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YS/T 953.1-2014Methods for chemical analysis of fire smelting nickel substrate material - Part 1: Determination of nickel content - Dimethylglyoxime spectrophotometric method and dimethylglyoxime gravimetric method (English PDF)

火法冶炼镍基体料化学分析方法第1部分：镍量的测定丁二酮肟分光光光度法和丁二酮肟重量法

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Issued by

Ministry of Industry and Information Technology of the PRC

Level / Type

National · Recommended

Issue date

October 14, 2014

Implementation date

April 1, 2015

Scope

YS/T 953.1-2014 is the English-translated version of 火法冶炼镍基体料化学分析方法第1部分：镍量的测定丁二酮肟分光光光度法和丁二酮肟重量法.

YS/T 953.1-2014 — This Part of YS/T 953 specifies the dimethylglyoxime spectrophotometric method and dimethylglyoxime gravimetric method for the determination of nickel content in the fire smelting nickel substrate material.

This Part applies to the determination of nickel content in the fire smelting nickel substrate material. The determination range of Method 1 is 0.50%~5.00%. The determination range of Method 2 is 1.00%~25.00%.

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Document preview — YS/T 953.1-2014

National Standard of the People's Republic of China

ICS: 77.120.40
Classification: H 13

Issued by: Ministry of Industry and Information Technology of the PRC

Foreword...3
1 Scope...5
2 Normative references...5
3 Method 1 - Dimethylglyoxime spectrophotometric method...5
4 Method 2 - Dimethylglyoxime gravimetric method...9
5 Test report...12

Foreword

YS/T 953 "Methods for chemical analysis of fire smelting nickel substrate

material" is divided into 11 parts.

- Part 1.Determination of nickel content - Dimethylglyoxime

spectrophotometric method and dimethylglyoxime gravimetric method;

- Part 2.Determination of silicon content - Molybdosilicate blue

spectrophotometric method and perchloric acid dehydration gravimetric

method;

- Part 3.Determination of phosphorus content - Bismuth phosphomolybdate

blue spectrophotometric method;

- Part 4.Determination of chrome content - Ammonium ferrous sulfate

titration method;

- Part 5.Determination of manganese content - Potassium periodate

spectrophotometric method;

- Part 6.Determination of cobalt content - 5-CI-PADAB spectrophotometric

method and flame atomic absorption spectrometric method;

- Part 7.Determination of copper content - BCO spectrophotometric method

and flame atomic absorption spectrometric method;

- Part 8.Determination of iron content - Titanium trichloride reduction-

potassium dichromate titrimetric method;

- Part 9.Determination of carbon and sulfur contents - Infrared absorption

method after high frequency combustion;

- Part 10.Determination of nickel, chromium, manganese, cobalt, copper and

phosphorus contents - Inductively coupled plasma atomic emission

spectrometric method;

- Part 11.Determination of Lead, Arsenic, Cadmium and Mercury contents -

Inductively coupled plasma-mass spectrometric method.

This Part is Part 1 of YS/T 953.Method 2 is the arbitration method.

This Part is drafted in accordance with the rules given in GB/T 1.1-2009.

This Part shall be under the jurisdiction of National Technical Committee 243

on Nonferrous Metals of Standardization Administration of China (SAC/TC 243).

Responsible drafting organization of this Part. Zhongbao Binhai Nickel Industry

Co., Ltd.

Drafting organizations of Method 1 of this Part. Zhongbao Binhai Nickel Industry

Co., Ltd., Guangdong General Research Institute for Industrial Technology

(Guangzhou Research Institute of Non-ferrous Metals).

Participating drafting organizations of Method 1 of this Part. Northwest Institute

for Non-ferrous Metal Research, Shanxi Taigang Stainless Steel Co., Ltd., Gejiu

Research Institute of Metallurgy, Nantong Entry-Exit Inspection and Quarantine

Bureau of the PRC.

Main drafters of Method 1 of this Part. Zhou Jiannan, Liu Xianbin, Luo Hui, Dai

Fengying, Zhang Yongjin, Sun Baolian, Zhou Kai, Zhao Shuying, Liu Aikun, Han

Ning, Su Linjian, Wu Lianfen, Dou Huaizhi, Zhou Xiaolu.

Drafting organization of Method 2 of this Part. Zhongbao Binhai Nickel Industry

Co., Ltd.

Participating drafting organizations of Method 2 of this Part. Shanxi Taigang

Stainless Steel Co., Ltd., Henan Nashi Technology Co., Ltd., Guangdong

General Research Institute for Industrial Technology (Guangzhou Research

Institute of Non-ferrous Metals), Guangxi Yinyi Science and Technic Mine

Metallurgy Co., Ltd.

Main drafters of Method 2 of this Part. Zhou Jiannan, Liu Xianbin, Shen Yahong,

Liu Aikun, Hu Jianchun, Zhang Xiaoqin, Zhang Junfang, Sun Huina, Dai

Fengying, Sun Hongying, Cao Guohua, Cui Anfang.

Methods for chemical analysis of fire smelting nickel

substrate material - Part 1.Determination of nickel

content - Dimethylglyoxime spectrophotometric

method and dimethylglyoxime gravimetric method

1 Scope

This Part of YS/T 953 specifies the dimethylglyoxime spectrophotometric

method and dimethylglyoxime gravimetric method for the determination of

nickel content in the fire smelting nickel substrate material.

This Part applies to the determination of nickel content in the fire smelting nickel

substrate material. The determination range of Method 1 is 0.50%~5.00%. The

determination range of Method 2 is 1.00%~25.00%.

2 Normative references

The following documents are indispensable for the application of this document.

For the dated references, only the editions with the dates indicated are

applicable to this document. For the undated references, the latest edition

(including all the amendments) are applicable to this document.

GB/T 20066 Steel and iron - Sampling and preparation of samples for the

determination of chemical composition

3 Method 1 - Dimethylglyoxime spectrophotometric

method

3.1 Method summary

USE hydrochloric acid and nitric acid to dissolve the test portion. USE

potassium sodium tartrate as a masking agent; in an alkaline medium of sodium

hydroxide, use ammonium persulfate as an oxidant; nickel and

dimethylglyoxime form a soluble wine-red complex. At the 460 nm wavelength

of the spectrophotometer, measure the absorbance and calculate the nickel

content.

3.2 Reagents

Unless otherwise specified, only reagents confirmed to be analytically pure and

distilled water or deionized water or water of equivalent purity are used in the

analysis.

3.2.1 Hydrochloric acid (rho=1.19 g/mL).

3.2.10 Nickel standard solution

3.2.10.1 Nickel standard solution (1.0 mg/mL). WEIGH 0.5000 g of metallic

nickel (wNi>=99.99%) and place it in a 250 mL beaker; ADD 20 mL of nitric acid

solution (3.2.2) along the wall of the beaker; COVER the watch glass; HEAT it

to dissolve; REMOVE and cool to room temperature; TRANSFER to a 500 mL

volumetric flask; USE water to dilute to the mark and mix well.

3.4.2 Number of determinations

Perform two determinations independently and take the average.

3.4.3 Blank test

WEIGH 0.090 g of pure iron (wNi<=0.005%); do a blank test along with the test

portion.

3.4.4 Determination

3.4.4.1 Dissolution of test portion

PLACE the test portion (3.4.1) in a 250 mL polytetrafluoroethylene beaker; ADD

10 mL of hydrochloric acid (3.2.1), 10 mL of nitric acid (3.2.2); HEAT at low

temperature to almost no reaction; then add 3~5 drops of hydrofluoric acid

(3.2.3) in portions until completely dissolved. ADD 2 mL of perchloric acid

(3.2.4);

3.4.5 Drawing of working curve

PIPETTE 0 mL, 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL of nickel

standard solution (3.2.10.2) respectively; PLACE them in seven 100 mL

volumetric flasks. ADD 10 mL of iron blank solution (3.2.11); prepare the color

developing solution according to step 3.4.4.2; USE the standard color

developing solution without nickel as the reference; MEASURE the absorbance.

USE the mass of nickel as the abscissa and the absorbance as the ordinate;

DRAW a working curve.

3.5 Calculation of analysis results

The nickel content is calculated by the mass fraction wNi of nickel. The value is

expressed in %, calculated according to formula (1).

3.6 Precision

3.6.1 Repeatability

For the measured values of two independent test results obtained under

repeatability conditions, within the average range given below, the absolute

difference between the two test results does not exceed the repeatability limit

(r). Exceeding the repeatability limit (r) does not exceed 5%. The repeatability

limit (r) is obtained by linear interpolation method according to the data in Table

4 Method 2 - Dimethylglyoxime gravimetric method

4.1 Method summary

USE a mixed acid of hydrochloric acid and nitric acid to decompose the test

portion. ADD a small amount of hydrofluoric acid and emit perchloric acid fume.

In the ammoniacal medium of tartrate, use dimethylglyoxime ethanol solution

to precipitate nickel. The precipitate is dried at 145 °C to a constant weight,

weighed. Calculate the nickel content.

4.2 Reagents

Unless otherwise specified, only reagents confirmed to be analytically pure and

distilled water or deionized water or water of equivalent purity are used in the

analysis.

4.3 Samples

TAKE and prepare samples according to GB/T 20066 or appropriate national or

industrial standards.

4.4 Analytical procedures

4.4.1 Mass of test portion

According to Table 3, weigh the sample (4.3), accurate to 0.0001 g.

4.4.2 Number of determinations

Perform two determinations independently and take the average.

4.4.3 Blank test

Do a blank test along with the test portion.

4.4.4 Determination

4.6.2 Reproducibility

For the measured values of two independent test results obtained under

reproducibility conditions, within the average range given below, the absolute

difference between the two test results does not exceed the reproducibility limit

(R). Exceeding the reproducibility limit (R) does not exceed 5%. The

reproducibility limit (R) is obtained by linear interpolation method according to

the data in Table 5.

5 Test report

This clause specifies the content to be included in the test report. At least the

following shall be given.

......

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 12 pages — is available in the English PDF.

Referenced standards

Normative references

GB/T 20066Steel and iron -- Sampling and preparation of samples for the determination of chemical composition

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