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