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GB/T 8151.24-2021: Methods for chemical analysis of zinc concentrates - Part 24: Determination of soluble zinc content - Flame atomic absorption spectrometry
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Methods for chemical analysis of zinc concentrates - Part 24: Determination of soluble zinc content - Flame atomic absorption spectrometry
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GB/T 8151.24-2021
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Basic data | Standard ID | GB/T 8151.24-2021 (GB/T8151.24-2021) | | Description (Translated English) | Methods for chemical analysis of zinc concentrates - Part 24: Determination of soluble zinc content - Flame atomic absorption spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H13 | | Word Count Estimation | 6,611 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 8151.24-2021: Methods for chemical analysis of zinc concentrates - Part 24: Determination of soluble zinc content - Flame atomic absorption spectrometry
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Methods for chemical analysis of zinc concentrates - Part 24.Determination of soluble zinc content - Flame atomic absorption spectrometry
ICS 77.120.60
CCSH13
National Standards of People's Republic of China
Chemical analysis methods of zinc concentrate
Part 24.Determination of soluble zinc content
Flame atomic absorption spectrometry
Released on 2021-04-30
2021-11-01 implementation
State Administration of Market Supervision and Administration
Issued by the National Standardization Management Committee
Foreword
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules of Standardization Documents"
Drafting.
This document is part 24 of GB/T 8151 "Methods for Chemical Analysis of Zinc Concentrates". GB/T 8151 has released the following parts.
---Part 1.Determination of the amount of zinc precipitation separation Na2EDTA titration method and extraction separation Na2EDTA titration method;
---Part 2.Determination of Sulfur Content Combustion Neutralization Titration Method;
---Part 3.Determination of iron content by Na2EDTA titration;
---Part 4.Determination of the amount of silica molybdenum blue spectrophotometry;
---Part 5.Determination of lead content by flame atomic absorption spectrometry;
---Part 6.Determination of copper content by flame atomic absorption spectrometry;
---Part 7.Determination of arsenic content, hydride generation-atomic fluorescence spectrometry and potassium bromate titration;
---Part 8.Determination of cadmium content by flame atomic absorption spectrometry;
---Part 9.Determination of fluorine content by ion selective electrode method;
---Part 10.Determination of the amount of tin hydride generation-atomic fluorescence spectrometry;
---Part 11.Determination of the amount of antimony hydride generation-atomic fluorescence spectrometry;
---Part 12.Determination of silver content by flame atomic absorption spectrometry;
---Part 13.Determination of the amount of germanium, hydride generation-atomic fluorescence spectrometry and benzofluorenone spectrophotometry;
---Part 14.Determination of nickel content by flame atomic absorption spectrometry;
---Part 15.Determination of Mercury Atomic Fluorescence Spectrometry;
---Part 16.Determination of cobalt content by flame atomic absorption spectrometry;
---Part 17.Determination of the amount of zinc hydroxide precipitation-Na2EDTA titration;
---Part 18.Determination of the amount of zinc ion exchange-Na2EDTA titration;
---Part 19.Determination of gold and silver content, lead precipitation or ash-blowing fire assay and flame atomic absorption spectrometry;
---Part 20.Determination of copper, lead, iron, arsenic, cadmium, antimony, calcium, magnesium content inductively coupled plasma atomic emission spectrometry;
---Part 21.Determination of thallium content by inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission spectrometry;
---Part 22.Determination of zinc, copper, lead, iron, aluminum, calcium and magnesium content by wavelength dispersive X-ray fluorescence spectrometry;
---Part 23.Determination of Mercury Content Direct Method of Solid Injection;
--- Part 24.Determination of soluble zinc content by flame atomic absorption spectrometry.
This document was proposed by China Nonferrous Metals Industry Association.
This document is under the jurisdiction of the National Nonferrous Metals Standardization Technical Committee (SAC/TC243).
Drafting organizations of this document. Shenzhen Zhongjin Lingnan Nonferrous Metal Co., Ltd., Shenzhen Zhongjin Lingnan Nonferrous Metal Co., Ltd.
Shaoguan Smelter, Zijin Mining Group Co., Ltd., Jiangsu Beimin Metal Recycling Technology Co., Ltd., China Certification & Inspection Group
West Co., Ltd., Changsha Research Institute of Mining and Metallurgy Co., Ltd., Guangxi Zhuang Autonomous Region Analysis and Testing Research Center, Fangcheng Customs Comprehensive Technical Service
Business Center, Zhuzhou Smelting Group Co., Ltd., Shuikoushan Nonferrous Metals Co., Ltd., Northern Copper Co., Ltd., Qingyuan Jiazhi
New Materials Research Institute Co., Ltd., Yunnan Chihong Zinc and Germanium Co., Ltd., Hunan Nonferrous Geological Exploration Research Institute, Chenzhou City Product Quality
Supervision and inspection institute.
The main drafters of this document. Shi Shilong, Cai Hui, Zuo Hongyi, Huang Ping, Tan Xiuli, Yang Yehao, Suo Yunxiao, Ye Lingling, Yang Binghong, Huang Yifan,
Xie Yuqun, Luo Ronggen, Zhou Tong, Wei Yajuan, Yi Jia, Wei Meng, He Longliang, Lei Suhan, Yu Canhui, Li Hongying, Fu Haikuo, Cheng Lin, Li Jinyan, Xie Lei,
Xie Xiqing, Liu Jianfeng, Zhang Caizhi, Luo Yueying, Gao Yanfen, Huang Lining, Yang Huadong, Xie Yanhong, Wu Xueying, Qian Junfei.
Chemical analysis methods of zinc concentrate
Part 24.Determination of soluble zinc content
Flame atomic absorption spectrometry
1 Scope
This document specifies the method for determining the soluble zinc content in zinc concentrate.
This document is applicable to the determination of soluble zinc content in zinc concentrate. Measuring range. 0.1%~10.5%.
2 Normative references
The contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations
Only the version corresponding to that date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to
This document.
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Solublezinc
A variety of zinc-containing compounds such as zinc sulfate, zinc carbonate, and zinc oxide, which are easily dissolved in the ammonia-ammonium chloride solvent in the zinc concentrate.
4 Method summary
The sample uses ammonia water-ammonium chloride as the solvent to selectively leaching soluble zinc, and adding an appropriate amount of ascorbic acid and stannous dichloride dihydrate as the inhibitor
The preparation enables effective separation of soluble zinc such as zinc sulfate, zinc oxide, and zinc carbonate from zinc sulfide and insoluble zinc salts. In dilute nitric acid medium, make
Use an air-acetylene flame to measure the absorbance of zinc at a wavelength of 213.9nm in an atomic absorption spectrometer, and calculate the soluble zinc according to the standard curve method.
content.
5 Reagents
Unless otherwise specified, only use reagents confirmed to be analytically pure and secondary water that meets the requirements of GB/T 6682 in the analysis.
5.1 Stannous dichloride dihydrate.
5.2 Nitric acid (ρ=1.40g/mL).
5.3 Nitric acid (1 1).
5.4 Ammonia-ammonium chloride-ascorbic acid solution. weigh 160g ammonium chloride, 5g ascorbic acid and dissolve in.200mL water, add 400mL ammonia
Water (ρ=0.91g/mL), dilute with water to 1000mL, and mix well. This solution is prepared for immediate use.
5.5 Zinc standard storage solution. Weigh 1.0000g metallic zinc (wZn≥99.99%) into a 250mL beaker, and slowly add 60mL nitric acid
(5.3), cover the watch glass, after the violent reaction is complete, heat at low temperature until the dissolution is complete, rinse the watch glass and the cup wall with a small amount of water, and boil to drive off the nitrogen
Remove and cool the oxides, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix well. This solution 1mL contains 1mg zinc.
5.6 Zinc standard solution A. Pipette 10.00mL zinc standard stock solution (5.5) into a 100mL volumetric flask, add 6mL nitric acid (5.3),
Dilute with water to the mark and mix well. This solution 1mL contains 100μg zinc.
5.7 Zinc standard solution B. Pipette 1.00mL zinc standard stock solution (5.5) into a 100mL volumetric flask, add 6mL nitric acid (5.3), use
Dilute with water to the mark and mix well. This solution 1mL contains 10μg zinc.
6 Instruments
6.1 Atomic absorption spectrometer with zinc hollow cathode lamp.
Under the best working conditions of the instrument, anyone who can achieve the following indicators can be used.
---Characteristic concentration. In a solution consistent with the matrix of the measurement solution, the characteristic mass concentration of zinc is not greater than 0.04μg/mL;
---Precision. Use the highest concentration of standard solution to measure 10 times, and the standard deviation of its absorbance should not exceed its average absorbance
1.0%; Use the lowest concentration standard solution (not the "zero" concentration standard solution) to measure the absorbance 10 times, and the standard deviation should not exceed
0.5% of the average absorbance of the highest concentration standard solution;
---Linear working curve. Divide the working curve into 5 equal sections according to the concentration, the difference between the absorbance difference of the highest section and the absorbance difference of the lowest section
The ratio should not be less than 0.7.
6.2 Electric heating constant temperature water bath.
7 Specimen
7.1 The particle size of the sample should not be greater than 0.096mm.
7.2 The sample should be dried at 105℃±5℃ for 2h, and placed in a desiccator to cool to room temperature for later use.
8 Test procedure
8.1 Sample
Weigh 0.10g sample, accurate to 0.0001g.
8.2 Parallel test
Do two tests in parallel and take the average value.
8.3 Blank test
Do a blank test with the sample.
8.4 Determination
8.4.1 Place the sample in a 250mL beaker, moisten the sample with a small amount of water, and add 0.015g~0.025g of stannous dichloride dihydrate (5.1),
Shake loose, add 100mL ammonia-ammonium chloride-ascorbic acid solution (5.4), cover with a watch glass, and place in a 70℃±5℃ electric heating constant temperature water bath (6.2)
Medium heating and leaching for 1h, stirring intermittently (to prevent the sample from sticking to the bottom), remove, and cool. Transfer the solution to a 250mL volumetric flask, and dilute to the mark with water.
Mix well. Dry filter with medium speed filter paper, discard the first filtrate, and keep the middle filtrate.
8.4.2 Divide 10.00mL filtrate in a 100mL volumetric flask, add 6mL nitric acid (5.3), dilute to the mark with water, and mix.
8.4.3 Use an air-acetylene flame, adjust to zero with water at the wavelength of 213.9nm in the atomic absorption spectrometer, and measure simultaneously with a series of standard solutions
For the absorbance of zinc, check the corresponding zinc concentration from the working curve.
8.5 Drawing of working curve
8.5.1 Working curve I (range of soluble zinc content. 0.10%~2.00%).
Pipette 0mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL zinc standard solution B (5.7) into one
In a 100mL volumetric flask, add 6mL nitric acid (5.3), add 4mL ammonia-ammonium chloride-ascorbic acid solution (5.4), and dilute with water to 1 minute.
Degree, mix well.
8.5.2 Working curve Ⅱ (soluble zinc content range. >2.00%~10.50%).
Pipette 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL zinc standard solution A (5.6) into one
Group 100mL volumetric flask, add 6mL nitric acid (5.3), add 4mL ammonia-ammonium chloride-ascorbic acid solution (5.4). Dilute with water to
Scale and mix well.
8.5.3 Using an air-acetylene flame, adjust the angle of the combustion head according to the mass concentration, and use water at the wavelength of 213.9nm in the atomic absorption spectrometer.
Zero adjustment. Measure the absorbance of a series of standard solutions, subtract the absorbance of the "zero concentration" solution in the series of standard solutions, and take the mass concentration of zinc as the horizontal
The coordinates, absorbance is the ordinate, and the working curve is drawn.
8.6 Test data processing
The soluble zinc content is calculated as the mass fraction of zinc w soluble zinc, calculated according to formula (1).
w Soluble zinc=
(ρ-ρ0)·V·V2×10-6
m·V1 ×
100% (1)
Where.
ρ --- The concentration of zinc in the test solution obtained from the working curve, in micrograms per milliliter (μg/mL);
ρ0---The concentration of zinc in the blank test solution obtained from the working curve, in micrograms per milliliter (μg/mL);
V --- the total volume of the test solution, in milliliters (mL);
V2---determine the volume of the test solution, the unit is milliliters (mL);
m---the mass of the sample, in grams (g);
V1---The volume of the test solution, the unit is milliliters (mL).
The calculation result is expressed to two decimal places. The rounding of values shall be implemented in accordance with the provisions of GB/T 8170.
9 Precision
9.1 Repeatability
The measured value of two independent test results obtained under repeatability conditions, within the average range given below, these two test results
The absolute difference does not exceed the repeatability limit (r), and the repeatability limit (r) does not exceed 5%. The repeatability limit (r) is based on the data in Table 1.
Obtained by sexual interpolation or extension method.
Table 1 Repeatability limits
w Soluble zinc/% 0.33 1.31 3.16 6.12 10.08
r/% 0.09 0.16 0.25 0.36 0.50
9.2 Reproducibility
The absolute difference between the two independent test results obtained under the reproducibility condition does not exceed the reproducibility limit (R) and exceeds the reproducibility limit (R)
If the situation does not exceed 5%, the reproducibility limit (R) is obtained by linear interpolation or extrapolation according to the data in Table 2.
10 Test report
This chapter specifies the content included in the test report. At least the following aspects should be given.
---Sample;
---Analysis results and their representation;
---Differences from the basic analysis steps;
--- Abnormal phenomena observed in the measurement;
---Test date.
1202-
42.1518
T/
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