AS 4873.1-2005

Recommended practice for inductively coupled plasma-mass spectrometry (ICP-MS) Principles and techniques

Standards Australia

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1 - AS 4873.1-2005 RECOMMENDED PRACTICE FOR INDUCTIVELY COUPLED PLASMA-MASS SPECTROMETRY (ICP-MS) - PRINCIPLES AND TECHNIQUES
4 - PREFACE
5 - CONTENTS
7 - SECTION 1 SCOPE AND GENERAL
7 - 1.1 SCOPE
7 - ¿1.2 REFERENCED DOCUMENTS¿
8 - 1.3 DEFINITIONS
8 - 1.3.1 Accuracy
8 - 1.3.2 Analyte
8 - 1.3.3 Blank reagent solution
8 - 1.3.4 Blank sample solution
8 - 1.3.5 Blank calibration solution
8 - 1.3.6 Calibration solution
8 - 1.3.7 Check calibration solution
8 - 1.3.8 Concentration (C)
8 - 1.3.9 Determination
8 - 1.3.10 Interference check solutions
9 - 1.3.11 Instrument detection limit (IDL)
9 - 1.3.12 Isobaric interference
9 - 1.3.13 Laboratory sample
9 - 1.3.14 Linearity
9 - 1.3.15 Linearity verification solution
9 - 1.3.16 Mass discrimination effects
9 - 1.3.17 Mean result
9 - 1.3.18 Method detection limit (MDL)
9 - 1.3.19 Net intensity (I)
9 - 1.3.20 Net intensity ratio (IR)
9 - 1.3.21 Outer flow
9 - 1.3.22 Polyatomic interferences
9 - 1.3.23 Practical quantitation limit (PQL)
9 - 1.3.24 Precision
10 - 1.3.25 Pure chemical
10 - 1.3.26 Raw intensity (Iraw)
10 - 1.3.27 Repeatability (r)
10 - 1.3.28 Repeatability conditions
10 - 1.3.29 Reproducibility (R)
10 - 1.3.30 Reproducibility conditions
10 - 1.3.31 Reproducibility limit
10 - 1.3.32 Reproducibility standard deviation
10 - 1.3.33 Result
10 - 1.3.34 Sensitivity (S)
10 - 1.3.35 Stock solution
10 - 1.3.36 Test portion
11 - 1.3.37 Test sample
11 - 1.3.38 Test sample solution
11 - 1.3.39 Uncertainty of measurement
11 - 1.3.40 Unified atomic mass unit (u)
11 - 1.4 PRINCIPLE
11 - 1.5 SAFETY PRECAUTIONS
11 - 1.5.1 General
11 - 1.5.2 Ultraviolet radiation
11 - 1.5.3 Exhaust extraction system
11 - 1.5.4 Radiofrequency leakage
13 - SECTION 2 INSTRUMENTATION
13 - 2.1 GENERAL
13 - 2.2 SAMPLE INTRODUCTION
13 - 2.2.1 General
14 - 2.2.2 Sample pump
14 - 2.2.3 Nebulizer
15 - 2.2.4 Spray chamber
15 - 2.2.5 Alternative sample introduction systems
16 - 2.3 TORCH AND PLASMA
17 - 2.4 GAS AND GAS CONTROL
17 - 2.5 GENERATOR
18 - 2.6 TRANSFER OF THE IONS TO THE MASS SPECTROMETER
19 - 2.7 THE MASS SPECTROMETER
19 - 2.7.1 General
19 - 2.7.2 Ion optics system
19 - 2.7.3 Mass analysers
21 - 2.7.4 The detector
22 - 2.8 SIGNAL PROCESSING AND INSTRUMENT CONTROL
24 - SECTION 3 INTERFERENCES BY CONCOMITANTS
24 - 3.1 GENERAL
24 - 3.2 SPECTRAL INTERFERENCES
24 - 3.2.1 General
24 - 3.2.2 Possible remedies for polyatomic ion interference
25 - 3.2.3 Correction equations
27 - 3.3 NON-SPECTRAL INTERFERENCES
27 - 3.3.1 General
27 - 3.3.2 Interferences in the nebulization process
28 - 3.3.3 Interferences in the plasma
29 - 3.3.4 Interferences in the interface/ion optics
29 - 3.3.5 Possible remedies for non-spectral interferences (matrix effects)
33 - SECTION 4 OPTIMIZATION OF THE INSTRUMENT
33 - 4.1 GENERAL
33 - 4.2 PRELIMINARY INSPECTION
33 - 4.3 OPTIMIZING THE INSTRUMENT
33 - 4.3.1 General
33 - 4.3.2 Alignment of the plasma
33 - 4.3.3 Mass calibration
34 - 4.3.4 Resolution
34 - 4.3.5 Detector settings
35 - 4.3.6 Ion optics
35 - 4.3.7 Plasma gas flows
35 - 4.4 VERIFICATION OF INSTRUMENT PERFORMANCE CRITERIA
35 - 4.5 INSTRUMENT DETECTION LIMIT
36 - 4.6 MEASUREMENT STABILITY
37 - SECTION 5 METHOD DEVELOPMENT
37 - 5.1 GENERAL
37 - 5.2 CHOICE OF ISOTOPES
38 - 5.3 CHOICE OF INSTRUMENT SETTINGS
38 - 5.3.1 General
38 - 5.3.2 General remarks on the effects of instrument parameters
39 - 5.3.3 Effect of the temperature of the sampled plasma on sensitivity
39 - 5.3.4 Effects of RF power on sensitivity through plasma potential
39 - 5.3.5 Effect of the temperature of the sampled plasma on interferences
40 - 5.3.6 Effect of inner gas flow rate
40 - 5.3.7 Effect of sampling depth
40 - 5.3.8 Effect of sample uptake rate
40 - 5.3.9 Choice of rinsing time
40 - 5.3.10 Memory effects
41 - 5.4 CHOICE OF INTEGRATION TIME
41 - 5.5 CHOICE OF REFERENCE ELEMENTS
42 - 5.6 LINEARITY AND WORKING RANGE
42 - 5.7 COMPOSITION OF CALIBRATION SOLUTIONS
42 - 5.8 METHOD DEVELOPMENT FOR SPECIALIZED APPLICATIONS
43 - 5.9 DETERMINATION OF THE METHOD PERFORMANCE
43 - 5.9.1 General
43 - 5.9.2 Method detection limit (MDL)
45 - 5.9.3 Precision of the method
45 - 5.9.4 Method validation
46 - SECTION 6 ANALYSIS
46 - 6.1 CALIBRATION
46 - 6.2 SOLUTIONS TO BE PREPARED
48 - 6.3 MEASUREMENT
48 - 6.3.1 General
49 - 6.3.2 Preparing the instrument
49 - 6.3.3 Checking the interference factors
49 - 6.3.4 Measurements
49 - 6.3.5 Analyte addition measurements
51 - SECTION 7 ANALYTICAL QUALITY ASSURANCE
51 - 7.1 GENERAL
51 - 7.2 INSTRUMENT CALIBRATION AND OPTIMIZATION
51 - 7.3 VALIDATION OF ANALYTICAL PROCEDURE
51 - 7.3.1 Traceability of samples
51 - 7.3.2 Documentation of analytical methods
51 - 7.3.3 Monitoring of analytical performance
52 - 7.4 TREATMENT OF DATA FROM MONITORING PROCEDURE
52 - 7.5 TRACEABILITY OF RESULTS
52 - 7.6 CORRECTIVE ACTION
53 - APPENDIX A - SPECTRAL INTERFERENCES, CHOICE OF ISOTOPES AND METHOD DETECTION LIMITS FOR QUADRUPOLE ICP-MS INSTRUMENTS
61 - APPENDIX B - BIBLIOGRAPHY
62 - APPENDIX C - GLOSSARY OF TERMS
62 - C1 GLOSSARY
76 - C2 REFERENCES

Abstract

Sets out principles, techniques and operating procedures involved in the setting up and operation of inductively coupled plasma mass spectrometry for the use of chemical methods of analysis.

Scope

This Standard sets out recommendations and operating procedures in the application of inductively coupled plasma-mass spectrometry (ICP-MS) to chemical analysis. This Standard refers principally to quadrupole based instruments, but some clauses are applicable to other types of ICP-MS instruments such as magnetic sector and time-of-flight mass spectrometers.
This Standard should be read in conjunction with the instrument manufacturers recommendations and AS3641.1.
An overview of possible spectral interferences is given in AppendixA.