GB/T 11064.9-2023 PDF English
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| GB/T 11064.9-2023 | English | 195 |
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 9: Determination of sulfate content - Barium sulfate turbidity method
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| GB/T 11064.9-2013 | English | 85 |
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 9: Determination of sulfate content -- Barium sulfate nephelometry method
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| GB/T 11064.9-1989 | English | 199 |
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Lithium carbonate, lithium hydroxide monohydrate and lithium chloride--Determination of sulphide content--Reduction titrimetric method
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GB/T 11064.9-2023: Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 9: Determination of sulfate content - Barium sulfate turbidity method
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT11064.9-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
CCS H 14
Replacing GB/T 11064.9-2013
Methods for Chemical Analysis of Lithium Carbonate, Lithium
Hydroxide Monohydrate and Lithium Chloride - Part 9.
Determination of Sulfate Content - Barium Sulfate Turbidity Method
Issued on. AUGUST 6, 2023
Implemented on. MARCH 1, 2024
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
Introduction... 5
1 Scope... 7
2 Normative References... 7
3 Terms and Definitions... 7
4 Principle... 7
5 Reagents and Materials... 8
6 Instruments and Equipment... 8
7 Samples... 8
8 Test Procedures... 9
9 Processing of Test Data... 10
10 Precision... 10
11 Test Report... 11
Appendix A (informative) Statistical Data Obtained through Interlaboratory Results 12
Foreword
This document was drafted in accordance with the rules of GB/T 1.1-2020 Directives for
Standardization - Part 1.Rules for the Structure and Drafting of Standardizing Documents.
This is Part 9 of GB/T 11064 Methods for Chemical Analysis of Lithium Carbonate, Lithium
Hydroxide Monohydrate and Lithium Chloride. GB/T 11064 has issued the following parts.
---Part 1.Determination of Lithium Carbonate Content - Acid-alkali Titrimetric Method;
---Part 2.Determination of Lithium Hydroxide Content - Acid-alkali Titrimetric Method;
---Part 3.Determination of Lithium Chloride Content - Potentiometric Method;
---Part 4.Determination of Potassium and Sodium Content - Flame Atomic Absorption
Spectrometric Method;
---Part 5.Determination of Calcium Content - Flame Atomic Absorption Spectrometric
Method;
---Part 6.Determination of Magnesium Content - Flame Atomic Absorption Spectrometric
Method;
---Part 7.Determination of Iron Content - 1,10-phenanthroline Spectrophotometric
Method;
---Part 8.Determination of Silicon Content - Molybdenum Blue Spectrophotometric
Method;
---Part 9.Determination of Sulfate Content - Barium Sulfate Nephelometry Method;
---Part 10.Determination of Chloride Content - Silver Chloride Nephelometry Method;
---Part 11.Determination of Acid-insolubles Content - Gravimetric Method;
---Part 12.Determination of Carbonate Content - Acid-alkali Titrimetric Method;
---Part 13.Determination of Aluminum Content - Chromazurol S-cetylpyridine Bromide
Spectrophotometric Method;
---Part 14.Determination of Arsenic Content - Molybdenum Blue Spectrophotometric
Method;
---Part 15.Determination of Fluoride Content - Ion Selective Method;
---Part 16.Determination of Calcium, Magnesium, Copper, Lead, Zinc, Nickel,
Manganese, Cadmium, Aluminum, Iron and Sulfate Contents - Inductively Coupled
Plasma Atomic Emission Spectrometry.
This document serves as a replacement of GB/T 11064.9-2013 Methods for Chemical Analysis
of Lithium Carbonate, Lithium Hydroxide Monohydrate and Lithium Chloride - Part 9.
Determination of Sulfate Content - Barium Sulfate Nephelometry Method. In comparison with
GB/T 11064.9-2013, apart from structural adjustments and editorial modifications, the main
technical changes are as follows.
a) The scope of determination is modified (see Chapter 1; Chapter 1 of Version 2013);
b) The barium chloride solution is modified into anhydrous barium chloride solid (see
5.2; 3.5 of Version 2013);
c) The operation of determination is modified (see 8.4; 6.4 of Version 2013);
d) The “drawing of working curve” is modified (see 8.3; 6.5 of Version 2013);
e) The “reproducibility clause” is added (see 10.2);
f) “Allowable difference” is deleted (see 8.2 of Version 2013).
Please be noted that certain content of this document may involve patents. The institution
issuing this document does not undertake the responsibility of identifying these patents.
This document was proposed by China Non-ferrous Metals Industry Association.
This document shall be under the jurisdiction of National Technical Committee 243 on
Nonferrous Metals of Standardization Administration of China (SAC/TC 243).
The drafting organizations of this document. Tianqi Lithium Co., Ltd.; Jiangsu Ganfeng
Lithium Group Co., Ltd.; Guangdong BRUNP Recycling Co., Ltd.; Yichun Yin Li New Energy
Co., Ltd.; Yahua Lithium (Yaan) Co., Ltd.; Jiangsu General Lithium Co., Ltd.; Xinjiang Institute
for Nonferrous Metal; China United Test & Evaluation (Qingdao) Co., Ltd.; Zijin Mining Group
Co., Ltd.; Zhejiang Huayou Cobalt Co., Ltd.; Center for Industrial Analysis and Testing,
Guangdong Academy of Sciences; Yichun Lithium Battery Industry Research Institute (Jiangxi
Lithium Battery Product Quality Supervision and Inspection Center); Jiangsu Jiuling Lithium
Co., Ltd.
The main drafters of this document. Du Mingze, Jiang Hucheng, Liang Shan, Zhou Jiahong,
Huang Aihong, Deng Hongyun, Liu Zhihua, Wan Sicheng, Wen Liangmao, Yang Lei, Guan
Lixiao, Liu Kai, Qiu Lizhen, Gao Juanya, Xu Siting, Deng Bei, Wang Qingling.
This document was firstly issued in 1989 and firstly revised in 2013.This is the second revision.
1 Scope
This document describes the method for the determination of sulfate content in lithium
carbonate, lithium hydroxide monohydrate and lithium chloride.
This document is applicable to the determination of sulfate content in lithium carbonate, lithium
hydroxide monohydrate and lithium chloride. The range of determination is 0.050% ~ 0.800%
(mass fraction).
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in this text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 8170 Rules of Rounding off for Numerical Values & Expression and Judgement of
Limiting Values
GB/T 17433 Foundation Terms for Chemical Analysis of Metallurgical Products
3 Terms and Definitions
The terms and definitions defined in GB/T 17433 are applicable to this document.
4 Principle
In the presence of hydrochloric acid medium and a stabilizer, barium ions and sulfate radicals
in the sample generate insoluble barium sulfate, which is suspended in the solution for a certain
period of time.
5 Reagents and Materials
Unless it is otherwise specified, only analytically pure reagents are used.
5.1 Water, GB/T 6682, Grade-2.
5.3 Hydrochloric acid (1 + 1).
5.4 Hydrochloric acid (1 + 3).
5.5 Ammonia water (1 + 3).
5.6 Glycerol (1 + 4).
5.7 P-nitrophenol indicator (1 g/L).
5.9 Lithium salt matrix solution. weigh-take 20.00 g of lithium carbonate [w (Li2CO3) 99.99%]
in a 300 mL beaker, use water to moisten it, then, dropwise add 2 drops of p-nitrophenol
indicator (5.7) and slowly add hydrochloric acid (ρ = 1.19 g/mL). When lithium carbonate is
completely decomposed (the yellow color disappears), heat and boil it to drive out carbon
dioxide, then, cool to room temperature, and transfer the test solution into a 100 mL volumetric
flask, use water to dilute to the scale and shake it well.
6 Instruments and Equipment
Spectrophotometer, 3 cm cuvette.
7 Samples
7.1 The lithium carbonate and lithium chloride samples are baked at 250 C ~ 260 C for 2 h in
advance, then, placed in a desiccator to cool to room temperature.
8 Test Procedures
8.1 Test Portions
In accordance with Table 1, weigh-take the sample, accurate to 0.0001 g.
8.2 Parallel Test
Carry out two tests in parallel and take the average value.
8.4 Determination
8.5 Drawing of Working Curve
8.5.1 Transfer-take 0 mL, 1.00 mL, 1.50 mL, 2.00 mL, 3.00 mL and 4.00 mL of sulfate standard
solution (5.8) and 5.0 mL of lithium salt matrix solution (5.9), respectively place them into a
set of 100 mL volumetric flasks, then, in accordance with 8.4.3, conduct the determination.
8.5.2 Transfer part of the solution (8.5.1) into a 3 cm cuvette and use the reagent blank as a
reference; at a wavelength of 420 nm of the spectrophotometer, measure its absorbance. With
the mass of sulfate as the x-coordinate and the absorbance as the y-coordinate, draw the working
curve.
9 Processing of Test Data
The sulfate content, which is counted by the mass fraction of sulfate, shall be calculated
in accordance with Formula (1).
10 Precision
10.1 Repeatability
In terms of the determined values of two independent test results obtained under repeatability
conditions, within the range of average values provided in Table 2, the absolute difference
between the two test results does not exceed the repeatability limit (r), and the cases of
exceeding the repeatability limit (r) does not exceed 5%.
10.2 Reproducibility
In terms of the determined values of two independent test results obtained under reproducibility
conditions, within the range of average values provided in Table 3, the absolute difference
between the two test results does not exceed the reproducibility limit (R), and the cases of
exceeding the reproducibility limit (R) does not exceed 5%.
11 Test Report
The test report shall at least provide contents in the following aspects.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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