ISO 12677:2011
Chemical analysis of refractory products by X-ray fluorescence (XRF) — Fused cast-bead method
ISO 12677:2011 specifies a method for the chemical analysis of refractory and technical ceramic raw materials, intermediates and products, by means of the X-ray fluorescence (XRF) fused cast-bead method. Typical materials that can be analysed by ISO 12677:2011 are given in Clause 3. ISO 12677:2011 is not applicable to non-oxide materials, such as silicon carbides or nitrides, etc. The method is applicable to a wide range of materials containing a wide range of elements.
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1 Scope
2 Normative references
3 Types of material
4 Principle
5 Apparatus
6 Sample grinding
7 Loss on ignition (and/or drying)
8 Flux
8.1 Choice of flux and ratio of flux to sample
8.2 Compensations for moisture in flux
9 Fusion casting procedures
9.1 Fusion of samples and casting of beads
9.1.1 Choice of procedure
9.1.2 Requirements
9.1.3 Conversion of the sample to bead form
9.1.4 Manual casting of beads
9.1.4.1 General
9.1.4.2 Cooling of beads
9.2 Automatic bead preparation
9.3 Storage
9.4 Special problems
10 Calibration
10.1 Calibration standards
10.2 Reagents and series reference materials (SeRMs)
10.2.1 Purity and preparation of reagents
10.2.2 Preparation of series reference materials (SeRMs)
10.3 Calibration using reagents
10.3.1 Calibration standards
10.3.2 Method of calibration using binary and ternary standards
10.3.2.1 General
10.3.2.2 Definition of matrix
10.3.2.3 Drift correction
10.3.2.4 Calibration standards
10.3.2.5 Calculation of calibration coefficients
10.3.2.6 Line-overlap correction standards
10.3.2.7 Line-overlap corrections
10.3.2.8 Mass-absorption correction standards
10.3.2.9 Model for mass-absorption correction coefficients
10.3.2.10 Calculation of mass-absorption correction coefficients
10.3.2.11 Criteria for determination of theoretical mass-absorption correction coefficients
10.3.3 Multi-element calibration
10.3.4 Calibration ranges
10.4 Calibration using SeRMs
10.4.1 Calibration standards
10.4.2 Calibration curve and equation
10.4.2.1 Preparation of calibration curve
10.4.2.2 Preparation of calibration equation
11 Corrections
11.1 Line-overlap correction
11.2 Background correction
11.3 Drift correction
11.4 Calculation of results
11.5 Software requirements
12 Reproducibility and repeatability
12.1 Fusion tests
12.2 Frequency of instrument tests
12.3 Maximum allowance differences of sample holders
12.4 Sample measuring positions
12.5 Instrument repeatability
12.6 Sequential systems
12.7 Dead time
12.8 Other tests
12.9 Flow gas
13 Accuracy determined by certified reference materials
13.1 Validation of synthetic calibrations
13.2 Validation of SeRM calibrations
13.3 Fresh beads of the CRMs or synthetic standards used to check SeRM calibrations
14 Definitions of limits of detection
15 Test report
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1 Scope
2 Normative references
3 Types of material
4 Principle
5 Apparatus
6 Sample grinding
7 Loss on ignition (and/or drying)
8 Flux
8.1 Choice of flux and ratio of flux to sample
8.2 Compensations for moisture in flux
9 Fusion casting procedures
9.1 Fusion of samples and casting of beads
9.1.1 Choice of procedure
9.1.2 Requirements
9.1.3 Conversion of the sample to bead form
9.1.4 Manual casting of beads
9.1.4.1 General
9.1.4.2 Cooling of beads
9.2 Automatic bead preparation
9.3 Storage
9.4 Special problems
10 Calibration
10.1 Calibration standards
10.2 Reagents and series reference materials (SeRMs)
10.2.1 Purity and preparation of reagents
10.2.2 Preparation of series reference materials (SeRMs)
10.3 Calibration using reagents
10.3.1 Calibration standards
10.3.2 Method of calibration using binary and ternary standards
10.3.2.1 General
10.3.2.2 Definition of matrix
10.3.2.3 Drift correction
10.3.2.4 Calibration standards
10.3.2.5 Calculation of calibration coefficients
10.3.2.6 Line-overlap correction standards
10.3.2.7 Line-overlap corrections
10.3.2.8 Mass-absorption correction standards
10.3.2.9 Model for mass-absorption correction coefficients
10.3.2.10 Calculation of mass-absorption correction coefficients
10.3.2.11 Criteria for determination of theoretical mass-absorption correction coefficients
10.3.3 Multi-element calibration
10.3.4 Calibration ranges
10.4 Calibration using SeRMs
10.4.1 Calibration standards
10.4.2 Calibration curve and equation
10.4.2.1 Preparation of calibration curve
10.4.2.2 Preparation of calibration equation
11 Corrections
11.1 Line-overlap correction
11.2 Background correction
11.3 Drift correction
11.4 Calculation of results
11.5 Software requirements
12 Reproducibility and repeatability
12.1 Fusion tests
12.2 Frequency of instrument tests
12.3 Maximum allowance differences of sample holders
12.4 Sample measuring positions
12.5 Instrument repeatability
12.6 Sequential systems
12.7 Dead time
12.8 Other tests
12.9 Flow gas
13 Accuracy determined by certified reference materials
13.1 Validation of synthetic calibrations
13.2 Validation of SeRM calibrations
13.3 Fresh beads of the CRMs or synthetic standards used to check SeRM calibrations
14 Definitions of limits of detection
15 Test report