GB/T 21933.1-2008 Ferronickel - Determination of nickel content - The dimethylglyoxime gravimetric method
WARNING: Persons using this part shall be familiar with normal laboratory practice. This part does not purport to address all of the safety concerns, if any, associated with its use. Users shall be responsible for taking appropriate safety and health measures and ensuring conformity to the conditions stipulated by relevant national regulations of China.
1 Scope
This part of GB/T 21933 specifies a dimethylglyoxime gravimetric method for the determination of the nickel content of ferronickel.
This part is applicable to the determination of the nickel content of ferronickel in the range 15% to 60 % (mass fraction).
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of GB/T 21933. For dated references, subsequent amendments (excluding corrections) to, or revisions of, any of these publications do not apply to this part of GB/T 21933. However parties to agreements based on this part of GB/T 21933 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies.
GB/T 12805 Laboratory glassware - Burettes
GB/T 12806 Laboratory glassware - One-mark volumetric flasks
GB/T 12808 Laboratory glassware - One mark pipettes
GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions (GB/T 6379.1-2004, ISO 5725-1:1994, IDT)
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method (GB/T 6379.2-2004, ISO 5725-2:1994, IDT)
GB/T 11415-1989 Laboratory sintered (fritted) filters-Porosity grading, classification and designation
3 Principle
Dissolution of a test portion in nitric acid. Precipitation of silica by dehydration in perchloric acid. Removal of silica by filtration. Precipitation of nickel from a tartro-ammoniacal medium by an ethanolic solution of dimethylglyoxime. A second precipitation of nickel and weighing after drying at 150℃. Determination of residual nickel in the filtrates by atomic absorption spectrometry.
4 Reagents and materials
Unless otherwise stated, only the recognized analytical reagents and distilled water or deionized water or water with equivalent purity shall be used during the analysis.
4.1 Hydrochloric acid, ρ1.19 g/mL.
4.2 Ammonia, ρ0.925g/mL.
4.3 Nitric acid, ρ1.42g/mL.
4.4 Perchloric acid, ρ1.67g/mL.
4.5 Hydrofluoric acid, ρ1.13g/mL.
4.6 Acetic acid, ρ1.05g/mL.
Contents
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Apparatus
6 Sampling and preparation of samples
7 Analytical procedure
8 Expression of results
9 Test report
Annex A (Normative) Determination of nickel in combined filtrates by atomic absorption spectrometry
Annex B (Informative) Statistical report of interlaboratory tests
GB/T 21933.1-2008 Ferronickel - Determination of nickel content - The dimethylglyoxime gravimetric method
WARNING: Persons using this part shall be familiar with normal laboratory practice. This part does not purport to address all of the safety concerns, if any, associated with its use. Users shall be responsible for taking appropriate safety and health measures and ensuring conformity to the conditions stipulated by relevant national regulations of China.
1 Scope
This part of GB/T 21933 specifies a dimethylglyoxime gravimetric method for the determination of the nickel content of ferronickel.
This part is applicable to the determination of the nickel content of ferronickel in the range 15% to 60 % (mass fraction).
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of GB/T 21933. For dated references, subsequent amendments (excluding corrections) to, or revisions of, any of these publications do not apply to this part of GB/T 21933. However parties to agreements based on this part of GB/T 21933 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies.
GB/T 12805 Laboratory glassware - Burettes
GB/T 12806 Laboratory glassware - One-mark volumetric flasks
GB/T 12808 Laboratory glassware - One mark pipettes
GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions (GB/T 6379.1-2004, ISO 5725-1:1994, IDT)
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method (GB/T 6379.2-2004, ISO 5725-2:1994, IDT)
GB/T 11415-1989 Laboratory sintered (fritted) filters-Porosity grading, classification and designation
3 Principle
Dissolution of a test portion in nitric acid. Precipitation of silica by dehydration in perchloric acid. Removal of silica by filtration. Precipitation of nickel from a tartro-ammoniacal medium by an ethanolic solution of dimethylglyoxime. A second precipitation of nickel and weighing after drying at 150℃. Determination of residual nickel in the filtrates by atomic absorption spectrometry.
4 Reagents and materials
Unless otherwise stated, only the recognized analytical reagents and distilled water or deionized water or water with equivalent purity shall be used during the analysis.
4.1 Hydrochloric acid, ρ1.19 g/mL.
4.2 Ammonia, ρ0.925g/mL.
4.3 Nitric acid, ρ1.42g/mL.
4.4 Perchloric acid, ρ1.67g/mL.
4.5 Hydrofluoric acid, ρ1.13g/mL.
4.6 Acetic acid, ρ1.05g/mL.
Contents of GB/T 21933.1-2008
Contents
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Apparatus
6 Sampling and preparation of samples
7 Analytical procedure
8 Expression of results
9 Test report
Annex A (Normative) Determination of nickel in combined filtrates by atomic absorption spectrometry
Annex B (Informative) Statistical report of interlaboratory tests