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GB/T 11064.2-2023 English PDF (GBT11064.2-2023)

GB/T 11064.2-2023 English PDF (GBT11064.2-2023)

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GB/T 11064.2-2023: Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 2: Determination of lithium hydroxide content -- Acid-alkali titrimetric method

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%.
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 and 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 ???: Weigh 0.1 g of bromocresol green, dissolve it in ethanol (95%), and dilute the solution to 100 mL with ethanol (95%).
Solution ???: 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 ??? and 10 mL of solution ???, 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 (??=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;

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