YS/T 1028.3-2015 in English

VALID

Methods for chemical analysis of lithium iron phosphate―Part 3:Determination of phosphor content―Quinoline phosphomolybdate gravimetry

Issued on:2015-04-30
Implemented on:2015-10-01
File Format:PDF
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Standard No:	YS/T 1028.3-2015
Document status:	VALID
Title in English:	Methods for chemical analysis of lithium iron phosphate―Part 3:Determination of phosphor content―Quinoline phosphomolybdate gravimetry
Title in Chinese:	磷酸铁锂化学分析方法第3部分：磷量的测定磷钼酸喹啉称量法
Language:	English
File Format:	Electronic (PDF)
Delivery:	Via email within 1~3 business days
Issued on:	2015-04-30
Implemented on:	2015-10-01
ICS Classification:	77.120.99-Other non-ferrous metals and their alloys
Chinese Classification:	H71-Metal and alloy powder
Professional Classification:	YS-Non-ferrous Metal
Related Keywords:	lithium iron phosphate lithium iron phosphate ― part lithium determination determination method phosphor content ― quinoline phosphomolybdate gravimetry introduction standard technical background
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Phosphate Consistency Phosphorylation site mass spectrometry analysis Determination method of ferric iron in ferric phosphate Inorganic phosphorus analysis method Detection of lithium iron phosphate Molybdic acid detection method Phosphoric acid purity detection method Iron phosphate detection National standard method for phosphoric acid detection Lithium iron phosphate fluoride content Lithium iron phosphate national standard analysis method Enzymatic Cell Chemistry Methods for Lead Phosphate Sugar phosphorylation detection method Quality after phosphating Lithium iron phosphate industry Lithium iron phosphate metal foreign matter Interference of total phosphorus determination method for molybdate fraction Determination methods and principles of phosphorus The preferred method for determination of chloroquine phosphate content National standard measurement method for total phosphorus Phosphoric acid gravimetric detection method Lithium iron phosphate product quality Total fluorine content in lithium iron phosphate Method for synthesizing lithium iron phosphate from lithium carbonate Basis for manual determination of phosphine Lithium phosphate related Lithium Iron Phosphate International Comparison of Lithium Iron Phosphate Digestion Methods How to identify phosphate radicals Test method for hypophosphorous acid content Lithium iron phosphate detection method Method for welding lithium iron phosphate between copper and nickel Potassium phosphate content determination method Iron Phosphate Purchase Cyclic Phosphate Detection Method Iron phosphide detection Lithium phosphate testing standards Ferric Phosphate Flake Group Phosphate determination method ammonium molybdate Iron phosphate national quality Test method for iron content of ferric phosphate Determination method of lithium carbonate by weighing method Lithium iron phosphate industry Method for detecting chloroquine phosphate Analysis and calculation method of chemical nickel for medium phosphorus iron 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Organophosphoric acidification Aluminum phosphate content test method Measurement method of organic phosphorus Ferric pyrophosphate preparation method ys/t3503-2015

本部分规定了磷酸铁锂中磷量的测定方法。本部分适用于磷酸铁锂中磷含量的测定。测定范围：16%～20%。

Introduction

Standard Technical Background

With the rapid development of lithium-ion battery industry, lithium iron phosphate is the mainstream positive electrode material, and the accurate determination of its chemical composition directly affects the battery performance. As the third part of the YS/T1028 series, this standard specifically regulates the determination method of phosphorus, and together with the flame photometry method for lithium determination and ICP-AES method for impurity elements, it constitutes a complete material analysis system.

Detailed explanation of the method principle

In nitric acid medium, phosphate ions react with quinomolybdic acid reagent to generate yellow precipitate quinoline phosphomolybdate ((C₉H₇N)₃H₃[PO₄·12MoO₃]), and its chemical reaction equation is:

PO₄^3- + 12MoO₄^2- + 3C₉H₇N + 24H⁺ → (C₉H₇N)₃H₃[PO₄·12MoO₃]↓ + 12H₂O

Method parameters	This method	Spectrophotometry	ICP-OES method
Detection range	16-20%	0.01-5%	0.001-10%
Precision (RSD)	≤0.3%	1-3%	0.5-2%
Equipment requirements	General laboratory equipment	Spectrophotometer	Plasma spectrometer

Key operating points

1. Reagent preparation specifications

The preparation of quinomolybdate reagent must be strictly carried out in accordance with clause 3.4:

Sodium molybdate in solution A must be completely dissolved
Solution D needs to be stirred slowly when quinoline is added
The final reagent must be stored in a polyethylene container

2. Precipitation condition control

Note in step 6.4.2:

The micro-boiling temperature should be controlled at 80-90℃
Maintain continuous stirring
The insulation time should be strictly controlled at 2-3min

Error control strategy

According to clause 8.1 of the standard, the actual test should focus on:

The difference between parallel samples should be less than the repeatability limit specified in Table 1 (e.g. r=0.09% when 17.96%)
The allowable difference between laboratories is 0.30%
The cooling time of the dryer should be controlled at 30±5min for constant weight operation

Implementation suggestions

For laboratories of lithium battery manufacturers:

Establish a reagent validity management system (it is recommended that quinoline reagent should not be stored for more than 2 months)
Perform regular G4 crucible aperture inspections (use standard substances to verify recovery)
It is recommended to add two temperature points of 167°C and 193°C to verify the effect of drying temperature

More samples: DL/T 5154-2012 JJG 21-2008 YD/T 3934-2021

Sample only — not a preview of YS/T 1028.3-2015

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