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HG/T 4067-2015 PDF English

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HG/T 4067-2015: Cell liquor of lithium hexafluorophosphate
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HG/T 4067: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
HG/T 4067-2015English115 Add to Cart 0-9 seconds. Auto-delivery Cell liquor of lithium hexafluorophosphate Valid
HG/T 4067-2008English399 Add to Cart 3 days Lithium Hexafluorophosphate and Cell liquor of Lithium Hexafluorophosphate. Part 2: Cell liquor of Lithium Hexafluorophosphate Obsolete

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HG/T 4067-2015: Cell liquor of lithium hexafluorophosphate

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HG 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

Table of Contents

Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Classification... 5 4 Requirements... 5 5 Test methods... 6 6 Inspection rules... 13 7 Marking, labeling... 14 8 Packaging, transportation and storage... 14

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). This Standard was proposed by China Petroleum and Chemical Industry Federation. This Standard shall be under the jurisdiction of Subcommittee on Inorganic Chemical Industry of National Standardization Technical Committee of Chemical (SAC/TC 63/SC 1). The drafting organizations of this Standard. CenerTech Tianjin Chemical Research and Design Institute Co., Ltd., Tianjin Jinniu Power Materials Co., Ltd., Henan Huarui Advanced Material Co., Ltd., Shenzhen Capchem Technology Co., Ltd., Guangzhou Tinci Materials Technology Co., Ltd., Beijing Institute of Chemical Reagents. Chief drafting staffs of this Standard. Wang Yan, Zhang Dongqing, Lv Xiuhang, Mao Yuhua, Liu Jiansheng, Wang Lianwang, Wang Ying. The previous versions of the standards which are replaced by this Standard are. -- HG/T 4067-2008. Cell liquor of lithium hexafluorophosphate Warning. The samples and some of the reagents used in this test method are toxic or corrosive, and shall be handled carefully in a fume hood! If it splashes on the eyes or skin, rinse it with water for more than 15 minutes and treat immediately. Where flammable products are used, it is strictly forbidden to use an open flame for heating.

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

4.1 Appearance. transparent liquid. 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.

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. manufacturer name, factory address, product name, category, net content, batch number or production date, shelf life, 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. HG/T 4067-2015 HG 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

Table of Contents

Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Classification... 5 4 Requirements... 5 5 Test methods... 6 6 Inspection rules... 13 7 Marking, labeling... 14 8 Packaging, transportation and storage... 14

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). This Standard was proposed by China Petroleum and Chemical Industry Federation. This Standard shall be under the jurisdiction of Subcommittee on Inorganic Chemical Industry of National Standardization Technical Committee of Chemical (SAC/TC 63/SC 1). The drafting organizations of this Standard. CenerTech Tianjin Chemical Research and Design Institute Co., Ltd., Tianjin Jinniu Power Materials Co., Ltd., Henan Huarui Advanced Material Co., Ltd., Shenzhen Capchem Technology Co., Ltd., Guangzhou Tinci Materials Technology Co., Ltd., Beijing Institute of Chemical Reagents. Chief drafting staffs of this Standard. Wang Yan, Zhang Dongqing, Lv Xiuhang, Mao Yuhua, Liu Jiansheng, Wang Lianwang, Wang Ying. The previous versions of the standards which are replaced by this Standard are. -- HG/T 4067-2008. Cell liquor of lithium hexafluorophosphate Warning. The samples and some of the reagents used in this test method are toxic or corrosive, and shall be handled carefully in a fume hood! If it splashes on the eyes or skin, rinse it with water for more than 15 minutes and treat immediately. Where flammable products are used, it is strictly forbidden to use an open flame for heating.

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

4.1 Appearance. transparent liquid. 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.

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. manufacturer name, factory address, product name, category, net content, batch number or production date, shelf life, 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. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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