GB/T 23853-2022 PDF English (GB/T 23853-2009: Older version)

GB/T23853-2022 (GBT23853-2022): PDF in English

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 H.......
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