YS/T 582-2023 English PDF (YS/T582-2023)

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YS/T 582-2023: Battery grade lithium carbonate
YS/T 582-2023
YS
NONFERROUS METAL INDUSTRY STANDARD
ICS 77.150.99
CCS H64
Replacing YS/T 582-2013
Battery grade lithium carbonate
ISSUED ON. DECEMBER 20, 2023
IMPLEMENTED ON. JULY 01, 2024
Issued by. Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Terms and definitions... 5
4 Classification... 6
5 Technical requirements... 6
6 Test methods... 7
7 Inspection rules... 7
8 Marking, packaging, transportation, storage, accompanying documents... 8
9 Order form content... 10
Appendix A (Normative) Determination of boron content in lithium carbonate --
Inductively coupled plasma atomic emission spectrometry... 11
Appendix B (Normative) Determination of magnetic impurity content in lithium
carbonate - Inductively coupled plasma atomic emission spectrometry... 15
Appendix C (Normative) Determination of loss on ignition... 20
Battery grade lithium carbonate
1 Scope
This document specifies the classification, technical requirements, test methods,
inspection rules, marking, packaging, transportation, storage, accompanying
documents, order forms of battery-grade lithium carbonate.
This document is applicable to battery-grade lithium carbonate, which is produced by
various methods.
2 Normative references
The contents of the following documents constitute essential clauses of this document
through normative references in the text. Among them, for dated references, only the
version corresponding to that date applies to this document; for undated references, the
latest version (including all amendments) applies to this document.
GB/T 191 Packaging - Pictorial marking for handling of goods
GB/T 6284 Chemical products for industrial use - General method for determination
of water content - The loss of mass on drying method
GB/T 6678-2003 General principles for sampling chemical products
GB/T 11064 (all parts) Methods for chemical analysis of lithium carbonate, lithium
hydroxide monohydrate and lithium chloride
GB/T 19077 Particle size analysis - Laser diffraction methods
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Magnetic impurity
Material that can be directly or indirectly adsorbed by ferromagnetic bodies.
Note. Mainly refers to magnetic substances in transition elements such as iron, chromium,
nickel, zinc and their alloys.
The moisture content in the product shall not exceed 0.20%.
5.4 Loss on ignition
The loss on ignition in the product shall not exceed 0.50%.
5.5 Particle size
The particle size of the product shall meet the following requirements. D10 ≥ 1 µm, 4
µm ≤ D50 ≤ 8 µm, 9 µm ≤ D90 ≤ 15 µm, D99 ≤ 30 µm; or determined by negotiation
between the supplier and the buyer.
5.6 Appearance quality
The product is in the form of white powder with no visible inclusions.
6 Test methods
6.1 The determination of the chemical composition of the product shall be carried out
in accordance with the provisions of GB/T 11064 (all parts). The determination of the
boron content shall be carried out in accordance with the provisions of Appendix A.
6.2 The determination of magnetic impurity in the product shall be carried out in
accordance with the provisions of Appendix B.
6.3 The determination of moisture in the product shall be carried out in accordance with
the provisions of GB/T 6284.
6.4 The determination of the loss on ignition in the product shall be carried out in
accordance with the provisions of Appendix C.
6.5 The determination of the particle size of the product shall be carried out in
accordance with the provisions of GB/T 19077.
6.6 The appearance quality of the product shall be visually inspected.
7 Inspection rules
7.1 Inspection and acceptance
7.1.1 The product shall be inspected by the supplier or a third party, to ensure that the
product quality complies with the provisions of this document and the order form.
7.1.2 The purchaser may inspect the received products in accordance with the
provisions of this document. If the inspection results are inconsistent with the
provisions of this document and the order form, it shall be proposed to the supplier
b) Product name;
c) Batch number;
d) Net weight;
e) Main content;
f) This document number;
g) Origin;
h) "Avoid-rain" mark in GB/T 191.
8.2 Packaging, transportation, storage
8.2.1 The product is packed in polyethylene (PE) lined bags, polypropylene (PP) outer
bags or two to three layers of paper bags. The inner bag is tied or heat-sealed; the outer
bag is firmly tied. The net weight of each bag is implemented according to the
requirements of the buyer.
8.2.2 The product shall avoid contact with acid during transportation; the packaging
bag shall be prevented from being damaged during handling; attention shall be paid to
moisture-proof.
8.2.3 The product shall be stored in a dry, acid-free environment.
8.3 Accompanying documents
Each batch of products shall be accompanied by accompanying documents, which shall
include supplier information, product information, this document number, exit-factory
date or packaging date; it should also include.
a) Product quality guarantee, which shall include the following.
● Main performance and technical parameters of the product;
● Product characteristics (including manufacturing process and raw material
characteristics);
● Responsibility for product quality;
● Quality certification obtained by the product and various analytical test results.
b) Product certificate, which shall include the following.
● Inspection items and their results or test conclusions;
● Batch size or batch number;
Appendix A
(Normative)
Determination of boron content in lithium carbonate -- Inductively coupled
plasma atomic emission spectrometry
A.1 Overview
This Appendix is applicable to the determination of boron content in lithium carbonate,
which has a determination limit of 0.000050% ~ 0.010% boron content.
A.2 Principle
The sample is dissolved in hydrochloric acid. The boron content is determined by the
standard working curve method on an inductively coupled plasma atomic emission
spectrometer.
A.3 Reagents or materials
Unless otherwise specified, only reagents confirmed to be of superior purity are used in
the analysis. Boron-containing vessels shall be avoided during the experiment.
A.3.1 Water, GB/T 6682, grade 2.
A.3.2 Hydrochloric acid (ρ = 1.19 g/mL).
A.3.3 Hydrochloric acid (1 + 1).
A.3.4 Boric acid (99.99%), spectrally pure. Dry under vacuum at 60 °C for 2 h; place
in a desiccator to cool to room temperature.
A.3.5 Boron standard stock solution. Weigh 5.7179 g of boric acid (A.3.4) in a 200 mL
polytetrafluoroethylene beaker. Add 50 mL of water to dissolve completely. Transfer to
a 1000 mL volumetric flask. Add water to 900 mL. Add 20 mL of hydrochloric acid
(A.3.2). Use water to dilute it to the mark. Shake well. Transfer to a plastic bottle for
storage. 1 mL of this solution contains 1 mg of boron.
A.3.6 Boron standard solution A. Pipette 20.00 mL of boron standard stock solution
(A.3.5) into a 200 mL beaker. Add 4 mL of hydrochloric acid (A.3.2). Use water to
dilute to the mark. Shake well. Transfer to a plastic bottle for storage. 1 mL of this
solution contains 100 μg of boron.
A.3.7 Boron standard solution B. Pipette 10.00 mL of boron standard solution A (A.3.6)
into a 100 mL volumetric flask. Add 2 mL of hydrochloric acid (A.3.2). Use water to
dilute to the mark. Shake well. Transfer to a plastic bottle for storage. 1 mL of this
solution contains 10 μg of boron.
Appendix B
(Normative)
Determination of magnetic impurity content in lithium carbonate - Inductively
coupled plasma atomic emission spectrometry
B.1 Summary
This Appendix is used to determine the content of magnetic impurity in lithium
carbonate, which has a determination limit of 5.00 μg/kg ~ 1000.00 μg/kg.
B.2 Principle
Magnetic impurity in the sample is adsorbed and enriched by magnetic rods,
decomposed with aqua regia; the content of magnetic impurity is determined by the
standard working curve method on an inductively coupled plasma atomic emission
spectrometer
B.3 Reagents or materials
Unless otherwise specified, only reagents confirmed to be of superior purity are used in
the analysis. All the instruments used in the experiment are soaked in nitric acid (1 + 4)
and then thoroughly cleaned with ultrapure water.
B.3.1 Water, GB/T 6682, Grade II.
B.3.2 Nitric acid (ρ = 1.42 g/mL).
B.3.3 Hydrochloric acid (ρ = 1.19 g/mL).
B.3.4 Nitric acid (1 + 1)
B.3.5 Aqua regia. Mix 1 volume of nitric acid (B.3.2) and 3 volumes of hydrochloric
acid (B.3.3); prepare it when needed.
B.3.6 Iron standard storage solution. Weigh 1.0000 g of pure metal iron wire (≥ 99.9%)
into a 200 mL beaker. Add 20 mL of nitric acid (B.3.4). Dissolve in a water bath until
clear. Cool it. Transfer to a 1000 mL volumetric flask. Use water to dilute to the mark.
Shake well. 1 mL of this solution contains 1 mg of iron.
B.3.7 Zinc standard stock solution. Weigh 1.0000 g of pure metallic zinc (≥ 99.9%) in
a 200 mL beaker. Add 20 mL of nitric acid (B.3.4). Dissolve at low temperature until
clear. Cool it. Transfer to a 1000 mL volumetric flask. Use water to dilute to the mark.
Shake well. 1 mL of this solution contains 1 mg of zinc.
B.3.8 Nickel standard stock solution. Weigh 1.0000 g of pure metallic nickel (≥ 99.9%)
in a 200 mL beaker. Add 20 mL of nitric acid (B.3.4). Dissolve at low temperature until
clear. Cool it. Transfer to a 1000 mL volumetric flask. Use water to dilute to the mark.
Shake well. 1 mL of this solution contains 1 mg of nickel.
B.3.9 Chromium standard storage solution. Weigh 1.0000 g of pure metallic chromium
(purity 99.99%) into a 200 mL beaker. Add 20 mL of nitric acid (B.3.4). Dissolve at
low temperature until clear. Cool it. Transfer to a 1000 mL volumetric flask. Use water
to dilute to the mark. Shake well. 1 mL of this solution contains 1 mg of chromium.
B.3.10 Mixed standard solution A. Transfer 20.00 mL of each standard storage solution
(B.3.6 to B.3.9) into a 200 mL volumetric flask. Add 20 mL of nitric acid (B.3.4). Use
water to dilute to the mark. Shake well. 1 mL of this solution contains 100 μg of iron,
zinc, nickel, chromium.
B.3.11 Mixed standard solution B. Pipette 10.00 mL of mixed standard solution A
(B.3.10) into a 100 mL volumetric flask. Add 10 mL of nitric acid (B.3.4). Use water to
dilute to the mark. Shake well. 1 mL of this solution contains 10 μg of iron, zinc, nickel,
chromium.
B.3.12 Argon (wAr ≥ 99.995%).
B.4 Instruments and equipment
B.4.1 Inductively coupled plasma atomic emission spectrometer.
B.4.2 Magnetic bar. 6000 Gs ~ 8000 Gs, Φ17 mm × 53 mm, wrapped with
polytetrafluoroethylene. Before adsorption, place it in a 200 mL beaker; add 130 mL of
ultrapure water and 8 mL of aqua regia (B.3.5); boil slightly for 30 min; then wash with
ultrapure water.
B.4.3 Rod mill, which has speed regulation and timing functions.
B.5 Sample
Take a dried, non-agglomerated battery-grade lithium carbonate sample; place it in a
desiccator for testing.
B.6 Test steps
B.6.1 Parallel test
Perform two tests in parallel.
B.6.2 Blank test
Perform a blank test with the sample.
B.6.3 Preparation of test solution
Appendix C
(Normative)
Determination of loss on ignition
C.1 Principle
Weigh a certain amount of specimen. Dry it at 500 °C. Calculate the thermal drying
loss. Calculate the loss on ignition in the specimen.
C.2 Equipment
C.2.1 Porcelain crucible. 30 mL.
C.2.2 Muffle furnace.
C.2.3 Dryer.
C.3 Test steps
Weigh 5 g ~ 10 g of specimen into a porcelain crucible that has been pre-dried at 500 °C
to a constant weight (accurate to 0.0001 g). Place in a muffle furnace heated to 500 °C
±5 °C and heat for 30 min. Take out the sample and place it in a dryer. Cool to room
temperature and weigh it.
Repeat the operation until the difference between the two weighing is no more than
0.0003 g, which is regarded as constant weight.
C.4 Test data processing
Calculate the loss on ignition of the sample according to formula (C.1); the value is
expressed in %.
Where.
m2 - The mass of the porcelain crucible, in grams (g);
m3- The mass of the porcelain crucible and the specimen before drying, in grams (g);
m1 - The mass of the porcelain crucible and the specimen after drying, in grams (g).
The calculation result is expressed to two decimal places.
C.5 Allowable difference of results
w loss on ignition