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GB/T 11064.9-2023 (GB/T11064.9-2023, GBT 11064.9-2023, GBT11064.9-2023)
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GB/T 11064.9-2023: PDF in English (GBT 11064.9-2023)

GB/T 11064.9-2023
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.
Methods for Chemical Analysis of Lithium Carbonate,
Lithium Hydroxide Monohydrate and Lithium Chloride -
Part 9: Determination of Sulfate Content - Barium Sulfate
Turbidity Method
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. At a wavelength of 420 nm of the spectrophotometer, measure its absorbance
and calculate the sulfate content.
5 Reagents and Materials
Unless it is otherwise specified, only analytically pure reagents are used.
5.1 Water, GB/T 6682, Grade-2.
5.2 Anhydrous barium chloride. Dihydrate barium chloride are pre-burned in a muffle furnace
at 500 C for 30 min, cooled to room temperature in a desiccator, and ground for later use
(particle size is not greater than 75 m).
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).
5.8 Sulfate standard solution: weigh-take 0.9075 g of potassium sulfate (excellent grade of
purity) that has been baked at 105 C ~ 110 C for 2 h and cooled to room temperature in a
desiccator; place it in a 250 mL beaker, use water to dissolve it, then, transfer the solution into
a 1,000 mL volumetric flask; use water to dilute to the scale and shake it well. 1 mL of this
solution contains 0.5 mg of sulfate.
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.
7.2 The lithium hydroxide monohydrate samples shall be packed in plastic containers and sealed
for storage.
8.4.5 Subtract the absorbance of the blank solution and find the corresponding mass of sulfate
from the working curve.
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):
Where,
m1---the mass of sulfate determined in the test solution, expressed in (mg);
m0---the mass of sulfate in the blank solution, expressed in (mg);
V---the total volume of the test solution, expressed in (mL);
m---the mass of the test portion, expressed in (g);
V1---the volume of the transferred test solution, expressed in (mL).
The calculation result is expressed in three decimal places. The rounding-off of the numerical
values shall be carried out in accordance with the stipulations of GB/T 8170.
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%. The repeatability limit (r) is obtained
by the linear interpolation or extrapolation method in accordance with the data in Table 2.
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.