HG/T 4067-2015 English PDF (HGT4067-2015)

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HG/T 4067-2015: Cell liquor of lithium hexafluorophosphate
HG/T 4067-2015
HG
CHEMICAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
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
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
Use a pipette to transfer 1 mL of sulfate standard stock solution prepared according to
HG/T 3696.2; put it in a 100 mL volumetric flask; use water to dilute to the mark; shake
well. Formulate the solution when needed.
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.
5.3.3.2 Preparation of sample solution: In a fume hood, weigh about 3 g of the sample,
accurate to 0.01 g. Then, operate in accordance with 5.3.3.1 from “add 0.3 mL ... in
turn” to “...shake well; let stand for 1 h”. Perform visual turbidimetry with the standard
comparison solution prepared at the same time.
5.3.3.3 Judgment: The turbidity of the sample solution shall not be greater than the
standard comparison solution containing 1.50 mL of sulfate standard 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.
5.4.2.2 Silver nitrate solution: 17 g/L.
5.4.2.3 Chloride standard solution: 1 mL of solution contains 10 μg of chloride (Cl).
Use a pipette to pipette 10 mL of chloride standard stock solution prepared according
to HG/T 3696.2; put it in a 100 mL volumetric flask; use water to dilute to the mark;
shake well. Use a pipette to pipette 10 mL; place in a 100 mL volumetric flask; use
water to dilute to the mark; shake well. Formulate the solution when needed.
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.
5.4.3.2 Preparation of sample solution: Weigh about 5 g of the sample in the glove box,
accurate to 0.01 g. Take it out; put it into a 50 mL colorimetric tube filled with 15 mL
of water; 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. Determine by visual turbidimetry;
compare the turbidity presented with the standard turbidimetric solution.
5.4.3.3 Judgment: The turbidity of the sample solution shall not be greater than the
standard turbidimetric solution containing 0.50 mL of chloride standard 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.
5.5.2.2 Mixed standard solution: 1 mL of solution contains 0.01 mg of cations Al, As,
Cd, Cr, Cu, Hg, K, Mg, Ni, Pb and Zn each, and 0.10 mg of cations Ca, Fe and Na each.
Pipette 1 mL of standard stock solutions of cations Al, As, Cd, Cr, Cu, Hg, K, Mg, Ni,
Pb, and Zn prepared according to HG/T 3696.2, and 10 mL of standard stock solutions
of cations Ca, Fe, and Na; place in the same 100 mL volumetric flask; use ethyl methyl
carbonate-absolute ethanol solution to dilute to the mark; shake well. Alternatively, use
the standard stock solution (1 000 μg/mL) of the national standard sample to accurately
dilute. Formulate this solution when needed.
5.5.3 Instruments and apparatuses
5.5.3.1 Inductively coupled plasma-optical emission spectrometer (ICP-OES):
equipped with a fluoride-resistant sampling system.
5.5.3.2 Volumetric flask: polyethylene or other corrosion-resistant materials, with a
volume of 100 mL.
Before each use, use nitric acid solution (10%) to soak and wash.
5.5.3.3 Pipette and tip: 100 μL ~ 1 000 μL.
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
5.6.2.1 Method summary
Prepare potassium chloroplatinate, cobalt chloride and hydrochloric acid in a certain
proportion into an aqueous solution (platinum-cobalt standa...