GB/T 17418.7-2010 Methods for analysis of noble metals in geochemical samples—Part 7:Determination of platinum group elements—By nickel sulfide fire assay-inductively coupled plasma mass spectrometry (English Version)
Methods for analysis of noble metals in geochemical samples—Part 7:Determination of platinum group elements—By nickel sulfide fire assay-inductively coupled plasma mass spectrometry
Methods for analysis of noble metals in geochemical samples - Part 7: Determination of platinum group elements - By nickel sulfide fire assay-inductively coupled plasma mass spectrometry
Warning: It has been assumed in the drafting of this part that the execution of its provisions is entrusted to appropriately qualified and experienced people. This part does not address all the safety problems. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This part of GB/T 17418 specifies the method for determination of platinum group elements by nickel sulfide fire assay-inductively coupled plasma mass spectrometry (ICP-MS) in geochemical samples.
This part is applicable to the determination of platinum, palladium, rhodium, iridium, osmium and ruthenium in geochemical samples.
See Annex A for the determination scope.
2 Normative references
The following normative documents contain provisions which, through reference in this part, constitute provisions of this part. For dated references, subsequent amendments (excluding corrections) to, or revisions, of any of these publications do not apply. However, parties to agreements based on this part are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest editions apply to this part.
GB/T 14506.1 Methods for chemical analysis of silicate rocks - Part 1: Determination of hygroscopic water content
GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods
3 Principle
The test portion is mixed with the fluxing agent in proportion and melted at 1,100℃. Noble metals are separated from other elements by nickel sulfide capture, nickel sulfide buckle is dissolved with hydrochloric acid, then filtered by suction and precipitated, filtered into a sealed sample dissolver with filter membrane, and dissolved with aqua regia. Platinum group elements are determined directly by ICP-MS, and osmium is determined by isotope dilution method. Tellurium coprecipitation method can improve the recovery and reproducibility of noble metals.
4 Reagents and solutions
Unless otherwise specified, only the recognized analytical reagents deionized water or water with equivalent purity shall be used during the analysis. The used water shall be in accordance with GB/T 6682-2008. In the blank test (7.1), if it has been detected that the content of the analytical reagent used is greater than the method detection limit of the element to be determined in this part, and it is confirmed that the determination of the low amount of the element to be determined in the test portion has been affected, the reagent shall be purified.
4.1 Borax: bake and dehydrate at 100℃, and grind it for later use.
4.2 Lithium tetraborate.
4.3 Sodium carbonate.
4.4 Nickel carbonyl: the particle size is 2.2μm to 2.8μm, and platinum group element blank test shall be conducted before use. Warning: highly toxic chemicals, handle with care.
4.5 Sublimed sulfur.
4.6 Silicon dioxide
4.7 Flour: common flour on the market.
4.8 Covering agent (1+1): well mixed borax (4.1) and sodium carbonate (4.3).
4.9 Stannous chloride solution (ρ 1mol/L): 1mol/L stannous chloride solution (3mol/L hydrochloric acid medium) is prepared by stannous chloride.
4.10 Hydrochloric acid (ρ 1.18g/mL): guaranteed reagent or high purity.
4.11 Hydrochloric acid (1+9).
4.12 Nitric acid (ρ 1.42g/mL), guaranteed reagent or high purity.
4.13 Aqua regia: prepared by hydrochloric acid (4.10) and nitric acid (4.12) in the proportion of 3+1.
Foreword i 1 Scope 2 Normative references 3 Principle 4 Reagents and solutions 5 Apparatuses 6 Specimen 7 Analytical steps 8 Calculation of result 9 Precision Annex A (Normative) Analytical isotope, method detection limit and determination range Annex B (Informative) Preparation of single element standard stock solutions Annex C (Informative) Working reference conditions of inductively coupled plasma mass spectrometer Bibliography
Standard
GB/T 17418.7-2010 Methods for analysis of noble metals in geochemical samples—Part 7:Determination of platinum group elements—By nickel sulfide fire assay-inductively coupled plasma mass spectrometry (English Version)
Standard No.
GB/T 17418.7-2010
Status
valid
Language
English
File Format
PDF
Word Count
6000 words
Price(USD)
180.0
Implemented on
2011-2-1
Delivery
via email in 1 business day
Detail of GB/T 17418.7-2010
Standard No.
GB/T 17418.7-2010
English Name
Methods for analysis of noble metals in geochemical samples—Part 7:Determination of platinum group elements—By nickel sulfide fire assay-inductively coupled plasma mass spectrometry
Methods for analysis of noble metals in geochemical samples - Part 7: Determination of platinum group elements - By nickel sulfide fire assay-inductively coupled plasma mass spectrometry
Warning: It has been assumed in the drafting of this part that the execution of its provisions is entrusted to appropriately qualified and experienced people. This part does not address all the safety problems. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This part of GB/T 17418 specifies the method for determination of platinum group elements by nickel sulfide fire assay-inductively coupled plasma mass spectrometry (ICP-MS) in geochemical samples.
This part is applicable to the determination of platinum, palladium, rhodium, iridium, osmium and ruthenium in geochemical samples.
See Annex A for the determination scope.
2 Normative references
The following normative documents contain provisions which, through reference in this part, constitute provisions of this part. For dated references, subsequent amendments (excluding corrections) to, or revisions, of any of these publications do not apply. However, parties to agreements based on this part are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest editions apply to this part.
GB/T 14506.1 Methods for chemical analysis of silicate rocks - Part 1: Determination of hygroscopic water content
GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods
3 Principle
The test portion is mixed with the fluxing agent in proportion and melted at 1,100℃. Noble metals are separated from other elements by nickel sulfide capture, nickel sulfide buckle is dissolved with hydrochloric acid, then filtered by suction and precipitated, filtered into a sealed sample dissolver with filter membrane, and dissolved with aqua regia. Platinum group elements are determined directly by ICP-MS, and osmium is determined by isotope dilution method. Tellurium coprecipitation method can improve the recovery and reproducibility of noble metals.
4 Reagents and solutions
Unless otherwise specified, only the recognized analytical reagents deionized water or water with equivalent purity shall be used during the analysis. The used water shall be in accordance with GB/T 6682-2008. In the blank test (7.1), if it has been detected that the content of the analytical reagent used is greater than the method detection limit of the element to be determined in this part, and it is confirmed that the determination of the low amount of the element to be determined in the test portion has been affected, the reagent shall be purified.
4.1 Borax: bake and dehydrate at 100℃, and grind it for later use.
4.2 Lithium tetraborate.
4.3 Sodium carbonate.
4.4 Nickel carbonyl: the particle size is 2.2μm to 2.8μm, and platinum group element blank test shall be conducted before use. Warning: highly toxic chemicals, handle with care.
4.5 Sublimed sulfur.
4.6 Silicon dioxide
4.7 Flour: common flour on the market.
4.8 Covering agent (1+1): well mixed borax (4.1) and sodium carbonate (4.3).
4.9 Stannous chloride solution (ρ 1mol/L): 1mol/L stannous chloride solution (3mol/L hydrochloric acid medium) is prepared by stannous chloride.
4.10 Hydrochloric acid (ρ 1.18g/mL): guaranteed reagent or high purity.
4.11 Hydrochloric acid (1+9).
4.12 Nitric acid (ρ 1.42g/mL), guaranteed reagent or high purity.
4.13 Aqua regia: prepared by hydrochloric acid (4.10) and nitric acid (4.12) in the proportion of 3+1.
Contents of GB/T 17418.7-2010
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and solutions
5 Apparatuses
6 Specimen
7 Analytical steps
8 Calculation of result
9 Precision
Annex A (Normative) Analytical isotope, method detection limit and determination range
Annex B (Informative) Preparation of single element standard
stock solutions
Annex C (Informative) Working reference conditions of inductively coupled plasma mass spectrometer
Bibliography
