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HG/T 4067-2015Lithium hexafluorophosphate electrolyte solution (English PDF)

六氟磷酸锂电解液

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Issued by

MIIT

Level / Type

Industry · Recommended

Issue date

July 14, 2015

Implementation date

January 1, 2016

Scope

HG/T 4067-2015 is the English-translated version of 六氟磷酸锂电解液.

HG/T 4067-2015 is the Chinese standard "Cell liquor of lithium hexafluorophosphate". Its scope clause reads: This Standard specifies the classification, requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of cell liquor of lithium hexafluorophosphate.

This Standard applies to cell liquors containing lithium hexafluorophosphate in different solvent systems. This product is used in the production of lithium-ion batteries and lithium-ion ultra-capacitors.

Its clauses include classification; requirements; test methods; inspection rules; marking, labeling; packaging, transportation and storage. It was issued by the Ministry of Industry and Information Technology of the People's Republic of China on JULY 29, 2015 and took effect on JANUARY 01, 2016.

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Document preview — HG/T 4067-2015

National Standard of the People's Republic of China

Replacing
HG/T 4067-2008

Issued by: Ministry of Industry and Information Technology of the People's Republic of China

Contents

  • Foreword3
  • 1 Scope4
  • 2 Normative references4
  • 3 Classification5
  • 4 Requirements5
  • 5 Test methods6
  • 6 Inspection rules13
  • 7 Marking, labeling14
  • 8 Packaging, transportation and storage14

Foreword

This Standard was drafted in accordance with the rules given in GB/T 1.1-2009.

This Standard replaces HG/T 4067-2008 Lithium hexafluorophosphate and cell liquor of lithium Hexafluorophosphate - Part 2: Cell liquor of lithium hexafluorophosphate; compared with HG/T 4067-2008, the main technical changes, except editorial changes, are as follows.

-- Modify the scope of application of cell liquor of lithium hexafluorophosphate (see 1; 1 of the 2008 edition);

-- Add the classification of cell liquor of lithium hexafluorophosphate (see 3);

-- Adjust the index requirements for sulfate content, iron content and sodium content (see 4.2; 3.2 of the 2008 edition);

-- Add the index requirements for aluminum (Al), calcium (Ca), cadmium (Cd), chromium (Cr), copper (Cu), mercury (Hg), magnesium (Mg), nickel (Ni), lead (Pb), zinc (Zn) and arsenic (As) (see 4.2);

-- Modify the determination method of chloride to turbidimetric method (see 5.4; 4.9 of the 2008 edition);

-- Add the colorimeter method (arbitration method) for the measurement of chromaticity (see 5.6; 4.3 of the 2008 edition);

-- Add the density instrument method (arbitration method) for the measurement of density (see 5.7; 4.4 of the 2008 edition).

1 Scope

This Standard specifies the classification, requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of cell liquor of lithium hexafluorophosphate.

This Standard applies to cell liquors containing lithium hexafluorophosphate in different solvent systems. This product is used in the production of lithium-ion batteries and lithium-ion ultra-capacitors.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the dated version applies to this document. For undated references, the latest edition (including all amendments) applies to this document.

GB 150.1, Pressure vessels - Part 1: General requirements

GB 150.2, Pressure vessels - Part 2: Materials

GB 150.3, Pressure Vessels - Part 3: Design

GB 150.4, Pressure vessels - Part 4: Fabrication, inspection and testing, and acceptance

GB 190-2009, Packing symbol of dangerous goods

GB/T 191-2008, Packaging - Pictorial marking for handling of goods

GB/T 605-2006, Chemical reagent - General method for the measurement of colour

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 & expression and judgment of limiting values

GB/T 19282-2014, Analytic method for lithium hexafluorophosphate

3 Classification

Cell liquor of lithium hexafluorophosphate is divided into two categories according to its different uses.

4 Requirements

4.2 Cell liquor of lithium hexafluorophosphate, when tested according to the test method specified in this Standard, shall meet the technical requirements in Table 1.

4.1 Appearance. transparent liquid

5 Test methods

5.1 General provisions

The reagents and water used in this Standard refer to analytical reagents and grade-3 water specified in GB/T 6682-2008, unless otherwise specified. The standard titration solutions, impurity standard solutions, preparations and products that are required in the test shall be prepared in accordance with the provisions of HG/T 3696.1, HG/T 3696.2, HG/T 3696.3 when no other requirements are specified.

5.2 Appearance inspection

In a fume hood, judge the appearance visually.

5.3 Determination of sulfate content

5.3.3 Analysis steps

5.3.3.1 Preparation of standard comparison solution. Into a series of 50 mL colorimetric tubes, transfer 0.50 mL, 1.00 mL, 1.50 mL, 2.00 mL, 2.50 mL and 3.00 mL of sulfate standard solution respectively; add 0.3 mL of hydrochloric acid solution and 3 mL of absolute ethanol in turn; use water to dilute to 25 mL; shake well; then, respectively transfer into 2 mL of barium chloride solution; shake well; let stand for 1 h. Compare with the sample solution.

5.4 Determination of chloride content

5.4.1 Method summary

After the sample is dissolved, add silver nitrate to the nitric acid medium to form a white silver chloride suspension with chloride ions, and compare the turbidity with the standard.

5.4.2 Reagents

5.4.2.1 Nitric acid solution. 1+2.

5.4.3 Analysis steps

5.4.3.1 Preparation of standard turbidimetric solution. Into a series of 50 mL colorimetric tubes, transfer 0.05 mL, 0.10 mL, 0.20 mL, 0.30 mL, 0.40 mL and 0.50 mL of chloride standard solution, respectively. Use water to dilute to about 15 mL; add 5 mL of nitric acid solution and 1 mL of silver nitrate solution; use water to dilute to 25 mL; shake well; let stand for 15 min. Compare with the sample solution.

5.5 Determination of cation content

5.5.1 Method summary

Measure each cation content in the sample by the working curve method on an inductively coupled plasma optical emission spectrometer (ICP-OES) with a fluoride-resistant sampling system.

5.5.2 Reagents

5.5.2.1 Ethyl methyl carbonate-absolute ethanol solution. Dissolve the electronic grade ethyl methyl carbonate, absolute ethanol and water evenly in each other according to the volume ratio of 1.4.5.

5.5.4 Analysis steps
5.5.4.1 Preparation of sample solution

Weight 5 g of the sample in the glove box to the nearest 0.002 g. Take it out from the glove box; put it in a 50 mL (V) volumetric flask; add ethyl methyl carbonate-absolute ethanol solution to dilute to the mark; shake well.

5.5.5 Result calculation

Calculate the content of cations in mass fraction w1; express the value in mg/kg; calculate according to Formula (1).

5.6 Chromaticity

5.6.1 Colorimeter method (arbitration method)
5.6.1.1 Equipment

Automatic colorimeter. measuring wavelength range 420 nm ~ 720 nm, step 10 nm.

5.6.1.2 Analysis steps

Import the sample into a cuvette with an optical path of 50 mm; pour it into about 2/3 of the volume of the cuvette; use lens tissue to wipe the outside of the cuvette; put the cuvette into the colorimeter; close the cover and perform measurement; read the measured platinum-cobalt data.

5.6.2 Platinum-cobalt standard solution colorimetric method
5.6.2.3.2 Standard light box
5.6.2.4 Analysis steps

Inject the sample into the colorimetric tube; compare it with the platinum-cobalt standard solution of 50 Hazen visually along the axis of the colorimetric tube in the standard light box. The color of the sample shall not be darker than the platinum-cobalt standard solution.

5.7 Determination of density

5.7.1 Density instrument method (arbitration method)
5.7.1.1 Method summary

Use a density instrument to measure the density of the cell liquor at 20°C.

5.7.2 Density meter method
5.7.2.1 Method summary

Use a density meter to measure the density of the cell liquor at 20°C.

5.7.2.2 Instrument

5.7.2.2.1 Density meter.

5.7.2.2.2 Constant temperature water bath. the temperature can be controlled at 20°C ± 0.5°C.

5.8.2 Equipment

5.8.2.1 Conductivity meter.

5.8.2.2 Constant temperature water bath. the temperature can be controlled at 25°C ± 0.5°C.

5.8.3 Analysis steps

Use a dry and clean corrosion-resistant sample bottle to take about 100 mL of the sample; place it in a constant temperature water bath at 25°C ± 0.5°C; shake it from time to time. When the temperature of the sample is constant, replace the cap of the sample bottle with a rubber stopper inserted with an electrode; when the temperature is within the range of 25°C ± 0.5°C, read the data, which is the conductivity of the tested sample.

5.9 Determination of moisture

5.9.1 Method principle

According to the provisions of 3.7.1 in GB/T 19282-2014.

5.9.2 Instrument

According to the provisions of 3.7.2 in GB/T 19282-2014.

5.9.3 Analysis steps

Carry out in a glove box (required dew point <= -40°C); weigh 1 g of the sample; then, measure according to 3.7.3 in GB/T 19282-2014.

5.9.4 Result calculation

According to the provisions of 3.5.5 in GB/T 19282-2014.

5.10 Determination of free acid content

5.10.1 Method summary

According to the provisions of 3.9.1 in GB/T 19282-2014.

6 Inspection rules

6.1 This Standard adopts type inspection and exit-factory inspection. Type inspection and exit-factory inspection shall meet the following stipulations.

6.2 The cell liquor of lithium hexafluorophosphate, which is produced continuously - with the same materials and basically under the same production conditions - by the production enterprise, shall be the same batch. Each batch of products shall not exceed 50 t.

6.3 The number of sampling units shall be determined in accordance with the provisions of GB/T 6678. Use clean and dry corrosion-resistant bottles for airtight sampling. The sampling volume of each batch of products shall not be less than 200 g.

6.4 If any of the inspection results does not meet the requirements of this Standard, re-inspection shall be taken from twice the number of products.

7 Marking, labeling

7.1 There shall be firm and clear markings on the outer packaging of the cell liquor product of lithium hexafluorophosphate, including.

7.2 Each batch of cell liquor products of lithium hexafluorophosphate leaving the factory shall be accompanied by a quality certificate, including.

8 Packaging, transportation and storage

8.1 Cell liquor of lithium hexafluorophosphate shall be packaged under airtight and dry conditions. The products shall be packaged in stainless-steel barrels that meet the requirements of GB 150.1~150.4.

8.2 During transportation, there shall be coverings to avoid the sun and rain, so as to prevent the packaging from being damaged. For special products, select the appropriate transportation conditions according to the instructions attached to the product.

8.3 Keep the original packing barrel intact and airtight; place it in a cool,

8.4 Under the packaging, transportation and storage conditions specified in this Standard, the cell liquor of lithium hexafluorophosphate shall have a shelf life of not less than 2 months from the date of production, and shall still be usable if it passes the inspection after the expiration date. CHEMICAL INDUSTRY STANDARD

ICS 71.060.50

G 12 Record number. 50871-2015 Replacing HG/T 4067-2008 Cell liquor of lithium hexafluorophosphate Issued on. JULY 29, 2015 Implemented on. JANUARY 01, 2016 Issued by. Ministry of Industry and Information Technology of the People's Republic of China […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

Referenced standards

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Editions of HG/T 4067

EditionTitleRevisionStatus
HG/T 4067-2015Lithium hexafluorophosphate electrolyte solutioncurrent editionCurrent
HG/T 4067-2008Lithium hexafluorophosphate electrolyte solutionprevious editionSuperseded

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