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YS/T 252.3-2007Methods for chemical analysis of nickel matte. Determination of cobalt content. Flame atomic absorption spectrometric method (English PDF)

高镍锍化学分析方法钴量的测定火焰原子吸收光谱法

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Issued by

National Development and Reform Commission of PRC

Level / Type

National · Recommended

Issue date

April 13, 2007

Implementation date

October 1, 2007

Scope

YS/T 252.3-2007 is the English-translated version of 高镍锍化学分析方法钴量的测定火焰原子吸收光谱法.

YS/T 252.3-2007 — This Part specifies the method for determination of cobalt content in high nickel matte. This Part is applicable to the determination of cobalt content in high-nickel matte. Measuring range: 0.1% ~ 2%.

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Document preview — YS/T 252.3-2007

National Standard of the People's Republic of China

ICS
77.120.40
Classification
H 13

Issued by: National Development and Reform Commission of PRC

Contents

  • Foreword...3
  • 1 Scope...5
  • 2 Method summary...5
  • 3 Reagents...5
  • 4 Instruments...6
  • 5 Analytical procedures...6
  • 6 Calculation and expression of analysis results...7
  • 7 Precision...8
  • 8 Quality assurance and control...8

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 3.

This Part replaces YS/T 252.3-1994 "Determination of cobalt content by sulfosalicylic

acid photometric method". Compared with YS/T 252.3-1994, this Part mainly has the

following changes:

- CHANGE the measurement method from sulfosalicylic acid photometric method

to flame atomic absorption spectrometry;

- ADJUST the measurement range from 0.30% ~ 1.50% to 0.1% ~ 2%;

- 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.

1 Scope

This Part specifies the method for determination of cobalt content in high nickel matte.

This Part is applicable to the determination of cobalt content in high-nickel matte.

Measuring range: 0.1% ~ 2%.

2 Method summary

Decompose the sample with hydrochloric acid, nitric acid-potassium chlorate saturated

solution. Use air-acetylene flame in hydrochloric acid (2 + 98) medium, to measure the

absorbance at the wavelength of 240.7 nm of atomic absorption spectrometer, after

subtracting the background. Calculate the cobalt content according to the standard curve

method.

3 Reagents

3.1 Hydrochloric acid (rho1.19 g/mL).

3.2 Nitric acid (rho1.42 g/mL).

3.3 Nitric acid (1 + 1).

3.4 Ammonia (1 + 3).

3.5 Nitric acid-potassium chlorate saturated solution: Dissolve potassium chlorate in

nitric acid (3.2) until saturated.

3.6 Cobalt standard storage solution: Weigh 1.0000 g of metallic cobalt (mass fraction

of cobalt >= 99.95%). Slowly add 20 mL of nitric acid (3.3) into a 400 mL beaker. Cover

with a watch glass. Heat at low temperature to completely dissolve. Remove it. Use

water to rinse the watch glass and cup wall. Heat and boil to remove nitrogen oxides.

Remove it. Cool to room temperature. Transfer it into a 1000 mL volumetric flask. Use

water to wash the watch glass and cup wall. Combine the washing liquid into the

volumetric flask. Use water to make the volume reach to the mark. 1 mL of this solution

contains 1 mg of cobalt.

3.7 Cobalt standard solution: Pipette 20.00 mL of cobalt standard storage solution (3.6)

into a 200 mL volumetric flask. Make the volume reach to the mark. 1 mL of this

solution contains 100 µg of cobalt.

4 Instruments

Atomic absorption spectrometer (with background subtraction function), equipped with

cobalt hollow cathode lamp.

Under the best working conditions of the instrument, those that can meet the following

indicators can be used.

Characteristic concentration: In a solution that is basically consistent with the

measurement test solution, the characteristic concentration of cobalt shall not be greater

than 0.06 µg/mL.

Precision: Use the highest concentration standard solution to make 10 measurements of

the absorbance; the standard deviation shall not exceed 1.0% of the average absorbance.

Use the lowest concentration standard solution (not the "zero" standard solution) to

make 10 measurements of the absorbance; the standard deviation shall not exceed 0.5%

of the average absorbance of the highest concentration standard solution.

Linearity of the working curve: Divide the working curve into five equal segments

according to concentration. The ratio -- of the absorbance difference of the highest

segment to the absorbance difference of the lowest segment -- shall not be less than

0.85.

5 Analytical procedures

5.1 Sample

Weigh 0.400 g of specimen, accurate to 0.0001 g.

5.2 Blank test

Do a blank test along with the sample.

5.3 Determination

5.3.1 Place the sample (5.1) in a 400 mL beaker. Moisten it with a small amount of

water. Add 10 mL of hydrochloric acid (3.1). Cover with a watch glass. Dissolve at low

temperature and evaporate to a volume of about 2 mL. Cool it. Add 20 mL of saturated

nitric acid-potassium chlorate solution (3.5). Continue to heat to dissolve and evaporate

to a volume of 2 mL ~ 3 mL. Cool it. Wash the watch glass and cup wall with about 20

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 8 pages — is available in the English PDF.

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