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Method for determining content of 1,3-propanesultone

A propane sultone and content technology, which is applied in the field of analysis and detection, can solve the problems of difficult detection and complex matrix, and achieve the effect of simple content, high recovery rate and precision, and meet the needs of detection

Active Publication Date: 2016-05-25
HEILONGJIANG PONY TESTING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have shown that the matrix of this type of product is complex and difficult to detect

Method used

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  • Method for determining content of 1,3-propanesultone
  • Method for determining content of 1,3-propanesultone
  • Method for determining content of 1,3-propanesultone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In embodiment 1 dye sample, the mensuration of 1,3-propane sultone content

[0031] (1) Analysis steps

[0032] Take 50g dye sample and mix well. Weigh 1.03g and 1.01g samples respectively into 50mL glass centrifuge tubes, add 20mL n-hexane, vortex mix, room temperature ultrasonic extraction for 30min, 8000r / min high-speed centrifugation for 10min, take the supernatant, repeat extraction with 10mL n-hexane to combine the upper layer For the supernatant, use n-hexane to dilute the supernatant to 50mL as the solution to be tested, centrifuge at 8000r / min for 10min at a high speed, measure 2mL at the middle scale of the solution to be tested with a pipette, filter through a 0.22μm nylon filter membrane, and filter the filtrate through Gas chromatography-mass spectrometry analysis.

[0033] (2) Chromatography and mass spectrometry parameters

[0034] Gas chromatographic conditions, adopt chromatographic column DB-5MS, 30m×0.25mm×0.25μm, take 60℃ as the initial temperatur...

Embodiment 2

[0040] The standard substance of embodiment 2 dye sample 1,3-propane sultone adds and measures

[0041] (1) Analysis steps

[0042] Take the 1,3-propane sultone negative sample in Example 1. Weigh six samples of about 1g (accurate to three decimal places) into a 50mL glass centrifuge, add 0.1mL of 1,3-propane sultone standard stock solution of 1000μg / mL each, after standing still for a period of time, add 20mL of n-hexane , 8000r / min high-speed centrifugation for 10min, take the supernatant, repeat extraction with 10mL n-hexane to combine the supernatant, use n-hexane to dilute the supernatant to 50mL as the solution to be tested, 8000r / min high-speed centrifugation for 10min, use a pipette Measure 2 mL at the middle scale of the solution to be tested, filter through a 0.22 μm nylon filter membrane, and analyze the filtrate by gas chromatography-mass spectrometry.

[0043] (2) Instrument conditions

[0044]Gas chromatographic conditions, adopt chromatographic column DB-5MS,...

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Abstract

The invention discloses a method for determining the content of 1,3-propanesultone, belongs to the field of analysis and detection and in particular discloses a method for determining the content of the 1,3-propanesultone by using gas chromatography-mass spectrometry. The method comprises the following steps: putting a proper amount of uniform sample into a glass centrifugal pipe; adding n-hexane and uniformly mixing by vortex; carrying out ultrasonic extraction at a room temperature and centrifuging at a high speed; taking supernatant liquid and repeatedly extracting and combining the supernatant liquid; making the volume constant until the volume is 50mL; centrifuging at a high speed; metering 2mL at a middle scale of a solution to be detected by using a pipette; filtering with a filtering membrane, and carrying out gas chromatography-mass spectrometry analysis; quantifying with an external standard method. The method disclosed by the invention is simple and rapid, and accurate in qualitative and quantitative properties; the interference of sample matrix is effectively avoided and detection requirements can be met.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and relates to a method for measuring the content of 1,3-propane sultone, in particular to a method for measuring the content of 1,3-propane sultone by gas chromatography-mass spectrometry. Background technique [0002] 1,3-Propane sultone is an important pharmaceutical intermediate and electronic chemical. Its structure contains unsaturated bonds and heteroatoms. This unique structure makes it irreplaceable in the synthesis of heterocyclic drugs. In recent years, 1,3-propane sultone has been widely used as an additive for lithium battery electrolyte, which can improve battery performance and greatly extend the rechargeable life of the battery. 1,3-propane sultone is also used in bright Agents, dyes, diionic surfactants, sulfonating agents, etc. In the presence of water, this compound slowly hydrolyzes to the corresponding corrosive hydroxysulfonic acid, which decomposes on heating to produ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 宋薇高俊海
Owner HEILONGJIANG PONY TESTING TECH CO LTD
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