GB/T 11064.2-2023 (GB/T11064.2-2023, GBT 11064.2-2023, GBT11064.2-2023) & related versions
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 2: Determination of lithium hydroxide content -- Acid-alkali titrimetric method
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Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 2: Determination of lithium hydroxide content -- Acid-alkali titrimetric method
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| GB/T 11064.2-1989 | English | 199 |
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Lithium carbonate--Determination of lithium hydroxide content--Acid-alkali titrimetric method
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GB/T 11064.2-2023
GB
NATIONAL STANDARD OF THE
PEOPLE'S REPUBLIC OF CHINA
ICS 77.120.99
CCS H 14
Replacing GB/T 11064.2-2013
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride - Part 2:
Determination of lithium hydroxide content - Acid-alkali
titrimetric method
ISSUED ON: MAY 23, 2023
IMPLEMENTED ON: DECEMBER 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
Introduction ... 6
1 Scope ... 8
2 Normative references ... 8
3 Terms and definitions ... 8
4 Principles ... 9
5 Reagents or materials ... 9
6 Instruments and equipment ... 10
7 Samples ... 10
8 Test steps ... 10
9 Experimental data processing ... 11
10 Precision ... 12
11 Test report ... 12
Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride - Part 2:
Determination of lithium hydroxide content - Acid-alkali
titrimetric method
1 Scope
This document describes a method for the determination of lithium hydroxide content
in lithium hydroxide monohydrate by acid-alkali titration.
This document applies to the determination of lithium hydroxide content in lithium
hydroxide monohydrate. The determination range (mass fraction) is greater than or
equal to 55.00%.
2 Normative references
The following documents contain the provisions which, through normative reference in
this document, constitute the essential provisions of this document. For the dated
referenced documents, only the versions with the indicated dates are applicable to this
document; for the undated referenced documents, only the latest version (including all
the amendments) 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 judgment
of limiting values
GB/T 12805 Laboratory glassware - Burettes
GB/T 17433 Foundation terms for chemical analysis of metallurgical products
3 Terms and definitions
The terms and definitions defined in GB/T 17433 apply to this document.
4 Principles
The sample is dissolved with a certain amount of hydrochloric acid standard solution,
methyl red-bromocresol green is used as the indicator, then the total alkalinity of the
test solution is titrated with hydrochloric acid standard titration solution, and the content
of lithium hydroxide is calculated according to the consumption of hydrochloric acid
standard titration solution. The content of sodium, potassium, and carbonate in the
sample shall be converted to the content of lithium hydroxide and subtracted from the
calculation result.
5 Reagents or materials
Unless otherwise specified, only analytically pure reagents are used.
5.1 Water
It shall conform to grade II water specified in GB/T 6682, and shall be sealed and cooled
to room temperature after boiling.
5.2 Methyl red-bromocresol green indicator
Solution Ⅰ: Weigh 0.1 g of bromocresol green, dissolve it in ethanol (95%), and dilute
the solution to 100 mL with ethanol (95%).
Solution Ⅱ: Weigh 0.2 g of methyl red, dissolve it in ethanol (95%), and dilute the
solution to 100 mL with ethanol (95%).
Take 30 mL of solution Ⅰ and 10 mL of solution Ⅱ, and mix well.
5.3 Hydrochloric acid standard titration solution [cHCl =0.30 mol/L]
5.3.1 Preparation: Pipette 25 mL of hydrochloric acid (ρ=1.19 g/mL), place it in a 1000
mL volumetric flask, dilute to the mark with water, and mix well.
5.3.2 Calibration: Two operators respectively weigh 4 parts of 0.5 g of (accurate to
0.0001 g) anhydrous sodium carbonate working standard reagent, which has been pre-
dried at 270 °C~300 °C to a constant amount; dissolve them in 50 mL of water, add 10
drops of methyl red -Bromocresol green indicator (5.2), and titrate with the prepared
hydrochloric acid standard titration solution (5.3.1) until the solution changes from
green to wine red; boil for 2 minutes, and continue titrating until the solution turns wine
red again and does not fade for 30 seconds, that is the end point. The relative range of
parallel calibration results shall not be greater than the critical range of relative
repeatability of 0.15%, and the relative range of 8 parallel calibration results operated
by two persons shall not be greater than the critical range of relative repeatability of
Carry out two experiments in parallel, and take the average value as the result.
8.3 Blank test
Do a blank test at the same time as the sample test.
8.4 Determination
Put the test sample (8.1) in a 250 mL Erlenmeyer flask in which 30 mL of hydrochloric
acid standard titration solution (5.3) has been pre-added, add 10 drops of methyl red-
bromocresol green indicator (5.2), and titrate with hydrochloric acid standard titration
solution (5.3) until the test solution turns from green to wine red, that is the end point.
Carbon dioxide interference shall be avoided during the titration.
9 Experimental data processing
The content of lithium hydroxide is expressed as the mass fraction of lithium hydroxide
(wLiOH) and calculated according to formula (2):
where:
c -- the actual concentration of hydrochloric acid standard titration solution (5.3),
in moles per liter (mol/L);
V2 -- the volume of hydrochloric acid standard titration solution (5.3) consumed
by titration of the test solution, in milliliters (mL);
V1 -- the volume of hydrochloric acid solution consumed by the blank test, in
milliliters (mL);
23.94 -- the molar mass with (LiOH) as the basic unit, in grams per mole (g/mol);
m0 -- the mass of the sample, in grams (g);
wNa -- the mass fraction of sodium;
1.0416 -- the conversion factor of sodium to lithium hydroxide;
wK -- the mass fraction of potassium;
0.6125 -- the conversion factor of potassium to lithium hydroxide;
......
GB/T 11064.2-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing GB/T 11064.2-1989
Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and
lithium chloride -
Part 2. Determination of lithium hydroxide
content - Acid-alkali titrimetric method
ISSUED ON. SEPTEMBER 06, 2013
IMPLEMENTED ON. MAY 01, 2014
Issued by.
General Administration of Quality Supervision, Inspection
and Quarantine of the People’s Republic of China;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method summary ... 5
3 Reagents... 5
4 Samples ... 6
5 Analysis steps ... 6
6 Calculation of analysis results ... 7
7 Precision ... 8
8 Test report ... 8
Foreword
GB/T 11064.2-2013 “Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride” is divided into 16 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 - Determination of lithium chloride
content - Potentiometric 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 and aluminum content - Inductively coupled plasma
atomic emission spectrometry.
This Part is part 2 of GB/T 11064.
This Part is drafted in accordance with rules given in GB/T 1.1-2009.
The Part replaces GB/T 11064.2-1989 "Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and lithium chloride - Part 2. Determination
of lithium hydroxide content - Acid-alkali titrimetric method".
Compared with GB/T 11064.2-1989, the main changes of this Part are as follows.
- ADD the repeatability terms;
- RE-EDIT the text format; ADD the test report.
This Part shall be under the jurisdiction of National Standardization Technical
Committee of Nonferrous Metals (SAC/TC 243).
Drafting organizations of this Part. Xinjiang Wuxin Lithium Salt Development Co., Ltd.,
Sichuan Tianqi Lithium Co., Ltd., and Jiangxi Ganfeng Lithium Co., Ltd.
The main drafters of this Part. Xia Shufen, Gou Haixia, Luo Yuping, Yi Qingyun, Zeng
Xianqin, and Zhang Wenqin.
The historical version replaced by this Part is as follows.
- GB/T 11064.2-1989.
Methods for chemical analysis of lithium
carbonate, lithium hydroxide monohydrate and
lithium chloride -
Part 2. Determination of lithium hydroxide
content - Acid-alkali titrimetric method
1 Scope
This Part of GB/T 11064 specifies the determination method of lithium hydroxide in
lithium hydroxide monohydrate.
This Part applies to the determination of lithium hydroxide in lithium hydroxide
monohydrate. The determination range. more than 50.00%.
2 Method summary
The sample is dissolved in a certain amount of hydrochloric acid standard titration
solution; use methyl red - bromocresol green as the indicator; continue to titrate with
hydrochloric acid standard titration solution to titrate the total alkalinity of the test
solution; use the consumed amount of hydrochloric acid standard titration solution to
calculate the content of lithium hydroxide. Sodium and potassium content in test
sample shall be converted to lithium hydroxide content, then subtracted from the
calculation result.
3 Reagents
Unless otherwise indicated, all reagents used in this Part are analytical reagent, the
water used is deionized water.
3.1 Methyl red - bromocresol green indicator. Pipette 30mL of bromocresol green
solution (3.1.1) and 10mL of methyl red solution (3.1.2); mix well.
3.1.1 Bromocresol green solution. Weigh 0.1g of bromocresol green; dissolve it in
100mL of ethanol (95%) solution.
3.1.2 Methyl red solution. Weigh 0.2g of methyl red; dissolve it in 100mL of ethanol
(95%) solution.
7 Precision
7.1 Repeatability
For the two independent test results obtained under repeatability conditions, within the
average-value range as given below, the absolute difference of these two test results
does not exceed the repeatability limit (r), and the situation exceeding repeatability
limit (r) is not more than 5%. Repeatability limit (r), according to Table 1, adopts linear
interpolation to obtain.
Table 1
wLiOH / % 53.41 55.50 57.09
r / % 0.057 0.076 0.088
7.2 Allowable difference
The difference of analysis results among laboratories shall not be more than the
allowable difference in Table 2.
Table 2
Mass fraction of lithium hydroxide / % Allowable difference / %
> 50.00 0.25
8 Test report
The test report shall contain the following content.
- Sample;
- The number of this Part national standard;
- Analysis result and its expression;
- Difference with the basic analysis step;
- Anomalies observed in the determination;
- Determination date.
......
| Standard ID | GB/T 11064.2-2023 (GB/T11064.2-2023) | | Description (Translated English) | Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 2: Determination of lithium hydroxide content -- Acid-alkali titrimetric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 9,980 | | Date of Issue | 2023-05-23 | | Date of Implementation | 2023-12-01 | | Older Standard (superseded by this standard) | GB/T 11064.2-2013 | | Drafting Organization | Tianqi Lithium Industry Co., Ltd., Jiangxi Ganfeng Lithium Industry Co., Ltd., Guangdong Bangpu Recycling Technology Co., Ltd., Yichun Silver Lithium New Energy Co., Ltd., Yahua Lithium Industry (Ya'an) Co., Ltd., Jiangsu Ronghui General Lithium Industry Co., Ltd., Xinjiang Institute of Nonferrous Metals, Guohe General (Qingdao) Testing and Evaluation Co., Ltd., Zijin Mining Group Co., Ltd., Zhejiang Huayou Cobalt Co., Ltd., Industrial Analysis and Testing Center of Guangdong Academy of Sciences, Yichun Lithium Battery Industry Research Institute (Jiangxi Lithium Battery Product Quality Supervision and Inspection Center), Jiangxi Jiuling Lithium Industry Co., Ltd. | | Administrative Organization | National Nonferrous Metals Standardization Technical Committee (SAC/TC 243) | | Proposing organization | China Nonferrous Metals Industry Association | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Management Committee | | Standard ID | GB/T 11064.2-2013 (GB/T11064.2-2013) | | Description (Translated English) | Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 2: Determination of lithium hydroxide content - Acid-alkali titrimetric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H64 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 8,898 | | Older Standard (superseded by this standard) | GB/T 11064.2-1989 | | Drafting Organization | Xinjiang Hao Xin Development Co., lithium salt | | Administrative Organization | National Nonferrous Metals Standardization Technical Committee | | Regulation (derived from) | National Standards Bulletin 2013 No. 17 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies: lithium hydroxide monohydrate lithium hydroxide volume measuring methods. This standard applies to: lithium hydroxide monohydrate lithium hydroxide amount determined. Measuring range | | Standard ID | GB/T 11064.2-1989 (GB/T11064.2-1989) | | Description (Translated English) | Lithium carbonate--Determination of lithium hydroxide content--Acid-alkali titrimetric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H14 | | Classification of International Standard | 71.06 | | Word Count Estimation | 2,294 | | Date of Issue | 1989/3/31 | | Date of Implementation | 1990/2/1 | | Quoted Standard | GB 1.4; GB 1467 | | Drafting Organization | Xinjiang Non-ferrous metals Institute | | Regulation (derived from) | National Standards Bulletin 2013 No. 17 | | Proposing organization | China Institute of Standard Metrology, China Nonferrous Metals Industry Corporation | | Issuing agency(ies) | State Bureau of Technical Supervision | | Summary | This Standard specifies lithium hydroxide monohydrate determination of lithium hydroxide content. This Standard is applicable to industrial-grade lithium hydroxide monohydrate determination of lithium hydroxide content. Measuring range: greater than 50. 00%. |
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