or remove an element by clicking on the element in the periodic table (under the Selected El-

ements list). Elements will be added to the Selected Elements list with the default concentration.

e) Add polyatomic species to be included in the standard by finding the polyatomic species in the

Representation column of the Molecules list and checking the corresponding checkbox in the Use

in standard column. Then, the selected molecules should appear in the Selected Elements list with

the default concentration.

5) Isotopic standards

a) Type the Standard Name and Standard Description (optional) in the dialogue box.

44 Elemental and Isotopic cannot be mixed in the same LabBook but each may be combined with Internal (Isotopic).

47



b) All of the isotopes defined in the Analytes window (Section 9.6.2.1) may be added to the Selected

Isotopes list by checking the checkbox. The isotopes will be added to the Selected Isotopes list

with the default concentration.

c) Click OK.

d) Add or modify the isotopes to be included in each standard by right clicking an element in the pe-

riodic table. The isotopes window for the element should open. Check the checkboxes of the de-

sired isotopes

e) Click outside the isotopes window to close it.

f) Add polyatomic isotopes to be included in the standard as follows.

i) Select the polyatomic species from the list box at the top of the Molecules list.

ii) Check the checkbox in the Use in Standard column of the desired isotopes listed in the Repre-

sentation column. The selected isotopes should appear in the Selected Isotopes list with the

default concentration.

6) Modify the Concentration and Units of each item in the Selected Elements (Selected Isotopes) list as

desired. Normally, it will be necessary to multiply the concentration of each isotope by its abundance.

7) Add additional standards by one of the following methods.

a) Repeat steps 3) - 6).

b) Create a new standard from an existing standard using a dilution factor.

i) Select a standard from the Standard(s) list.

ii) Right click and select Copy from the dropdown list. The Select Dilution Factor dialogue box

should open.

iii) Type the desired dilution factor into the Dilution Factor box.

iv) Click OK. The new standard with the desired dilution factor should be added to the bottom of

the Standard(s) list.

v) Optional: Rename the new standard.

(1) Double-click the Name of the new standard.

(2) Type the new name.

(3) Press Enter.

48



8) Delete standards by selecting, right clicking, and selecting Delete from the dropdown list.

9.6.2.6.2 Standards Database

A standard in the database may be added to the Standard(s) list by:

1) Click the Open button in the Standard(s) toolbar.

2) Select the desired standard from the dropdown list.

3) Click OK. The standard should be added to the bottom of the Standard(s) list.

A standard in the Standard(s) list may be added to the global standards database by:

1) Select the standard in the Standard(s) list.

2) Right click and select Pass to global. The standard should be added to the global standards database.

9.6.2.7 Quantification

As discussed in Section , ICP-MS is inherently qualitative; however, it can be made quantitative by employ-

ing standards. The Quantification window enables the operator to specify the strategy for quantification.

Open dropdown lists by clicking near the right border of each cell.

1) In the left pane of the LabBook, select Method Parameters: Quantification. The Quantification window

should open, as shown in Figure 9-10, with each analyte selected in the Analytes window listed.

49



Figure 9-10: Method Parameters: Quantification window.

2) eQuant only: If desired, check the Use Quality Control checkbox. If checked, the Quality Control win-

dow should be added to the left pane under Method Parameters.45

3) Modify the default parameters for each analyte in the Quantification table as desired.

a) Quantify: Choose whether the analyte is to be quantified using standards using the dropdown list.

Choices are:

i) Yes

ii) No. The only choice for internal standards and molecules (see Section 9.6.2.6).

45 The Quality Control feature allows one to set a warning or error if specified parameters fall outside user-specified control lim-

its. It is only available for templates based on eQuant. This feature is outside the scope of this procedure. For information about

Quality Control, refer to the Qtegra for iCAP Q ICP-MS Software Manual.

50



b) Internal Standard: Select whether or not the analyte is to be used as an internal standard from the

dropdown list. If not, select which internal standard to use for correction or whether to use inter-

polation between adjacent internal standards.

c) Fit Type: Select from the dropdown list the type of fit to be used to generate the calibration curve.

Choices are:

i) Linear

ii) 2nd Order

d) Weighting: Select from the dropdown list how to weight the measurements used to generate the

calibration curve. Choices are:

i) None

ii) Absolute SD

iii) Relative SD

e) Forcing: Select from the dropdown list whether or not to force the calibration curve to pass

through certain points. Choices are:

i) No

ii) Zero

iii) Blank

f) Use for Semiquant: Allows an analyte to be selected to contribute to the semi-quantification curve

or not.46 Choices in the dropdown list are:

i) Yes

ii) No

4) eQuant only: Warning and failure limits for internal standards may be set in the IS Recovery section.47

46 For a definition of semi-quantification, see Section 2.

47 See Qtegra for iCAP Q ICP-MS Software Manual.

51



9.6.2.8 Regions

The Regions window is only available for templates based on trQuant. The Regions window allows one to

define time spans as regions over which the signal is averaged for evaluation.

9.6.2.9 Ratios

The Ratios window allows one to set up calculation of concentration ratios of analytes (eQuant and

trQuant templates) or isotopes (rQuant templates). The format of the table is somewhat different in each of

those two cases but how to fill in the table is self-evident. Since isotopes can be defined as analytes in

eQuant and trQuant templates, the corresponding Ratios window can also be used to calculate isotope

ratios for those templates.

Analytes or isotopes may be selected from dropdown lists by clicking near the right border of the Analyte

or Isotope cell, as shown in Figure 9-11.

52



Figure 9-11: Method Parameters: Ratios window for an eQuant template.

9.6.3 Sample Introduction

9.6.3.1 Manual Sampling

1) Activate Instrument Control.

2) Ensure that the Experiment Configuration is set to iCAP.

3) Activate Qtegra.

4) In the left pane of the LabBook, select Method Parameters: Manual Sample Control.

5) Ensure that Use Manual Sample Control is checked.

6) Set the uptake and wash times. Recommendations are:

a) Uptake time = 30 s. Uptake Time depends primarily on the manual probe length and flow rate.

53



b) Wash time = 10 s. Wash Time may need to be higher to reduce carry-over for high analyte concen-

trations and dirty matrices.

If a particular type of measurement is run routinely, it may be beneficial to optimize these times by observ-

ing the effect of changes on analyte intensities.

9.6.3.2 Autosampler

9.6.3.2.1 Determine FAST Loop Volume

The solution used in each measurement must be supplied by a single injection from the FAST loop. Conse-

quently, it is important to ensure that the loop has sufficient volume for the longest measurement. If the

loop volume is excessive, measurement time will be increased unnecessarily and sample will be wasted.

1) Determine the longest measurement time in the Sample List. The "Samplelist estimated runtime" dis-

played above the list is helpful in this respect.

2) Select the appropriate Loop Size from Table 9-1.48

3) Install the selected loop on the FAST valve between ports 1 and 4.

48 Loop Sizes in Table 9-1 are conservative. If sample volumes are insufficient for the recommended loop size, it may be accepta-

ble to use the next size down.

54



Table 9-1: Estimated measurement time as a function of FAST valve loop volume. Valid for 400 μL/min sample flow rate.49

Measurement Time (s)

Loop Size (mL)

Uptake Time (s)

Wash Time (s)

Probe in Sample (s)

<10 0.25 14 10 2

10-25 0.5 15 10 3

25-60 1 17 12 5

60-80 1.5 18 13 6

80-120 2 20 15 8

120-160 2.5 22 17 10

160-210 3 25 17 12

210-300 4 29 17 16

>300 Custom Custom Custom Custom

9.6.3.2.2 Configure Autosampler Settings in LabBook

1) Ensure that the autosampler is switched on.50

2) Activate Instrument Control.

3) Ensure that the Experiment Configuration is set to iCAP with DX FAST.

4) Select the ESI SC-4DX tab, which should appear to the right of the iCAP tab.

5) Ensure that "Connected and initialized" is displayed in the centre of the autosampler image.51

6) Activate Qtegra.

7) In the left pane of the LabBook, select ESI SC-4DX: Method Settings. The autosampler Method Settings

window should open.

8) Select Settings: Rack. The autosampler Rack window should open, as shown in Figure 9-12.

9) Ensure that the correct rack is selected.

49 Elemental Scientific, FAST Method Guide - iCAP Q, Document M-FMG-73, Table 1.

50 Rocker switch on the left side.

51 If not, select Tools: Initialize and wait for initialization to complete.

55



Figure 9-12: Autosampler Method Settings: Rack window.

10) Select Settings: Analysis. The autosampler Analysis window should open, as shown in Figure 9-13.

56



Figure 9-13: Autosampler Method Settings: Analysis window.

11) The following settings are suggested.

a) Sample: Uptake time [s] = 30 s.

b) Rinse 1: Wash Time [s] = 10 s. In the Sample section, Wash Time [s] should update.

c) Rinse 2: Wash Time [s] = 10 s.

12) In the left pane of the LabBook, select ESI SC-4DX: FAST Methods. The FAST Methods window should


57



Figure 9-14: Autosampler FAST Methods window. The current method is FAST 1.0mL.

13) Observe the current method in the tab at the top of the FAST Methods window. If it corresponds to the

current loop volume, configuring the autosampler is complete. If not,

a) Click +.

b) Under Open a template, click the arrowhead and scroll to the FAST method corresponding to the

current loop volume. The current method tab should update accordingly.

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9.6.4 Sample List

The Sample List is a list of measurements to be performed sequentially, using parameters from the Method

Parameters section and the sample introduction method listed in the left pane of the Qtegra window. An

example is shown in Figure 9-15.

Figure 9-15: Sample List table. The width of most columns has been reduced, truncating the headings, in this view.

The "Samplelist runtime estimate" is displayed above the sample list. This estimate is given by:

𝑅𝑢𝑛𝑡𝑖𝑚𝑒 = ∑(𝑁𝑆𝑆)(𝑆𝑢𝑟𝑣𝑒𝑦 𝑠𝑐𝑎𝑛 𝑡𝑖𝑚𝑒) + (𝑁𝑀𝑅)(𝑀𝑎𝑖𝑛 𝑟𝑢𝑛 𝑡𝑖𝑚𝑒) + (𝑆𝑎𝑚𝑝𝑙𝑒 𝑖𝑛𝑡𝑟𝑜 𝑡𝑖𝑚𝑒)

𝑀𝑒𝑎𝑠𝑢𝑟𝑒𝑚𝑒𝑛𝑡𝑠

where

NSS = number of survey scans

Survey scan time is displayed in the Survey scan settings window.

NMR = number of main runs.

Main run time is displayed in the Acquisition parameters window.

Sample intro time depends on the sample introduction settings, including such factors as the autosampler

loop settings (if applicable), uptake, and wash times.

In this section, the procedure for populating the Sample List is described.

59



1) In the left pane of the LabBook, select ESI SC-4DX: Sample List. The Samplelist window should open,

as shown in Figure 9-15.

2) A typical sequence of measurements is follows. If there are many samples, it is recommended to run

QC blanks and QC standards after each small subset of samples. If samples are dirty, it is recommend-

ed to run a QC blank and QC standard after each sample.

a) Rinse.

b) Calibration blank.

c) 3-5 external standards in order of increasing concentration.

d) Quality control blank.

e) Quality control external standard. Usually, an external standard with a concentration in the middle

of the range.

f) Samples.

g) Quality control blank.

h) Quality control external standard.

i) Rinse.

3) For each measurement, fill in a row of the sample list, as follows. For any columns not listed, use the

default values.

a) Label: Any text to identify the sample.

b) Survey Runs: Number of survey runs.52 Usually, 0 or 1.

c) Main Runs: Number of main runs. Value depends on the precision required but, typically 5 – 10.

d) Comment: Optional.

e) Evaluate: Check if results are to be evaluated. If unchecked, intensities will be measured but there

will be no analysis of the measurement.

f) Sample Type: Click just inside the right border of the cell and select one of the following options.

52 For dirty samples, very high intensities in the survey run may overload the detector and suppress intensities in the first few

main runs. In such situations, the sample concentration should be reduced or survey runs should be done in a separate meas-

urement from the main runs.

60



i) BLK for the blank sample to be used for calibration. There can be only one calibration blank

sample.

ii) STD for external standards.

iii) UNKNOWN for all other samples.

g) Standard: Only applicable for rows in which Sample Type = STD. Click just inside the right border

of the cell and select the correct standard from the dropdown list. The standards in the list were

defined in Method Parameters: Standards (see Section 9.6.2.6).

h) Rack Number: Click just inside the right border of the cell and select the number of the rack in

which the vial is located. See Figure 9-12. Irrelevant for manual sampling.

i) Vial Numbers: Click just inside the right border of the cell and select the vial position in the rack in

which the vial is located. See Figure 9-12. Irrelevant for manual sampling.

4) Save your LabBook.

Editing the Sample List

Description Action

Add a row to the bottom of the list Click + Add in the Qtegra toolbar

Delete rows Select the rows and click X in the Qtegra toolbar

Insert rows above Select a row, right click, select Insert rows ..., select the number of rows to insert, click OK.

Fill down Select a group of cells in a column, right click, select Fill down.

Figure 9-16: Sample list editing features.

9.6.5 Running a LabBook

9.6.5.1 Autosampler

The procedure for running a LabBook using the autosampler is described in this section. It is assumed that

the plasma has been ignited and the system warmed up (see Section 9.3). Generally, it is desirable that the

Performance Report for the selected measurement mode was run that day and all tests passed (see Sec-

tions 9.4 and 9.5).

61



1) Place your sample vials in the autosampler rack in the locations specified in the LabBook sample list.

2) Compare the sample list and vial locations and ensure that the vials are in the correct locations.

3) Remove the caps from the vials and either label them or place them in a location such that you will be

able to determine which cap belongs with each vial after measurements are completed.53

4) Ensure that there is nothing that might obstruct the motion of the autosampler.

5) Check that there is enough Ar gas in the gas cylinder to run your LabBook, bearing in mind that you

will use about 200 psi/hour from the gas cylinder. If not, you will need to switch off the plasma, have

the Ar gas cylinder replaced, and warm up the system again before running the LabBook.54

6) Ensure that the 10 L waste container is less than 75% full. When the peristaltic pump is on, solutions

flow at 24 mL/h. If the capacity is insufficient, ask the tool owner to empty the waste container.

7) Ensure that there is sufficient autosampler rinse solution. Typically, the container should be no less

than 25% full.55

8) If using KED mode, ensure that the CCT1 gas (He) has been flowing for at least 30 min to purge the Q-

cell and gas lines.

9) Depending upon whether an internal standard is required, either place the internal standard manual

probe into

a) the internal standard solution or

b) the carrier solution.

10) Place the other manual probe into the carrier solution.

11) Ensure that the desired LabBook is open and selected in Qtegra.

12) Run the LabBook by pressing the Schedule the LabBook button () in the toolbar. Normally, Qtegra is

configured to run the LabBook as soon as it is scheduled. If not,

a) Click Scheduler at the bottom left of the Qtegra window. The Scheduler section should expand.

b) Select the LabBook in the queue.

c) Click Run ().

53 This will help prevent cross-contamination of samples in case you wish to run them again.

54 If the plasma is extinguished for an hour or less, it should not necessary to run the Performance Report again.

55 Normally, the rinse solution is 2% nitric acid in deionized water (DIW).

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13) The LabBook should run. The current status may be observed in the status window at the bottom of

the Qtegra window.

14) After measurements commence, the Evaluation Results section will be created in the left pane of the

Qtegra window, as shown in Figure 9-17.

15) The Status column indicates the status of the measurement as follows.

a) Grey circle: Measurement has not started.

b) Green arrow: Measurement is in progress.

c) Green circle: Measurement completed successfully.

d) Red circle: Measurement started but aborted before completion.

16) Select Evaluation Results: Intensities. The Intensities window should open, as shown in Figure 9-17.

Figure 9-17: Evaluation Results: Intensities window.

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17) As measurements progress, observe the intensities and determine whether any problems are evident.

Questions to ask include:

a) Are the analyte intensities for rinse and blank solutions always low, except for internal standard

analytes? If not, there may be contamination or interferences.

b) For each analyte in each measurement, observe the plot of intensity vs. main run number, which is

displayed when the intensities of a measurement are expanded (see measurement #6 in Figure

9-17). Is there any trend in the main run intensities? Trends may indicate problems such as insuffi-

cient uptake time or wash time.

c) Are RSDs < 2%, except in cases that analytes are near background intensity values? If not, try

waiting longer for the system to stabilize, checking for trends and mitigating if present,

d) Are the intensities of any analytes in a sample very high, e.g., > 1 x 107 c/s? If so, try reducing the

analyte dwell time, changing the analyte resolution to high, or diluting the sample.

e) Are the intensities of all analytes in a sample very low? If so, try increasing the concentration of

the sample, provided that it does not make the TDS of the sample excessive. i.e., > 2%.56

f) Do the intensities of analytes in external standards change in proportion to the concentration? If

they do for high concentrations but not low concentrations, there may be contamination or inter-

ferences. If one external standard is anomalous, it may have been prepared incorrectly or the rack

and vial locations in the sample list may not match the actual location.

g) Are the analyte intensities for any sample unexpected? If so, the sample may have been prepared

incorrectly or the rack and vial locations in the sample list may not match the actual location.

18) When the LabBook has finished running, save it.

To abort a running LabBook:

1) If necessary, expand the Scheduler pane by clicking Scheduler at the bottom left of the Qtegra window.

2) Click the stop button (). You will have the option to stop immediately or at the end of the current

measurement.

56 TDS = Total Dissolved Solids. The iCAP Q requires TDS < 2% but preferably TDS < 0.2%.

64



After aborting a measurement, you may resume running any LabBook measurements, which have not al-

ready been run by clicking the Schedule the LabBook button (). You cannot re-run measurements which

have already been run or started; however, the LabBook may be edited to insert new measurements at any

desired position among the measurements that have not been run.

9.6.5.2 Manual Sampling

For manual sampling, the procedure for running a LabBook is almost identical to that using the au-

tosampler, except that you will be prompted to move the manual probes to each solution. Which probes

are moved depends upon whether or not you are using an internal standard.

With internal standards: The manual probe labelled internal standard remains in the internal standard

solution for the entire time that the LabBook is running. When prompted, move the sample probe to

the requested solution.

No internal standards: When prompted, move both manual probes to the requested solution.

9.7 Wrapping Up Measurements

1) Rinse 5-15 min using 2% nitric acid (trace metal grade or better) or deionized water before extinguish-

ing the plasma. Monitor 238U.

2) Extinguish the plasma as follows.57

a) Click on iCAP in the Instrument Control menu bar. The iCAP ribbon should open.

b) Press the Off button in the Control group on the iCAP ribbon.

3) Ensure that the autosampler is in its home position.

4) Ensure that the peristaltic pump is off.

5) Release the collar which clamps each peristaltic pump tube.

6) Release the tension on each peristaltic pump tube.

7) Ensure that the two manual probes are removed from any solution.

57 The shutdown procedure will take a few minutes.

65



8) Switch off the power to the autosampler.58

9) Wait for the message "Standby" to appear in the Log View window.59

10) Switch off the chiller pump, using the button on the front of the chiller.60

11) At the Ar gas cylinder:

a) Close the shut-off valve immediately after the pressure regulator.

b) Observe the pressure in the Ar gas cylinder.

c) Close the valve on top of the cylinder.

d) If the Ar gas cylinder pressure ≤ 500 psi, inform the tool owner.

12) Switch off the mini-environment lights.

13) Observe the liquid level in the waste tank under the iCAP Q bench. If it is more than 75% full, inform

the tool owner.

14) Observe the liquid level in the auto the autosampler probe rinse bottle on the ICAP Q bench. If it is less

than 25% full, inform the tool owner.

15) Close Qtegra.

16) Close Instrument Control.

17) Complete you log book record.

18) Complete your ticket on the 4D Labs User web site. List any supplies, which you have purchased.

9.8 Evaluation Results

9.8.1 Intensities, Concentrations, and Ratios

The Evaluation Results: Intensities window is discussed in Section 9.6.5. Main run intensity ratios, concen-

trations, and concentration ratios are displayed in a similar manner in their respective windows.

58 Rocker switch on the left side of the autosampler.

59 This indicates that shutdown of the plasma has completed.

60 The power switch at the rear of the chiller is normally left on at all times.

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9.8.2 Surveys

Intensities and concentrations measured in survey scans are displayed in tabular format in a similar manner

to main run intensities, as described in Section 9.6.5.

9.8.3 Spectra View

Evaluation Results: Spectra View displays intensities vs. mass/charge graphically for both main runs and

surveys. By selecting the corresponding button in the Spectra View Graph toolbar, data points may be dis-

played at points or sticks and intensities on a linear or logarithmic scale, as shown in Figure 9-18.

Checkboxes in the Details pane, allow one to simulate natural isotope abundances and common spectral

interferences.

Figure 9-18: Spectra View window.

9.9 Reports

After running a LabBook, various types of reports are available, a list of which may be obtained by expand-

ing the Reports list in the left pane of Qtegra. Of particular interest are the calibration curves, as shown in

Figure 9-19. Use the arrows in the toolbar of the Report Preview window move to different pages. Reports

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may be exported to .pdf or .rtf formats by clicking the Save As button in the toolbar of the Report Preview

window.

Figure 9-19: Reports window showing calibration curves.

Data may be exported to a spreadsheet, using the Export button in the Qtegra toolbar. This opens the Ex-

port Data window, shown in Figure 9-20, which allows one to select the data to be exported.

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Figure 9-20: Export Data window.

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