HG/T 4701-2021 PDF English
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HG/T 4701-2021: Iron phosphate for battery materials---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/HGT4701-2021
HG
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
CCS G 12
GB/T 4701-2021
Replacing HG/T 4701-2014
Iron phosphate for battery materials
Issued on: DECEMBER 02, 2021
Implemented on: APRIL 01, 2022
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... 6
4 Molecular formula and relative molecular mass... 6
5 Classification... 6
6 Requirements... 6
7 Test method... 7
8 Inspection rules... 18
9 Marking and labeling... 19
10 Packaging, transportation, storage... 19
Appendix A (Informative) Reference instrument working conditions... 20
Iron phosphate for battery materials
1 Scope
This document specifies the requirements, test methods, inspection rules, marking,
labeling, packaging, transportation, storage of iron phosphate for battery materials. This
document applies to iron phosphate for battery materials.
Note. This product is mainly used to manufacture lithium iron phosphate (LiFePO4)
lithium-ion battery positive electrode materials.
2 Normative references
The contents of the following documents constitute the essential terms of this document
through normative references in the text. Among them, for referenced documents with
dates, only the version corresponding to that date is applicable to this document; for
referenced documents without dates, the latest version (including all amendments) is
applicable to this document.
GB/T 191-2008 Packaging - Pictorial marking for handling of goods
GB/T 5162 Metallic powders - Determination of tap density
GB/T 6003.1-2012 Test sieves - Technical requirements and testing - Part 1.Test
sieves of metal wire cloth
GB/T 6678 General principles for sampling chemical products
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods
GB/T 6730.61-2005 Iron ores - Determination of carbon and sulfur content - High
frequency combustion with infrared absorption method
GB/T 8170 Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 19587 Determination of the specific surface area of solids by gas adsorption
using the BET method
HG/T 3696.3 Inorganic chemicals for industrial use - Preparations of standard and
reagent solutions for chemical analysis - Part 3.Preparations of reagent solutions
solution turns a stable purple-red color, which is the end point. The iron content is
calculated based on the consumption of potassium dichromate standard titration
solution.
7.3.2 Reagents or materials
7.3.2.1 Hydrogen peroxide.
7.3.2.2 Hydrochloric acid.
7.3.2.3 Sulfuric acid-phosphoric acid mixed solution.
Slowly add 15 mL of sulfuric acid to 70 mL water; cool it; add 15 mL of phosphoric
acid; mix well.
7.3.2.4 Stannous chloride solution. 100 g/L.
Weigh 10.0 g of stannous chloride (SnCl2·2H2O); place in a dry beaker; dissolve in 40
mL of hydrochloric acid; use water to dilute to 100 mL; add 1 tin particle; store in a
brown bottle.
7.3.2.5 Titanium trichloride solution. 2%.
Pipette 10 mL of titanium trichloride solution (15% ~ 20%); use hydrochloric acid
solution (1 + 9) to dilute to 100 mL; store in a brown bottle. It can be prepared before
use.
7.3.2.6 Potassium dichromate standard titration solution..
Prepare and process the test data according to the following steps.
a) Preparation. Weigh 2.45 g ± 0.2 g of the standard potassium dichromate (accurate
to 0.0001 g), which was dried at 120 °C ± 2 °C to a constant mass; dissolve it in
water; transfer all to a 1000 mL volumetric flask; use water to dilute to the mark;
shake well;
b) Test data processing. The concentration of the standard potassium dichromate
titration solution is expressed in moles per liter (mol/L), which
is calculated according to formula (1).
Where.
m - The mass of the standard potassium dichromate weighed, in grams (g);
V - The volume of the standard potassium dichromate titration solution, in milliliters
(mL);
M - The molar mass of potassium dichromate, in grams per mole (g/mol)
(M = 49.03).
7.3.2.7 Sodium tungstate indicator solution. 10%.
Weigh 10.0 g of sodium tungstate (NaWO4·2H2O); dissolve in 85 mL of water; add 5.0
mL of phosphoric acid; mix well; store in a brown bottle.
7.3.2.8 Sodium diphenylamine sulfonate indicator solution. 5 g/L.
7.3.3 Instruments and equipment
Test sieve. φ200 × 50 - 0.1/0.071 GB/T 6003.1-2012.
7.3.4 Test steps
7.3.4.1 Preparation of test solution A
Weigh 4 g of the sieved specimen (accurate to 0.0002 g); place it in a 250 mL beaker;
moisten it with a small amount of water. Add 25 mL of hydrochloric acid; cover with a
watch glass; heat at low temperature in a fume hood to dissolve. Rinse the watch glass
with a small amount of water; cool it (filter if necessary); transfer it to a 250 mL
volumetric flask; dilute to the mark; shake well. This is test solution A, which is used
for the determination of iron and phosphorus content.
7.3.4.2 Test
Use a pipette to transfer 10 mL of test solution A into a 250 mL conical flask. Add 5 mL
of hydrochloric acid; heat to near boiling. While hot, shake the conical flask and add
stannous chloride solution drop by drop, until the solution changes from brown to light
yellow (if the solution becomes colorless after adding too much stannous chloride, add
hydrogen peroxide until the solution turns light yellow). Add 4 ~ 5 drops of sodium
tungstate indicator solution; add titanium trichloride solution drop by drop while
shaking the conical flask, until the solution turns light blue. Immediately cool with
running water; add 50 mL of water; titrate with potassium dichromate standard titration
solution, until the blue color just fades (usually 1 ~ 2 drops, do not record the reading).
Add water to dilute it to 100 mL. Add 10 mL of sulfuric acid-phosphoric acid mixed
solution, 3 ~ 4 drops of sodium diphenylamine sulfonate indicator solution; titrate with
potassium dichromate standard titration solution until a stable purple-red color appears
(does not disappear in 30 s), which is the end point.
At the same time, perform a blank test. Except for not adding the specimen (except the
standard titration solution), the types and amounts of other reagents added to the blank
7.4.3.2 Electric constant temperature drying oven. Temperature can be controlled at
180 °C ± 5 °C.
7.4.4 Test procedure
Use a pipette to transfer 25 mL of test solution A (see 7.3.4.1) into a 250 mL volumetric
flask; dilute to the mark with water; shake well. Use a pipette to transfer 10 mL of this
test solution into a 250 mL beaker; add 10 mL of nitric acid solution; add water to about
100 mL. Cover with a watch glass; slowly heat to boil; keep it at a slight boil for 5
minutes. Add 50 mL of quinoline molybdate solution; keep it warm for 30 seconds (do
not use open flame when adding reagents or heating; do not stir when adding reagents
or heating to avoid the formation of clots). Cool to room temperature and stir 3 ~ 4
times during the cooling process. Use a glass crucible that has been dried to constant
mass at 180 °C ± 5 °C to filter the upper clear liquid; wash the precipitate 5 ~ 6 times
by decantation, using about 20 mL of water each time. Transfer the precipitate to a glass
crucible and continue washing with water 3 ~ 4 times. Place the glass crucible and the
precipitate in an electric constant temperature drying oven at 180 °C ± 5 °C; dry for 45
minutes. Take it out; cool it slightly; place it in a dryer; cool it to room temperature.
Weigh it to an accuracy of 0.0002 g.
At the same time, do a blank test. Except for not adding the sample to the blank test
solution, the types and amounts of other reagents added are the same as those of the test
solution.
7.4.5 Test data processing
The phosphorus content is calculated as the mass fraction w2 of phosphorus (P),
according to formula (3).
Wherein.
m1 - The mass of quinoline phosphomolybdic acid precipitate generated by the test
solution, in grams (g);
m2 - The mass of quinoline phosphomolybdic acid precipitate generated by the blank
test solution, in grams (g);
m - The mass of the sample, in grams (g);
0.0140 - The coefficient for converting quinoline phosphomolybdic acid into
phosphorus.
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results is not
Inductively coupled plasma emission spectrometer.
7.6.4 Test steps
7.6.4.1 Drawing of working curve
Pipette 0.00 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of standard
solution (see 7.6.2.2) respectively; place in seven 100 mL volumetric flasks; add 2 mL
of hydrochloric acid to each; dilute to the mark with water; shake well. Introduce into
inductively coupled plasma emission spectrometer for measurement. The wavelength
of the analysis spectrum and instrument working conditions are shown in Appendix A.
Draw the working curve, using the mass concentration (μg/mL) of the standard solution
as the abscissa and the corresponding emission intensity value as the ordinate.
7.6.4.2 Test
Weigh 1 g of specimen (accurate to 0.0002 g); place in a 250 mL beaker; moisten with
a small amount of water; add 20 mL of hydrochloric acid. Cover with a watch glass and
heat at low temperature in a fume hood until almost dry. After cooling, transfer to a 100
mL volumetric flask; dilute to the mark; shake well. Introduce into the inductively
coupled plasma emission spectrometer; measure the emission intensity value of the
corresponding element to be tested under the same conditions as 7.6.4.1.If the spectral
intensity of the test solution exceeds the range of the working curve, the test solution
shall be appropriately diluted and the acidity shall be kept consistent with that before
dilution. Find the mass concentration of the element to be tested in the test solution
from the standard curve.
At the same time, perform a blank test. Except for not adding the sample to the blank
test solution, the type and amount of other reagents added are the same as those of the
test solution.
7.6.5 Test data processing
The content of the elements to be tested (calcium, magnesium, sodium, potassium,
copper, zinc, nickel, manganese, aluminum, titanium, cobalt, lead, chromium) is
calculated as the mass fraction wi of the elements to be tested (Ca, Mg, Na, K, Cu, Zn,
Ni, Mn, Al, Ti, Co, Pb, Cr), according to formula (5).
Where.
ρi - The mass concentration of the element to be tested in the test solution, as found
from the working curve, in micrograms per milliliter (μg/mL);
ρ0 - The mass concentration of the element to be tested in the blank test solution, as
found from the working curve, in micrograms per milliliter (μg/mL);
m - The mass of the sample, in grams (g);
k - The dilution factor of the test solution.
The arithmetic mean of the parallel determination results is taken as the test result. The
absolute difference between the two parallel determination results shall not exceed 10%
of the arithmetic mean.
7.7 Determination of sulfur content
7.7.1 Principle
The specimen is heated and burned in the oxygen flow of a high-frequency induction
furnace. The generated sulfur dioxide is carried by oxygen to the measuring chamber
of the infrared analyzer. Sulfur dioxide absorbs infrared energy of a certain wavelength;
its absorption energy is proportional to its concentration. The sulfur content can be
measured according to the change in the energy received by the detector.
7.7.2 Reagents or materials
According to the provisions of Chapter 4 of GB/T 6730.61-2005.
7.7.3 Instruments and equipment
According to the provisions of Chapter 5 of GB/T 6730.61-2005.
7.7.4 Test steps
Weigh 0.2 g of the specimen burned according to 7.9 (accurate to 0.0002 g); measure
according to the provisions of Chapter 7 of GB/T 6730.61-2005.
7.7.5 Test data processing
According to the provisions of Chapter 8 of GB/T 6730.61-2005.
7.8 Determination of magnetic substance content
7.8.1 Principle
The magnetic substance in the specimen is adsorbed by a magnetic rod and then
dissolved with aqua regia. The intensity of the characteristic spectral lines of the
magnetic substance elements (iron, zinc, nickel, chromium) is determined by an
inductively coupled plasma emission spectrometer; the working curve method is used
for quantification. The content of the magnetic substance is obtained by calculation.
7.8.2 Reagents or materials
Add 150 mL of anhydrous ethanol and 300 mL of water; put in a clean magnetic bar;
cover the bottle cap and tighten it; roll it with a jar mill (speed 110 r/min) for 30 min.
After the mixed adsorption is completed, use a magnet to adsorb the magnetic bar on
the outside of the container; pour out the solution; rinse the magnetic bar with water
(ultrasonic cleaning for 30 seconds if necessary). Transfer the magnetic bar to a 250 mL
beaker; add 15 mL of aqua regia; then add 40 mL of water; cover with a watch glass;
heat to a slight boil on a heating plate. Remove it when it reaches about 10 mL ~ 20 mL;
cool to room temperature. Transfer all the solution to a 100 mL volumetric flask; wash
the magnetic bar 3 times with a small amount of water; pour it into the volumetric flask;
finally dilute it to the scale with water; shake it well. Introduce it into the inductively
coupled plasma emission spectrometer; determine the emission intensity value of the
corresponding element to be measured under the same conditions as 7.8.4.1.Find the
mass concentration of the element to be measured in the test solution from the standard
curve.
At the same time, a blank test is also performed. Except for not adding the sample to
the blank test solution, the types and amounts of other reagents added are the same as
those of the test solution.
7.8.5 Test data processing
The content of the elements to be tested (iron, zinc, nickel, chromium, phosphorus) is
calculated as the mass fraction wj of the elements to be tested (Fe, Zn, Ni, Cr, P),
according to formula (6).
The content of magnetic substances is calculated as the mass fraction w3 according to
formula (7).
In formula (6) and formula (7).
ρj - The mass concentration of the element to be tested in the test solution found
from the working curve, in micrograms per milliliter (μg/mL);
ρ0 - The mass concentration of the element to be tested in the blank test solution
found from the working curve, in micrograms per milliliter (μg/mL);
m - The mass of the sample, in grams (g);
wFe - The iron content of the magnetic substance, calculated according to formula
(6);
wP - The phosphorus (P) content in the iron phosphate adsorbed by the magnetic rod,
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results is not
greater than 0.2%.
7.10 Determination of tap density
The determination shall be carried out according to the method specified in GB/T 5162.
7.11 Determination of particle size
7.11.1 Reagents or materials
Anhydrous ethanol.
7.11.2 Instruments and equipment
7.11.2.1 Laser particle size analyzer. The measuring range shall meet the particle size
range to be detected.
7.11.2.2 Ultrasonic disperser. Power greater than 100 W.
7.11.3 Test steps
According to the requirements of the laser particle size analyzer, weigh a certain amount
of specimen; add 100 mL of water; then add 1.0 mL ~ 1.5 mL of anhydrous ethanol
dispersant; place the specimen solution on the ultrasonic disperser; perform ultrasonic
dispersion for 3 minutes. According to the operating steps of the laser particle size
analyzer, measure the particle size distribution of the specimen; the refractive index is
2.940.Report the measurement results as D50.
7.12 Determination of specific surface area
The measurement is carried out according to the method specified in GB/T 19587.The
adsorption gas is nitrogen; the degassing conditions are 180 °C, 1 h.
8 Inspection rules
8.1 All items specified in the requirements of this document are exit-factory inspection
items and shall be inspected batch by batch.
8.2 The same type of battery iron phosphate produced by the same manufacturer using
the same materials, under basically the same production conditions, in continuous
production or the same team production, forms a batch. Each batch of products shall
not exceed 10 t.
8.3 Determine the number of sampling units according to the provisions of GB/T 6678.
When sampling, insert the sampler vertically from the top of the packaging bag to 3/4
of the depth of the material layer. The sample taken from each bag is not less than 50 g.
Mix the collected samples; reduce them to about 1000 g by quartering method; pack
them into two dry, clean wide-mouth bottles or plastic bags; seal them; stick labels on
them, indicating the manufacturer name, product name, model, batch number, sampling
date, name of the sampler. One bottle (bag) is used for inspection; the other bottle (bag)
is kept for reference; the storage time is determined by the manufacturer based on actual
conditions.
8.4 If any index of the test result does not meet the requirements of this document, re-
sample from twice the amount of packaging for re-inspection. Even if only one index
of the re-inspection result does not meet the requirements of this document, the entire
batch of products shall be unqualified.
8.5 Use the rounded value comparison method specified in GB/T 8170, to determine
whether the test result meets the requirements of this document.
9 Marking and labeling
9.1 The packaging of iron phosphate for batteries shall be firmly and clearly marked,
including. manufacturer name, factory address, product name, model, net content, batch
number or production date, this document number, the "rainproof" and "sunproof" signs
specified in Table 1 of GB/T 191-2008.
9.2 Each batch of iron phosphate for batteries shipped out of the factory shall be
accompanied by a quality certificate, including. manufacturer name, factory address,
product name, model, net content, batch number or production date, proof that the
product quality complies with this document and this document number.
10 Packaging, transportation, storage
10.1 Iron phosphate for batteries is double-layer packed. The inner packaging is a
double-layer polyethylene plastic film bag; the outer packaging is a coated plastic
woven bag. The net content of each bag is 25 kg, 50 kg, 500 kg. It can also be packaged
according to user requirements.
10.2 Iron phosphate for batteries shall be covered during transportation to prevent rain,
moisture, sun exposure.
10.3 Iron phosphate for batteries shall be stored in a cool, dry warehouse.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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