YS/T 252.1-2007 English PDF (YST252.1-2007)

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YS/T 252.1-2007: Methods for chemical analysis of nickel matte. Determination of nickel content. Dimethylglyoxime gravimetric method
YS/T 252.1-2007
YS
NONFERROUS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.40
H 13
Replacing YS/T 252.1-1994
Methods for chemical analysis of nickel matte -
Determination of nickel content - Dimethylglyoxime
gravimetric method
ISSUED ON: APRIL 13, 2007
IMPLEMENTED ON: OCTOBER 01, 2007
Issued by: National Development and Reform Commission of PRC
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method summary ... 5
3 Reagents ... 5
4 Instruments ... 6
5 Analytical procedures ... 7
6 Calculation and expression of analysis results ... 8
7 Precision ... 9
8 Quality assurance and control ... 10
Foreword
YS/T 252 "Methods for chemical analysis of nickel matte" is divided into five parts:
YS/T 252.1 Methods for chemical analysis of nickel matte - Determination of nickel
content - Dimethylglyoxime gravimetric method
YS/T 252.2 Methods for chemical analysis of nickel matte - Determination of iron
content - Sulfosalicylic acid photometric method
YS/T 252.3 Methods for chemical analysis of nickel matte - Determination of cobalt
content - Flame atomic absorption spectrometric method
YS/T 252.4 Methods for chemical analysis of nickel matte - Determination of cobalt
content - Sodium thiosulphate titrimetric method
YS/T 252.5 Methods for chemical analysis of nickel matte - Determination of sulfur
content - Combustion-neutralization titrimetric method
This Part is Part 1.
This Part replaces YS/T 252.1-1994 "Determination of nickel content by
dimethylglyoxime gravimetric method". Compared with YS/T 252.1-1994, this Part
mainly has the following changes:
- ADJUST the measurement range from 45.00% ~ 70.00% to 20% ~ 80%;
- CHANGE the acidity of the solution from pH7 ~ pH8 to pH8 ~ pH9 during
precipitation;
- CANCEL Appendix A: Determination of nickel amount by EDTA titration method;
- ADD the determination of nickel content in the filtrate by dimethylglyoxime
gravimetric method;
- ADD the repeatability limits, supplementing quality assurance and control terms.
This Part was proposed by AND shall be under the jurisdiction of the National Technical
Committee for Standardization of Nonferrous Metals.
Responsible drafting organization of this Part: Jinchuan Group Co., Ltd.
Participated drafting organization of this Part: Beijing General Research Institute of
Mining and Metallurgy, Guangzhou Nonferrous Metals Research Institute.
The main drafters of this Part: Liu Haidong, Yu Shengjie, Lv Qingcheng, Lin Xiuying,
Zhao Junfeng, Zhu Yuqiang.
Methods for chemical analysis of nickel matte -
Determination of nickel content - Dimethylglyoxime
gravimetric method
1 Scope
This Part specifies the method for determination of nickel content in high nickel matte.
This Part is applicable to the determination of nickel content in high-nickel matte.
Measuring range: 20% ~ 80%.
2 Method summary
The sample is decomposed with hydrochloric acid or nitric acid-potassium chlorate
saturated solution. In the ammonia medium, nickel and diacetyl oxime form a red nickel
diacetyl oxime precipitate, which is separated from other impurity elements. The
precipitate is filtered, washed, and dried to constant weight; the amount of nickel is
calculated. The amount of nickel in the mixed filtrate is extracted with chloroform under
pH6.5, separated from other impurities, measured using diacetyl oxime
spectrophotometry and then corrected.
3 Reagents
3.1 Hydrochloric acid (ρ1.19 g/mL).
3.2 Hydrochloric acid (1 + 1).
3.3 Hydrochloric acid (1 + 24).
3.4 Nitric acid (ρ1.42 g/mL).
3.5 Nitric acid (1 + 1).
3.6 Sulfuric acid (ρ1.83 g/mL).
3.7 Ammonia (1 + 1).
3.8 Chloroform.
3.9 Nitric acid-potassium chlorate saturated solution: Dissolve potassium chlorate in
nitric acid (3.4) until saturated.
3.10 Potassium sodium tartrate solution (200 g/L), filter it before use.
3.11 Ammonium acetate solution (200 g/L), filter it before use.
3.12 Sodium thiosulfate solution (200 g/L), filter it before use.
3.13 Dimethylglyoxime ethanol solution (10 g/L), filter it before use.
3.14 Dimethylglyoxime-sodium hydroxide solution (10 g/L): Dissolve 15 g of sodium
hydroxide in 100 mL of water. After cooling to room temperature, dissolve 1 g of
dimethylglyoxime in the solution. Mix well.
3.15 Ferric persulfate solution (50 g/L).
3.16 Nickel standard stock solution:
Weigh 0.1000 g of metallic nickel (the mass fraction of nickel is ≥ 99.95%). Place it in
a 400 mL beaker. Add 10 mL of nitric acid (3.5). Cover it with a watch glass. Dissolve
it completely at low temperature. Add 2 mL of sulfuric acid (3.6). Continue heating
until a large amount of white smoke is gone. Cool down. Rinse the watch glass and cup
wall with water. Heat to dissolve the salts. Cool to room temperature. Transfer to a 1000
mL volumetric flask. Use water to make the volume reach the mark. 1 mL of this
solution contains 100 μg of nickel.
3.17 Nickel standard solution:
Pipette 10.00 mL of nickel standard storage solution (3.16) into a 200 mL volumetric
flask. Use water to make the volume reach the mark. 1 mL of this solution contains 5
μg of nickel.
4 Instruments
4.1 Spectrophotometer.
4.2 Electric constant temperature water bath.
4.3 Electric constant temperature drying oven.
4.4 Glass sand core crucible, G4 (pore diameter 7 μm ~ 16 μm/5 μm ~ 15 μm).
4.5 Suction filter bottle.
5.4.1 Collect the filtrate from 5.3.3. Cool it. Transfer it into a 500 mL or 1000 mL
volumetric flask depending on the volume. Use water to make the volume reach to the
mark.
5.4.2 Dispense 100.00 mL of the mixed filtrate (5.4.1) into a 250 mL separatory funnel.
Use hydrochloric acid (3.2) and ammonia water (3.7) to adjust the pH of the solution to
about 6.5. Add 15 mL of chloroform (3.8). Shake for 2 minutes. Let it stand for 5
minutes. After layering, move the organic phase into another separatory funnel. Add 15
mL of chloroform (3.8) to the aqueous phase, to repeat the extraction once. Combine
the organic phases. Discard the aqueous phase.
5.4.3 Add 15 mL hydrochloric acid (3.3) to the organic phase (5.4.2). Shake for 1 minute.
Let it stand for stratification. Transfer the organic phase into another separatory funnel.
Add 15 mL of hydrochloric acid (3.3) for back extraction once. Combine the aqueous
phase in a 100 mL beaker.
5.4.4 Heat the solution (5.4.3) in the beaker at low temperature, to evaporate to a volume
of about 2 mL. Remove to cool it. Add 2 mL of nitric acid (3.4). Continue heating and
evaporate to dryness. Cool it. Add hydrochloric acid (3.2) and heat slightly to dissolve
the salts. After cooling, transfer it into a 50 mL volumetric flask.
5.4.5 Add 5 mL of persulfate lock solution (3.15) and 5 mL of dimethylglyoxime-
sodium hydroxide solution (3.14). Mix well. Let it stand for 10 minutes. Use water to
make the volume reach to the mark.
5.4.6 Pipette part of the test solution (5.4.5) into a 1 cm cuvette. Use the reagent blank
as a reference, to measure the absorbance at the wavelength of 510 nm on the
spectrophotometer. Find out the corresponding nickel amount from the working curve.
5.4.7 Drawing of working curve:
Pipette 0.00 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL of nickel standard
solutions (3.17). Place them in a set of 50 mL volumetric flasks, respectively. Proceed
the following steps in accordance with (5.4.5). Using the reagent blank as a reference,
measure the absorbance at the wavelength of 510 nm wi...