GB/T 23853-2022 English PDF (GBT23853-2022)

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GB/T 23853-2022: Lithium carbonate made of brine
GB/T 23853-2022
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
CCS G 12
Replacing GB/T 23853-2009
Lithium carbonate made of brine
卤水碳酸锂
ISSUED ON: JULY 11, 2022
IMPLEMENTED ON: FEBRUARY 01, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 Terms and definitions... 6 
4 Molecular formula and relative molecular mass ... 6 
5 Classification ... 6 
6 Requirements ... 6 
7 Test methods ... 7 
8 Inspection rules ... 19 
9 Signs, labels and accompanying documents ... 20 
10 Packaging, transportation and storage ... 20 
Annex A (informative) Common spectral lines and detection limits of ICP-OES ... 22 
Lithium carbonate made of brine
1 Scope
This document specifies the classification, requirements, test methods, inspection rules
and signs, labels and accompanying documents, packaging, transportation and storage
for lithium carbonate made of brine.
This document applies to lithium carbonate made of brine.
NOTE: This product is mainly used in lithium-ion battery material production, glass manufacturing,
ceramics production and refrigeration, welding, lithium alloy and metallurgical continuous casting
and other fields.
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 191-2008, Packaging - Pictorial marking for handling of goods
GB/T 3050-2000, Inorganic chemical products for industrial use - General method
for determination of chloride content - Potentiometric method
GB/T 6678, General principles for sampling chemical products
GB/T 6682-2008, Water for analytical laboratory use - Specification and test
methods
GB/T 8170, Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 19077, Particle size analysis - Laser diffraction methods
HG/T 3696.1, Inorganic chemicals for industrial use - Preparations of standard and
reagent solutions for chemical analysis - Part 1: Preparations of standard
volumetric solutions
HG/T 3696.2, Inorganic chemicals for industrial use - Preparations of standard and
reagent solutions for chemical analysis - Part 2: Preparations of standard solutions
for impurity
7.3.2 Reagents
7.3.2.1 Hydrochloric acid solution: 1+4.
7.3.2.2 Alkali metal iron periodate solution. Dissolve 2g of potassium periodate in
10mL of potassium hydroxide solution (80g/L). Use water to dilute to 50mL. Add 3mL
of ferric chloride solution (100g/L). After well stirring, use potassium hydroxide
solution (80g/L) to dilute to 100mL.
7.3.2.3 Sodium chloride saturated solution.
7.3.3 Test steps
7.3.3.1 Preparation of test solution
Weigh about 2g of sample, to the nearest of 0.1g. Place in a 100mL tall beaker. Add
water to moisten. Add hydrochloric acid solution dropwise until the sample is just
dissolved. Use water to dilute to about 50mL. Mix well.
7.3.3.2 Identification
Add 1 drop of test solution to the watch glass. Then, add 1 drop of saturated sodium
chloride solution and 2 drops of alkali metal ferric periodate solution dropwise on it.
Use alcohol lamp or other safe heat source to heat to 45℃~50℃. Hold for 15s~20s.
Compared with the blank test, the solution shall be yellow-white turbid.
In the blank test, except that the test solution is not added, the amount of other reagents
added is exactly the same as that of the test solution.
7.4 Determination of lithium carbonate content
7.4.1 Principle
After adding water to the sample, use bromocresol green-methyl red as the indicator
solution. Use hydrochloric acid standard titration solution to titrate. Calculate the
lithium carbonate content according to the consumption of hydrochloric acid standard
titration solution.
7.4.2 Reagents or materials
7.4.2.1 Hydrochloric acid standard titration solution: c(HCl)≈0.5mol/L.
7.4.2.2 Bromocresol green-methyl red indicator solution.
7.4.2.3 Carbon dioxide free water.
7.4.3 Test steps
Weigh about 0.6g of the sample that has been dried at 250℃~260℃ to constant mass,
to the nearest of 0.0002g. Place it in a conical flask. Add 50mL of carbon dioxide-free
water and 10 drops of bromocresol green-methyl red indicator solution. Use
hydrochloric acid standard titration solution to titrate until the solution changes from
green to dark red. Boil for 2min. After cooling, continue to use hydrochloric acid
standard titration solution to titrate to dark red as the end point. Conduct the blank test
at the same time.
7.4.4 Test data processing
Lithium carbonate is calculated as the mass fraction w1 of lithium carbonate (Li2CO3)
according to formula (1):
Where,
c - The exact value of the concentration of hydrochloric acid standard titration solution,
in moles per liter (mol/L);
V1 - The value of the volume of hydrochloric acid standard titration solution consumed
by titrating the sample solution, in milliliters (mL);
V0 - The value of the volume of hydrochloric acid standard titration solution consumed
by the blank test, in milliliters (mL);
m - The value of the sample mass, in grams (g);
M - The value of the molar mass of lithium carbonate, in grams per mole (g/mol) [M
(1/2Li2CO3) = 36.94].
Take the arithmetic mean of the parallel determination results as the determination
result. The absolute difference between the two parallel determination results shall not
be greater than 0.2%.
7.5 Determination of sulfate content
7.5.1 Principle
In the acidic medium, sulfate ions and barium ions form insoluble barium sulfate. When
the sulfate ion content is low, barium sulfate will be in suspension within a certain
period of time, making the solution turbid. Visually compare the turbidity of the sample
solution to the standard turbidity solution.
7.5.2 Reagents or materials
7.5.2.1 Hydrochloric acid solution: 1+1.
7.5.2.2 Sodium chloride-hydrochloric acid-glycerol mixed solution. Weigh 12g of
sodium chloride and dissolve it in 40mL of water. Add 1mL of hydrochloric acid. Use
glycerol to dilute to 100mL. Mix well. If glycerol has a yellow color, it shall use
activated carbon to decolorize in advance.
7.5.2.3 Barium chloride solution: 250g/L.
7.5.2.4 Sulfate standard solution: 1mL of solution contains 0.10mg of sulfate (SO4).
Pipette 10mL of sulfate standard stock solution prepared according to HG/T 3696.2.
Place in a 100mL volumetric flask. Use water to dilute to the scale. Shake well.
7.5.3 Test steps
7.5.3.1 Preparation of test solution
Weigh about 2.5g ± 0.01g of sample. Place in a 100mL tall beaker. Use a little water to
moisten. After adding a watch glass, slowly add hydrochloric acid solution dropwise
until the sample is completely dissolved. Add 10mL of water. Heat to boil. After cooling,
transfer the entire solution to a 250mL volumetric flask. Use water to dilute to the scale.
Shake well. After the solution is still, use medium-speed qualitative filter paper to dry
filter. Discard the first 10mL of filtrate.
7.5.3.2 Test
Pipette 10mL of test solution. Place in a 50mL colorimetric tube. Add water to about
30mL. Add 1mL of hydrochloric acid solution, 10mL of sodium chloride-hydrochloric
acid-glycerol mixed solution. Shake well. Add 3mL of barium chloride solution
dropwise while shaking. Use water to dilute to the scale. Shake well. Place for 5min.
The turbidity shall not be greater than the standard turbidity comparison solution.
The standard turbidity comparison solution is to take 0.10mL (type I), 0.50mL (type II),
and 1.00mL (type III) of sulfate standard solution. Treat it in the same way as the sample
solution.
7.6 Determination of chloride content
7.6.1 Potentiometric titration (arbitration method)
7.6.1.1 Principle
See the provisions in Chapter 3 of GB/T 3050-2000.
7.6.1.2 Reagents or materials
Prepare according to the provisions of Chapter 4 in GB/T 3050-2000.
7.6.1.3 Instruments and equipment
Prepare according to the provisions of Chapter 5 in GB/T 3050-2000.
7.6.2.2.1 Nitric acid solution: 1+4.
7.6.2.2.2 Silver nitrate solution: 17g/L.
7.6.2.2.3 Chloride standard solution: 1mL of the solution contains 0.10mg of chlorine
(Cl). Pipette 10mL of chloride standard stock solution prepared according to HG/T
3696.2. Place in a 100mL volumetric flask. Use water to dilute to the scale. Shake well.
This solution is prepared before use.
7.6.2.3 Test steps
7.6.2.3.1 Preparation of test solution
Weigh about 2.5g ± 0.01g of sample. Place in a 100mL tall beaker. Use a little water to
moisten. After adding a watch glass, slowly add nitric acid solution dropwise until the
sample is completely dissolved. Heat to boil. After cooling, transfer all to a 250mL
volumetric flask. Use water to dilute to the scale. Shake well. After the solution is still,
use medium-speed qualitative filter paper to dry filter. Discard the first 10mL of filtrate.
7.6.2.3.2 Test
Pipette 10mL of test solution. Place in a 50mL colorimetric tube. Add water to about
40mL. Add 1mL of nitric acid solution, 1mL of silver nitrate solution. Use water to
dilute to the scale. Shake well. Place for 2min. The turbidity shall not be greater than
the standard turbidity comparison solution.
The standard turbidity comparison solution is to take 0.20mL (type I), 0.50mL (type II)
and 1.00mL (type III) of chloride standard solution. Treat it in the same way as the
sample solution.
7.7 Determination of content of hydrochloric acid insoluble matter
7.7.1 Principle
Weigh a certain amount of sample and dissolve it in hydrochloric acid solution. The
filtered residue is dried at a certain temperature to a constant mass. Determine the
content of hydrochloric acid insoluble matter.
7.7.2 Reagents or materials
7.7.2.1 Hydrochloric acid solution: 1+1.
7.7.2.2 Nitric acid solution: 1+4.
7.7.2.3 Silver nitrate solution: 17g/L.
7.7.2.4 Methyl orange indicator solution: 1g/L.
7.7.3 Instruments and equipment
7.9.2.4 Standard mixed solution of metal ions and boron and silicon: 1mL of the
solution contains 10μg of sodium (Na), potassium (K), calcium (Ca), magnesium (Mg),
iron (Fe), manganese (Mn), copper (Cu), boron (B) and silicon (Si) each. Pipette 10mL
of the standard solution of each ion in the standard solution of metal ions, boron and
silicon. Place in the same 100mL volumetric flask. Use water to dilute to the scale.
Shake well.
7.9.2.5 Water: Grade two water specified in GB/T 6682-2008.
7.9.3 Instruments and equipment
Inductively coupled plasma atomic emission spectrometer (ICP-OES): Determine
1mg/L or 10mg/L multi-element mixed standard solution. The RSD of 10 repeated
determinations is ≤0.5%. See Annex A for the commonly used spectral lines and
detection limits of ICP-OES for each measured ion.
7.9.4 Test steps
7.9.4.1 Preparation of test solution A
Weigh about 5g of sample, to the nearest of 0.01g. Put in a 400mL beaker. Add a little
water to moisten. After adding a watch glass, slowly add hydrochloric acid solution
dropwise until the sample is completely dissolved. Heat to boil. Cool to room
temperature. Transfer all into a 250mL (V1) volumetric flask. Use water to dilute to the
scale. Shake well. This solution is test solution A, used for the determination of metal
ions, boron and silicon contents.
7.9.4.2 Test
Pipette 20mL (V2) of test solution A respectively (see 7.9.4.1). Place in six 100mL
volumetric flasks. Add 5mL of nitric acid solution to each. Then add 0.0mL, 1.00mL,
2.00mL, 3.00mL, 4.00mL, 5.00mL of metal ions and standard mixed solutions of boron
and silicon, respectively. Use water to dilute to the scale. Shake well.
Turn on the inductively coupled plasma atomic emission spectrometer (ICP-OES).
After the operation is stable, under the selected optimized conditions, measure the
emission spectrum intensities of different masses of each ion separately. Take the
measured ion mass (A) as the abscissa, and the corresponding emission spectrum
intensity (I) as the ordinate, to draw a working curve. Intersect the reverse extension of
the curve with the abscissa. The distance between the intersection point and the origin
is the measured ion mass. The schematic diagram is shown in Figure 1. Calculate to
obtain the content of each ion.
inductively coupled plasma atomic emission spectrometer (ICP-OES) and standard
working curve method to determine the content of magnetic substances.
7.10.2 Reagents or materials
7.10.2.1 Nitric acid solution: 1+19. Use premium pure nitric acid to prepare.
7.10.2.2 Aqua regia: Mix 1 volume of nitric acid and 3 volumes of hydrochloric acid.
Prepare before use. Use premium pure nitric acid and premium pure hydrochloric acid
to prepare.
7.10.2.3 Magnetic substance standard solution: 1mL of the solution contains 0.1mg of
iron (Fe), zinc (Zn), chromium (Cr), and nickel (Ni) each. Respectively pipette 10mL
of iron (Fe), zinc (Zn), chromium (Cr), nickel (Ni) standard stock solutions prepared
according to HG/T 3696.2. Place in 100mL volumetric flasks separately. Use water to
dilute to the scale. Shake well.
7.10.2.4 Magnetic substance standard mixed solution: 1mL of the solution contains
10μg of iron (Fe), zinc (Zn), chromium (Cr) and nickel (Ni) each. Pipette 10mL of
standard solution of each ion in the magnetic substance standard solution, respectively.
Place in the same 100mL volumetric flask. Use water to dilute to the scale. Shake well.
7.10.2.5 Water: Grade two water specified in GB/T 6682-2008.
7.10.3 Instruments and equipment
7.10.3.1 Inductively coupled plasma optical emission spectrometer (ICP-OES):
Determine 1mg/L or 10mg/L multi-element mixed standard solution. The RSD of 10
repeated determinations is ≤0.5%. See Annex A for the commonly used spectral lines
and detection limits of ICP-OES for each measured ion. ...