ISO 16962:2017
Surface chemical analysis — Analysis of zinc- and/or aluminium-based metallic coatings by glow-discharge optical-emission spectrometry
ISO 16962:2017 specifies a glow-discharge optical-emission spectrometric method for the determination of the thickness, mass per unit area and chemical composition of metallic surface coatings consisting of zinc- and/or aluminium-based materials. The alloying elements considered are nickel, iron, silicon, lead and antimony.
This method is applicable to zinc contents between 0,01 mass % and 100 mass %; aluminium contents between 0,01 mass % and 100 mass %; nickel contents between 0,01 mass % and 20 mass %; iron contents between 0,01 mass % and 20 mass %; silicon contents between 0,01 mass % and 15 mass %; magnesium contents between 0,01 mass% and 20 mass%; lead contents between 0,005 mass % and 2 mass %, antimony contents between 0,005 mass % and 2 mass %.
NOTE Due to environmental and health risks, lead and antimony are avoided nowadays, but this document is also applicable to older products including these elements.
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Apparatus
5.1 Glow-discharge optical-emission spectrometer
5.1.1 General
5.1.2 Selection of spectral lines
5.1.3 Selection of glow-discharge source type
6 Adjusting the glow-discharge spectrometer system settings
6.1 General
6.2 Setting the parameters of a DC source
6.2.1 Constant applied current and voltage
6.2.2 Constant applied current and pressure
6.2.3 Constant voltage and pressure
6.3 Setting the discharge parameters of an RF source
6.3.1 General
6.3.2 Constant applied power and pressure
6.3.3 Constant applied power and DC bias voltage
6.3.4 Constant effective power and effective RF voltage
6.4 Minimum performance requirements
6.4.1 General
6.4.2 Minimum repeatability
6.4.3 Detection limit
7 Sampling
8 Calibration
8.1 General
8.2 Calibration samples
8.2.1 General
8.2.2 Brass calibration samples
8.2.3 Zn-Al alloy samples
8.2.4 Low alloy iron or steel samples
8.2.5 Stainless steel samples
8.2.6 Nickel alloy samples
8.2.7 Aluminium-silicon alloy samples
8.2.8 Aluminium-magnesium alloy samples
8.2.9 High-purity copper and zinc samples
8.3 Validation samples and optional RMs for calibration
8.3.1 General
8.3.2 Zinc-nickel electrolytically coated RM
8.3.3 Zinc-iron electrolytically coated RM
8.3.4 Zinc-aluminium hot dip coated RM
8.3.5 Zinc-iron hot dip coated and annealed RM
8.4 Determination of the sputtering rate of calibration and validation specimens
8.5 Emission intensity measurements of calibration specimens
8.6 Calculation of calibration equations
8.7 Validation using reference materials
8.7.1 General
8.7.2 Checking analytical accuracy using bulk reference materials
8.7.3 Checking analytical accuracy using surface layer reference materials
8.8 Verification and drift correction
9 Analysis of test specimens
9.1 Adjusting discharge parameters
9.2 Setting of measuring time and data acquisition rate
9.3 Quantifying depth profiles of test specimens
10 Expression of results
10.1 Expression of quantitative depth profile
10.2 Determination of total coating mass per unit area (coating aeric mass)
10.2.1 General method
10.2.2 Method for special applications
10.3 Determination of average mass fractions
11 Precision
12 Test report
Annex A (normative) Calculation of calibration constants and quantitative evaluation of depth profiles
Annex B (informative) Suggestions concerning suitable spectral lines
Annex C (informative) Determination of coating mass per unit area (coating areic mass)
Annex D (informative) Additional information on international cooperative tests
Bibliography
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Apparatus
5.1 Glow-discharge optical-emission spectrometer
5.1.1 General
5.1.2 Selection of spectral lines
5.1.3 Selection of glow-discharge source type
6 Adjusting the glow-discharge spectrometer system settings
6.1 General
6.2 Setting the parameters of a DC source
6.2.1 Constant applied current and voltage
6.2.2 Constant applied current and pressure
6.2.3 Constant voltage and pressure
6.3 Setting the discharge parameters of an RF source
6.3.1 General
6.3.2 Constant applied power and pressure
6.3.3 Constant applied power and DC bias voltage
6.3.4 Constant effective power and effective RF voltage
6.4 Minimum performance requirements
6.4.1 General
6.4.2 Minimum repeatability
6.4.3 Detection limit
7 Sampling
8 Calibration
8.1 General
8.2 Calibration samples
8.2.1 General
8.2.2 Brass calibration samples
8.2.3 Zn-Al alloy samples
8.2.4 Low alloy iron or steel samples
8.2.5 Stainless steel samples
8.2.6 Nickel alloy samples
8.2.7 Aluminium-silicon alloy samples
8.2.8 Aluminium-magnesium alloy samples
8.2.9 High-purity copper and zinc samples
8.3 Validation samples and optional RMs for calibration
8.3.1 General
8.3.2 Zinc-nickel electrolytically coated RM
8.3.3 Zinc-iron electrolytically coated RM
8.3.4 Zinc-aluminium hot dip coated RM
8.3.5 Zinc-iron hot dip coated and annealed RM
8.4 Determination of the sputtering rate of calibration and validation specimens
8.5 Emission intensity measurements of calibration specimens
8.6 Calculation of calibration equations
8.7 Validation using reference materials
8.7.1 General
8.7.2 Checking analytical accuracy using bulk reference materials
8.7.3 Checking analytical accuracy using surface layer reference materials
8.8 Verification and drift correction
9 Analysis of test specimens
9.1 Adjusting discharge parameters
9.2 Setting of measuring time and data acquisition rate
9.3 Quantifying depth profiles of test specimens
10 Expression of results
10.1 Expression of quantitative depth profile
10.2 Determination of total coating mass per unit area (coating aeric mass)
10.2.1 General method
10.2.2 Method for special applications
10.3 Determination of average mass fractions
11 Precision
12 Test report
Annex A (normative) Calculation of calibration constants and quantitative evaluation of depth profiles
Annex B (informative) Suggestions concerning suitable spectral lines
Annex C (informative) Determination of coating mass per unit area (coating areic mass)
Annex D (informative) Additional information on international cooperative tests
Bibliography