GB/T 33828-2017 (GB/T33828-2017, GBT 33828-2017, GBT33828-2017)
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Determination of contents of Fe (Ⅲ) in nano lithium iron phosphate
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GB/T 33828-2017
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| Standard ID | GB/T 33828-2017 (GB/T33828-2017) | | Description (Translated English) | Determination of contents of Fe (��) in nano lithium iron phosphate | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G12 | | Classification of International Standard | 71.060.50 | | Word Count Estimation | 9,915 | | Date of Issue | 2017-05-31 | | Date of Implementation | 2017-12-01 | | Quoted Standard | GB/T 601-2002; GB/T 603; GB/T 6682-2008 | | Proposing organization | Chinese Academy of Sciences | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, China National Standardization Administration Committee | | Summary | This standard specifies the principle, equipment, reagents, steps and test report contents of ferric iron content in lithium iron phosphate. This standard is applicable to the determination of trivalent iron in the range of 0.2% to 5.0% of potassium ferric phosphate. |
GB/T 33828-2017
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Determination of contents of Fe (III)
in nano lithium iron phosphate
ISSUED ON. MAY 31, 2017
IMPLEMENTED ON. DECEMBER 01, 2017
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
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Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Test principles ... 4
4 Equipment ... 5
5 Reagent ... 6
6 Test and calculation ... 7
7 Repeatability ... 10
8 Test report ... 11
Appendix A (Informative) Trivalent iron qualitative test method ... 12
Foreword
This standard was drafted in accordance with the rules given in GB/T
1.1-2009.
This standard was proposed by the Chinese Academy of Sciences.
This standard shall be under the jurisdiction of the National Nanotechnology
Standardization Technical Committee of Nano Materials Subcommittee
(SAC/TC 279 /SC 1).
The drafting organizations of this standard. Shenzhen BTR New Energy
Materials Co., Ltd., Hefei Guoxuan Hi-Tech Power Co., Ltd., Henan Kelong
New Energy Co., Ltd., Shenzhen BTR Nami Technology Co., Ltd., Tianjin BTR
New Energy Technology Co., Ltd., Metallurgical Industry Information
Standards Institute.
The main drafters of this standard. Huang Youyuan, Yue Min, Xu Xiaoming,
Cheng Di, Dai Shifeng, Gao Yingquan, Xie Ailiang, Xu Yunjun, Li Xiaojun, Liu
Xiuming, Chen Nanmin.
Determination of contents of Fe (III)
in nano lithium iron phosphate
1 Scope
This standard specifies the principle, equipment, reagents, procedures and
test report contents for the method of determination of trivalent iron content in
nano lithium iron phosphate.
This standard is applicable to the determination of trivalent iron in nano lithium
iron phosphate in the range of 0.2% ~ 5.0%.
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) are applicable to this Standard.
GB/T 601-2002 Chemical reagent - Preparation of standard volumetric
solutions
GB/T 603 Chemical reagent - Preparation of reagent solutions for use in
test methods
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods
3 Test principles
The difference between the mass fraction of total iron and the mass fraction of
ferrous iron in the sample is the mass fraction of trivalent iron content in the
sample.
First USE the hydrochloric acid to dissolve the sample to be tested to form a
solution; respectively TAKE two sets of solution sample, 20.00 mL for each set.
TAKE one set of sample solution; under the acidic condition (pH controlled at 1
~ 2), USE the SnCl2 solution to reduce most of the Fe (III); ADD the CuSO4-
isatin indicator; AND the solution changes from yellow to green; USE the TiCl3
solution to reduce the Fe (III) of the remaining part; the slightly excessive TiCl3
5 Reagent
WARNING. Some of the reagents used in this test method are toxic or
corrosive AND shall be handled with care!
5.1 General requirements
Unless otherwise specified, it shall use the analytical reagents and level 3
water as specified in GB/T 6682-2008. AND all the reagents shall be prepared
in accordance with the requirements of GB/T 603.
5.2 Hydrochloric acid
The mass fraction is more than 36%.
5.3 Sulfuric acid
The mass fraction is more than 98%.
5.4 Phosphoric acid
The mass fraction is more than 85%.
5.5 Hydrochloric acid solution (1 + 1)
MEASURE the equal volume of hydrochloric acid (5.2) and water; MIX it
uniformly to prepare for use.
5.6 Sulfur phosphoric acid solution (15%)
Slowly ADD 150 mL of sulfuric acid (5.3) into 500 mL of water while stirring;
after cooling it down, ADD 150 mL of phosphoric acid (5.4); USE water to dilute
it to 1000 mL; MIX it uniformly.
5.7 Tin dichloride solution
WEIGH 5 g of tin chloride; DISSOLVE it in 10 mL of hydrochloric acid solution
(5.5); USE water to dilute it to 100 mL; AND the solution shall be filtered if it is
turbid.
5.8 Potassium dichromate standard titration solution [c(1/6 K2Cr2O7) =
0.0500 mol/L]
PREPARE it in accordance with the method II in clause 4.5.2 of GB/T
601-2002.
5.9 Titanium trichloride solution
heating device to heat it slightly boiling for 30 min; TAKE it off and quickly ADD
approximately 1.0 g of sodium bicarbonate (5.16) and 30 mL of water; USE
water bath to cool it quickly to room temperature.
6.1.2 PLACE the medium-speed filter paper in a 100.00 mL volumetric flask;
USE water to rinse the volumetric flask for 3 ~ 4 times; RINSE the precipitate
for 3 ~ 4 times; MAKE its volume reach to the mark; SHAKE it uniformly to
prepare for use.
6.2 Determination of total iron content in sample solution
6.2.1 USE the single-line pipette (4.3) to accurately pipette 20.00 mL of the
newly prepared sample solution (6.1.2) into a 250 mL conical flask; ADD 30 mL
of water and 2 mL of hydrochloric acid (5.5); SHAKE it uniformly and PLACE it
on the heating device to heat it to boil for 30 s; TAKE it off; immediately ADD tin
dichloride solution (5.7) until the solution is pale yellow (if the solution itself is
yellow but not apparent, it can skip this step); then ADD 2 drops of copper
sulphate-isatin indicator (5.13) and the solution turns green; ADD titanium
trichloride solution (5.9) until the green disappears; ADD one more drop; LET it
stand; COOL it down.
6.2.2 After the solution is cooled to room temperature, it changes into blue;
ADD 20 mL of sulfur phosphoric acid solution (5.6) and 4 drops of
diphenylamine sulfonate indicator (5.14); USE the potassium dichromate
standard titration solution (5.8) for titration, until the solution changes from
green to purple, which is the end point; RECORD the volume of the consumed
potassium dichromate V.
6.2.3 USE the single-line pipette (4.4) to accurately pipette 5.00 mL of ferrous
ammonium sulfate solution (5.15) to perform blank test together with the
sample. USE the potassium dichromate standard titration solution (5.8) for
titration, until the solution changes from green to purple, which is the end point;
RECORD the volume of the consumed potassium dichromate standard
titration solution as V1; then ADD 5.00 mL of ammonium ferrous sulfate
solution (5.15); USE the potassium dichromate standard titration solution for
titration, until the solution changes from green to purple, which is the end point;
RECORD the volume of the consumed potassium dichromate standard
titration solution as V2.
Calculate the mass fraction of total iron in the sample in accordance with the
formula (4).
V3 - Volume of potassium dichromate standard titration solution consumed
for the titration of the ferrous iron in the sample solution, in milliliters (mL);
V1 - Volume of potassium dichromate standard titration solution consumed
for the titration of blank solution 1 (ADD 5.00 mL of ferrous ammonium
sulfate solution into the blank solution), in milliliters (mL);
V2 - Volume of potassium dichromate standard titration solution consumed
for the titration of blank solution 2 (TITRATE the blank solution 1 to the end
point and ADD 5.00 mL of ammonium ferrous sulfate solution), in milliliters
(mL);
55.84 - Molar mass of iron in grams per mole (g/mol);
m - The mass of the weighed sample, in grams (g).
6.4 Calculation of trivalent iron content in sample
CALCULATE the mass fraction of trivalent iron in the sample in accordance
with the formula (6).
Where.
WFe3+ - Mass fraction of trivalent iron in the sample, expressed in %
WFe - Mass fraction of total iron in the sample, expressed in %
WFe2+ - Mass fraction of ferrous iron in the sample, expressed in %.
7 Repeatability
7.1 This method does not have a suitable standard sample for determining the
deviation, so the repeatability is determined by repeated testing.
7.2 USE the same sample for the test in 4 laboratories, AND the
inner-laboratory and inter-laboratory sample average value and standard
deviation are respectively as shown in Table 1.
Table 1 -- Inner-laboratory and inter-laboratory sample average and
standard deviation
Item Requirements
Inter-laboratory average value 1.24%
Inter-laboratory standard deviation 0.052%
......
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