GB/T 11064.1-2024 PDF English
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 1: Determination of lithium carbonate content - Titration
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 1: Determination of lithium carbonate content -- Acid-alkali titrimetric method
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| GB/T 11064.1-1989 | English | 199 |
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Lithium carbonate--Determination of lithium carbonate content--Acid-alkali titrimetric method
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GB/T 11064.1-2024: Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 1: Determination of lithium carbonate content - Titration
---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/GBT11064.1-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
CCS H 14
GB/T 11064.1-2024
Replacing GB/T 11064.1-2013
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride - Part 1.
Determination of lithium carbonate content - Titration
Issued on. SEPTEMBER 29, 2024
Implemented on. APRIL 01, 2025
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
Introduction... 6
1 Scope... 8
2 Normative references... 8
3 Terms and definitions... 8
4 Method 1.acid-alkali titrimetric method... 9
4.1 Principle... 9
4.2 Reagents or materials... 9
4.3 Instrument... 10
4.4 Sample... 10
4.5 Test procedure... 10
4.6 Test data processing... 10
4.7 Precision... 11
5 Method 2.potentiometric method... 12
5.1 Principle... 12
5.2 Reagents or materials... 12
5.3 Instrument... 13
5.4 Sample... 13
5.5 Test procedure... 13
5.6 Test data processing... 13
5.7 Precision... 14
6 Test report... 15
Annex A (informative) Statistical results of raw data of precision test... 16
Foreword
This document was drafted in accordance with the provisions of GB/T 1.1-2020
“Directives for standardization - Part 1.Rules for the structure and drafting of
standardizing documents”.
This document is Part 1 of GB/T 11064 “Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and lithium chloride”. GB/T 11064 has
published the following parts.
- Part 1.Determination of lithium carbonate content - Titration;
- 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 turbidity 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-cetylpyridinium
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 replaces GB/T 11064.1-2013 “Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and lithium chloride - Part 1.
Determination of lithium carbonate content - Acid-alkali titrimetric method”.
Compared with GB/T 11064.1-2013, in addition to structural adjustments and editorial
changes, the main technical changes are as follows.
a) MODIFY the concentration of hydrochloric acid standard titration solution (see
4.2.3 of this document, 3.2.1 of the 2013 edition);
b) MODIFY the relevant content of “weighing mass” (see 4.5 of this document, 5.1
of the 2013 edition);
c) ADD the relevant content of “blank test” (see 4.5.3 of this document);
d) MODIFY the relevant content of “test data processing” (see 4.6 of this document,
Clause 6 of the 2013 edition);
e) DELETE the relevant content of “allowable difference” (see 7.2 of the 2013
edition);
f) ADD the reproducibility clause (see 4.7.2 of this document);
g) ADD the potentiometric method (see Clause 5 of this document).
Attention is drawn to the possibility that some of the elements of this document may be
the subject of patent rights. The issuing authority of this document shall not be held
responsible for identifying any or all such patent rights.
This document was proposed by China Nonferrous Metals Industry Association.
This document shall be under the jurisdiction of National Technical Committee on
Nonferrous Metals of Standardization Administration of China (SAC/TC 243).
Drafting organizations of this document. Jiangxi Ganfeng Lithium Industry Group Co.,
Ltd., Yichun Tianzhuo New Materials Co., Ltd., Yichun Yinli New Energy Co., Ltd.,
Shandong Ruifu Lithium Industry Co., Ltd., Tianqi Lithium New Energy Materials
(Suzhou) Co., Ltd., Yahua Lithium Industry (Ya’an) Co., Ltd., Center for Industrial
Analysis and Testing of Guangdong Academy of Sciences, Swiss Metrohm China Co.,
Ltd., Jiangxi Yongxing Special Steel New Energy Technology Co., Ltd., GEM (Wuxi)
Energy Materials Co., Ltd., Xinjiang Nonferrous Metals Research Institute Co., Ltd.,
Guangdong Brunp Recycling Technology Co., Ltd., Jiangsu Ronghui General Lithium
Co., Ltd., Tangshan Xinfeng Lithium Co., Ltd., Zhejiang Huayou Cobalt Co., Ltd.,
Chengdu Chemphys High Energy Chemical Industry Co., Ltd., Chengxin Lithium
Group Co., Ltd., Jiangxi Dongpeng New Material Co., Ltd., Guobiao (Beijing) Testing
and Certification Co., Ltd., Yichun Lithium Battery Industry Research Institute (Jiangxi
Lithium Battery Product Quality Supervision and Inspection Center), Jiangxi Jiuling
Lithium Industry Co., Ltd., Urumqi Ya’ou Rare Metals Co., Ltd., Ningdu Ganfeng
Lithium Co., Ltd., China Nonferrous Metals (Guilin) Geology and Minning Co., Ltd.
Main drafters of this document. Li Qiang, Zhao Wentao, Zhou Jiahong, Wu Jinfang,
Xiong Xiaoyan, Liu Binhua, Huang Yanjun, Kang Rujin, Zhang Jun, Zhao Jiang, Liu
Shanshan, Chen Yujun, Wang Yongsheng, Xie Tangfeng, Yang Lei, Wen Guangxue, Xu
Jianqing, Cai Rongfu, Wu Xuefeng, Peng Wenxiu, Zhang Yuxin, Dai Zehua, Wu Ling,
Deng Hongyun, Yang Huilin, Yao Li, Weina, Dai Xiaoyong, Xie Hui, Xu Hua.
This document was first issued in 1989 and revised for the first time in 2013.This is
the second revision.
1 Scope
This document describes the determination methods of lithium carbonate content in
lithium carbonate products, including acid-alkali titrimetric method (method 1) and
potentiometric method (method 2).
This document applies to the determination of lithium carbonate content in lithium
carbonate products, and the determination range (mass fraction). greater than 95.00 %.
If other forms of carbonate exist, they will be converted into lithium carbonate for
deduction.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
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 12805 Laboratory glassware - Burettes
GB/T 17433 Foundation terms for chemical analysis of metallurgical products
3 Terms and definitions
For the purpose of this document, the terms and definitions defined in GB/T 17433 apply.
4 Method 1.acid-alkali titrimetric method
4.1 Principle
The test material is dissolved in a certain amount of water, and methyl red-bromocresol
green is used as an indicator. The solution is titrated with a standard hydrochloric acid
titration solution until the solution changes from green to wine red.
4.2 Reagents or materials
Unless otherwise specified, only analytical reagents are used.
4.2.1 Water, GB/T 6682, grade 2, boiled and sealed and cooled to room temperature.
4.2.2 Methyl red-bromocresol green indicator. weigh 0.1 g of bromocresol green,
dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %) (solution I); weigh
0.2 g of methyl red, dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %)
(solution II). Take 30 mL of solution I and 10 mL of solution II and mix them well.
4.2.3 Hydrochloric acid standard titration solution (about 0.50 mol/L). pipette 45 mL
of hydrochloric acid (ρ = 1.19 g/mL) into a 1000 mL volumetric flask, dilute to the
mark with water, and mix well.
4.3 Instrument
Burette with stopper (Grade A), specification 50 mL, shall comply with the provisions
of GB/T 12805.
4.4 Sample
The sample is pre-dried at 250 ℃ ~ 260 ℃ for 2 h, placed in a desiccator, and cooled
to room temperature.
4.5 Test procedure
4.5.1 Test material
Weigh 0.5 g of sample (4.4) to the nearest 0.0001 g.
4.5.4 Determination
Place the test material (4.5.1) in a 250 mL conical flask, add 20 mL of water to dissolve
the test material, add 10 drops of methyl red-bromocresol green indicator (4.2.2), titrate
with hydrochloric acid standard titration solution (4.2.3) until the test solution changes
from green to wine red, boil for 2 min, drive off carbon dioxide, cool, and continue the
titration test until the test solution turns wine red, which is the end point.
4.6 Test data processing
The lithium carbonate content is calculated as the mass fraction of lithium carbonate,
w, according to formula (2).
4.7 Precision
4.7.1 Repeatability
The absolute difference between the two independent test results obtained under
repeatability conditions does not exceed the repeatability limit (r), as shown in Table 1,
and the case of exceeding repeatability limit (r) does not exceed 5 %. The original data
of precision test is shown in Annex A.
4.7.2 Reproducibility
The absolute difference between the two independent test results obtained under
reproducibility conditions shall not exceed the reproducibility limit (R), as shown in
5 Method 2.potentiometric method
5.1 Principle
The test material is dissolved in a certain amount of water and titrated using a
potentiometric titrator, with a pH glass composite electrode as the working electrode
and a hydrochloric acid standard titration solution as the titrant.
5.2 Reagents or materials
Unless otherwise specified, only analytical reagents shall be used.
5.2.1 Water, GB/T 6682, grade 2, boiled and sealed and cooled to room temperature.
5.2.2 Methyl red-bromocresol green indicator. weigh 0.1 g of bromocresol green,
dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %) (solution I);
5.2.3 Hydrochloric acid standard titration solution (about 0.50 mol/L).
5.3 Instrument
Potentiometric titrator.
5.4 Sample
to room temperature.
5.5 Test procedure
5.5.1 Test material
Weigh 0.5 g of sample (5.4) to the nearest 0.0001 g.
5.5.2 Parallel test
Perform two tests in parallel and take the average value.
5.5.3 Blank test
Perform a blank test with the test sample.
5.6 Test data processing
The lithium carbonate content is calculated as the mass fraction of lithium carbonate,
w, according to formula (4).
5.7 Precision
5.7.1 Repeatability
The absolute difference between the two independent test results obtained under
repeatability conditions does not exceed the repeatability limit (r), as shown in Table 3,
and the case of exceeding repeatability limit (r) does not exceed 5 %.
5.7.2 Reproducibility
The absolute difference between the two independent test results obtained under
reproducibility conditions does not exceed the reproducibility limit (R), as shown in
Table 4, and the case of exceeding repeatability limit (R) does not exceed 5 %.
6 Test report
The test report shall at least give the following.
- the test object;
- the serial number of this document;
- the method used;
- the analysis results and their expression;
- the differences from the basic analysis procedure;
- the abnormal phenomena observed;
- the test date.
Annex A
(informative)
Statistical results of raw data of precision test
A.1 The precision data of acid-alkali titration was determined by joint tests of 19
laboratories on 4 different levels of lithium carbonate samples. Each laboratory
independently determined each level of sample 11 times under repeatability conditions.
The statistical data of the determination results are shown in Table A.1.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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