GB/T 19282-2014 PDF English
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| GB/T 19282-2014 | English | 230 |
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Analytic method for Lithium hexafluorophosphate
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| GB/T 19282-2003 | English | 359 |
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Analytic method for Lithium hexafluorophosphate
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GB/T 19282-2014: Analytic method for Lithium hexafluorophosphate---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT19282-2014
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.01
G 10
Replacing GB/T 19282-2003
Analytic method for lithium hexafluorophosphate
Issued on. SEPTEMBER 03, 2014
Implemented on. MAY 01, 2015
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Analytical methods... 5
Appendix A (Informative) Recommended ion chromatograph operating conditions. 16
1 Scope
This standard specifies the identification of lithium hexafluorophosphate products AND
the analytical methods of related physical and chemical indicators.
This standard applies to lithium hexafluorophosphate products.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 6283-2008 Chemical products - Determination of water Karl·Fischer method
(general method)
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
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
HG/T 3696.3 Inorganic chemicals for industrial use - Preparations of standard and
reagent solutions for chemical analysis - Part 3.Preparations of reagent solutions
3 Analytical methods
3.1 General provisions
The reagents and water, which are used in this standard, refer to the first-grade pure
reagents and the first-grade water, which are specified in GB/T 6682-2008, unless other
requirements are specified. For the standard solutions for chemical analysis, standard
solutions of impurities, preparations and products, which are used in the test, they shall
be prepared in accordance with the provisions of HG/T 3696.1, HG/T 3696.2, HG/T
3696.3, unless other requirements are specified.
3.2 Identification test
3.3 Determination of cation content
3.3.1 Standard addition method
3.3.1.1 Method summary
The content of each cation in the specimen is determined, by standard addition method,
on an inductively coupled plasma optical emission spectrometer (ICP-OES), which has
a hydrofluoric acid-resistant sampling system.
3.3.1.2 Reagents
3.3.1.3 Instruments and equipment
3.3.1.4 Analytical procedures
3.3.1.4.1 Preparation of test solutions
3.3.1.5 Result calculation
The cation content is calculated in mass fraction w1; the value is expressed in mg/kg; it
is calculated according to formula (1).
3.3.2 Working curve method
3.3.2.1 Method summary
The content of each cation in the specimen is determined, by the working curve method,
on an inductively coupled plasma optical emission spectrometer (ICP-OES), which has
a hydrofluoric acid-resistant sampling system.
3.3.2.2 Reagents
It complies with the requirements, which are given in 3.3.1.2.
3.3.2.3 Instruments and equipment
It complies with the requirements, which are given in 3.3.1.3.
3.3.2.4 Analytical procedures
3.3.2.5 Result calculation
The cation content is calculated in mass fraction w1; the value is expressed in mg/kg; it
is calculated according to formula (2).
3.4 Determination of anion content
3.4.1 Method summary
The chloride ion and sulfate ion, in lithium hexafluorophosphate, are separated by
chromatographic column; detected by conductivity detector. The content of detected
anion is calculated by external standard method.
3.4.2 Reagents
3.4.2.1 Water. Deionized water, which has a conductivity (25 °C) not greater than
0.0055 mS/m.
3.4.2.2 Ice water. Add an appropriate amount of ice cubes to the water. Use it, when the
water temperature is ≤ 4 °C.
3.4.2.3 Regeneration fluid. According to the suppressor used and its usage, refer to the
instruction manual of the suppressor, to select a suitable regeneration fluid.
3.4.3 Instruments and equipment
3.4.3.1 Ion chromatograph. An analytical system, which is resistant to fluoride
corrosion.
3.4.3.1.1 Chromatographic column. The resolution of the detected anion R ≥ 1.5.
3.4.3.1.2 Filter membrane. ≤ 0.45 µm.
3.4.3.1.3 Detector. Conductivity detector, or other detectors, if it can be confirmed that
it has the same function.
3.4.3.2 Volumetric flask. Polyethylene or other corrosion-resistant materials, which
have a volume of 100 mL.
3.4.4 Analytical procedures
3.4.4.1 Preparation of working curve solution
Use a suitable pipette, to pipette each standard use solution into four 100 mL volumetric
flasks, according to the provisions of Table 2.Use water to dilute it to the mark. Shake
well.
3.4.5 Result calculation
The mass fraction of anion content is calculated in w2; the value is expressed in mg/kg;
it is calculated according to formula (3).
3.5 Determination of chloride ion content
3.5.1 Reagents
3.5.1.1 Nitric acid solution. 1 + 2.
3.5.1.2 Silver nitrate solution. 17 g/L.
3.5.1.3 Chloride standard solution. 1 mL solution contains 1 μg of chloride (Cl). Pipette
10 mL of chloride standard solution, which is prepared according to HG/T 3696.2.Put
it in a 100 mL volumetric flask. Use water to dilute it to the mark. Shake well. Pipette
1 mL into a 100 mL volumetric flask. Use water to dilute it to the mark. Shake well.
Store it at 4 °C. The validity period is 30 days.
3.5.2 Analytical procedures
3.6 Determination of sulfate content
3.6.1 Method principle
In hydrochloric acid medium, barium ions and sulfate ions form insoluble barium
sulfate. When the content of sulfate ions is low, barium sulfate will be in suspension,
within a certain period of time, making the solution turbid, which can be determined,
by the visual turbidimetry.
3.6.2 Reagents
3.6.2.1 Absolute ethanol.
3.6.2.2 Hydrochloric acid solution. 1 + 1.
3.6.2.3 Barium chloride solution. 250 g/L.
3.6.2.4 Sulfate standard solution. 1 mL solution contains 1.0 μg of sulfate (SO4). Pipette
10 mL of sulfate standard solution, which is prepared according to HG/T 3696.2.Put it
in a 100 mL volumetric flask. Use water to dilute it to the mark. Shake well. Pipette 1
mL into a 100 mL volumetric flask. Use water to dilute it to the mark. Shake well. Store
it at 4 °C. The validity period is 30 days.
3.6.3 Analytical procedures
3.6.3.1 Preparation of standard turbidity solution
Pipette 0.00 mL, 5.00 mL, 10.00 mL, 15.00 mL of sulfate standard solution, into a 25
mL colorimetric tube, respectively. Add 0.3 mL of hydrochloric acid solution and 3 mL
of absolute ethanol in sequence. Then use water to dilute it to 25 mL. Shake well. Add
2 mL of chlorine barium chloride solution. Shake well.
3.6.3.2 Determination
Weigh about 5 g of the specimen in the glove box, accurate to 0.01 g. Take it out and
place it in a polyethylene beaker, which is filled with 15 mL of water. Dissolve and
filter it into a 25 mL colorimetric tube. Then treat it, together with the standard turbidity
solution at the same time. The turbidity of the solution is compared with that of the
standard turbidity solution.
3.7 Determination of moisture
3.7.1 Method principle
Same as Chapter 3 of GB/T 6283-2008.
3.7.2 Instruments and equipment
3.7.2.1 Automatic moisture analyzer. Coulomb coulometric method.
3.7.2.2 Glove box. dew point < -40 °C.
3.7.3 Analytical procedures
The analytical procedure shall be carried out in a glove box. Weigh about 0.5 g of the
specimen, accurate to 0.001 g. Put the specimen into the measuring bottle of the
automatic moisture analyzer, until it is completely dissolved. Stir evenly. Then measure
its moisture.
3.7.4 Result calculation
The mass fraction w3 of water, expressed in mg/kg, is calculated according to formula (4).
3.8 Determination of dimethyl carbonate (DMC) insoluble content
3.8.1 Method summary
Use dimethyl carbonate to dissolve the specimen. Use a membrane filtration device to
filter it. Dry it at 105 °C ± 2 °C, until the mass is constant.
3.8.2 Reagents
Dimethyl carbonate (DMC). Moisture < 0.0010%.
3.8.3 Instruments and equipment
3.8.3.1 Membrane filtration device. 1000 mL, which is matched with a filter membrane
with a diameter of 50 mm.
3.8.3.2 Filter membrane. The material is polytetrafluoroethylene or other hydrofluoric
acid-resistant filter membrane, which has a pore size of 0.45 μm and a diameter of 50
mm.
3.8.3.3 Vacuum pump and filter equipment.
3.8.3.4 Magnetic stirrer.
3.8.3.5 Beaker. It has lid AND is made of polyethylene or other corrosion-resistant
material.
3.8.3.6 Electric heating constant temperature drying box. An explosion-proof constant
temperature box, whose temperature can be controlled at 105 °C ± 2 °C.
3.8.5 Result calculation
The insoluble content of dimethyl carbonate (DMC) is calculated in mass fraction w4;
the value is expressed in mg/kg; it is calculated according to formula (5).
3.9 Determination of free acid content
3.9.1 Method summary
Use a micro-burette. Use bromothymol blue as an indicator. Use standard titration
solution of sodium hydroxide, to titrate the free acid in the specimen.
3.9.2 Reagents
3.9.2.1 Sodium hydroxide standard titration solution. c(NaOH) ≈ 0.01 mol/L.
Preparation. Pipette 100 mL of sodium hydroxide standard solution, which is prepared
according to HG/T 3696.1.Place it in a 1000 mL volumetric flask. Use carbon dioxide-
free water to dilute it to the mark. Shake well.
3.9.2.2 Ice water. Add an appropriate amount of ice cubes to the water. Use it when the
water temperature is ≤ 4 °C.
3.9.2.3 Bromothymol blue indicator solution. 1 g/L.
3.9.3 Instruments and equipment
3.9.4 Analytical procedures
Weigh about 10 g of the sample by weight loss method, accurate to 0.0002 g. Quickly
pour the sample into a beaker, which contains 100 mL of ice water. Shake the beaker,
to dissolve the specimen quickly. Add 10 drops of bromothymol blue indicator solution.
Use sodium hydroxide standard titration solution, to rapidly titrate it to light blue (no
color fading in 10 s), which is the end point. At the end point, the temperature of the
solution shall still remain ≤ 4 °C.
3.9.5 Result calculation
The free acid content is calculated in terms of the mass fraction w5 of hydrofluoric acid
(HF); the value is expressed in mg/kg; it is calculated according to formula (6).
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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