CN107290449A - Three in a kind of textile（2 chloroethyls）The quick selective mechanisms method of phosphate - Google Patents
Three in a kind of textile（2 chloroethyls）The quick selective mechanisms method of phosphate Download PDFInfo
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- CN107290449A CN107290449A CN201710453262.7A CN201710453262A CN107290449A CN 107290449 A CN107290449 A CN 107290449A CN 201710453262 A CN201710453262 A CN 201710453262A CN 107290449 A CN107290449 A CN 107290449A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a kind of in textile three quick selective mechanisms methods of (2 chloroethyl) phosphate, it is characterised in that；Comprise the following steps, (1) preparation of samples：Textile to be measured is ground into fritter, sample is loaded to the cracking tube stage casing for cracking instrument probe；(2) sample dissociation：Thermal cracking instrument probe final temperature：290℃；Programming rate：20℃/millisecond；Pyrolysis time is 40s；(3) GC analysis conditions：(4) Mass Spectrometry Conditions：Chromatographic mass spectrometry interface temperature：320℃；Ionization mode：EI；Ionization voltage：70eV；Ion source temperature：300℃.This method is simple to operate, and using Thermal desorption Gas-phase acidity technology, in textile three (2 chloroethyl) phosphates are used for quickly detecting.Qualitative and half-quantitative detection sensitive, accurately and efficiently can be carried out in textile three (2 chloroethyl) phosphates, favorable reproducibility, sensitivity high the advantages of high with the rate of recovery.
Description
Technical field
The present invention relates to a kind of in detection method technical field, more particularly to textile three (2- chloroethyls) phosphates are quick
Selective mechanisms method.
Background technology
Statement in this part merely provides the background information relevant with present disclosure, thereby increases and it is possible to do not constitute
Prior art.
In the prior art on detect three (2- chloroethyls) phosphates (TCEP) national standard, only several industry marks
It is accurate：(1) three in toy material (2- chloroethyls) phosphate measure GC-MS methods (SN/T 3621-2013)；(2) weaving is imported and exported
The detection method (SN/T 3228-2012) of organophosphorous fire retardant in product；(3) phosphoric acid ester in bonding agent for building is imported and exported to increase
Mould the measure (SN/T 3352-2012) of agent；And one, Chinese invention patent " leather and its product in tricresyl phosphate (2- chloroethyls)
The assay method of ester " (application number： CN201310648842.3).
The detection of three (2- chloroethyls) phosphates is mostly derived from the REACH regulations limitation of European Union in current textile.It is domestic right
The detection of the compound only has professional standard.The commodity related generally in professional standard have toy, textile and bonding agent, its point
Analysis method generally uses organic solvent extraction-purification-Instrumental Analysis.Method is used first with ultrasonic extraction method to sample in patent
Product carry out pre-treatment, obtain extract；Then the mixed type bonded silica gel containing carboxyl and chain alkyl is used, is extracted as solid phase
Take pillar to carry out purification enrichment to extract, TCEP contents are finally determined using GC-MS.
According to existing professional standard and patent, such analysis method key step includes：Pre-treatment：Testing sample is put into
Organic solvent is dissolved and handled, and obtains being dissolved with the detected solution of three (2- chloroethyls) phosphates, and gas phase is used after purification
Chromatography mass spectrometry carries out assay.Its subject matter existed has：1. sample pretreatment process is cumbersome, tediously long, time-consuming, no
Fast and efficiently analysis can be met to require.2. using substantial amounts of poisonous and harmful organic solvent, serious shadow is caused to human body, environment
Ring.Cracking sample introduction-low-polarity components can solve the quick analysis problem of (2- chloroethyls) phosphate three in sample.Crack into
Sample-low-polarity components can Direct solid sampling, greatly simplify operating procedure, can more efficiently rapid screening textile whether
Contain three (2- chloroethyls) phosphates.
Therefore prior art is urgently improved and developed.
The content of the invention
The technical problem to be solved in the present invention is to provide the spinning that one kind is simple, quick, feasible, and selectivity is high, the rate of recovery is high
The quick selective mechanisms method of (2- chloroethyls) phosphate three in fabric.
The present invention technical solution be：
The quick selective mechanisms method of (2- chloroethyls) phosphate, comprises the following steps three in a kind of textile,
(1) preparation of samples：Textile to be measured is ground into fritter, sample is loaded to the cracking tube stage casing for cracking instrument probe；
(2) sample dissociation：Thermal cracking instrument probe final temperature：270℃-300℃；Programming rate：20℃/
millisecond；Pyrolysis time is 40s；
(3) GC analysis conditions：Chromatographic column：30m*0.25mm*0.25 μm of quartz capillary column；Injector temperature：280℃；
Carrier gas：Helium, purity >=99.999%, flow velocity 1.8mL/min, split ratio 100:1；GC/MS temperature programmings：90 DEG C of initial temperature, is protected
Temperature 1 minute；320 DEG C are warming up to 20 DEG C/min, 5.5 minutes are incubated；
(4) Mass Spectrometry Conditions：Chromatography-mass spectroscopy interface temperature：320℃；Ionization mode：EI；Ionization voltage： 70eV；Ion gun
Temperature：300℃；Transmission line temperature：280℃；Solvent-free delay；Mensuration mode：Total ion chromatogram (TIC) is qualitative, quality
Scanning range：M/Z=33~1000, selection ion detection (SIM) is quantitative；Select ion：Quota ion (m/z：249) it is, qualitative
Ion (m/z：143,205,223)；Determine whether thermal decomposition product is object by retention time and mass spectrometric data library searching.
Beneficial effects of the present invention：
The invention provides three (2- chloroethyls) phosphorus in a kind of textile based on Thermal desorption-gas phase-mass spectrometric hyphenated technique
The quick selective mechanisms method of acid esters poisonous and harmful substance.This method is simple to operate, utilizes Thermal desorption-gas phase-mass spectrometry skill
In textile three (2- chloroethyls) phosphates are used for quickly detecting by art.Can it is sensitive, accurately and efficiently in textile three
(2- chloroethyls) phosphate carries out qualitative and half-quantitative detection, high with the rate of recovery, favorable reproducibility, the advantages of sensitivity is high.
Embodiment
Embodiment：
The invention provides three (2- chloroethyls) phosphorus in a kind of textile based on Thermal desorption-gas phase-mass spectrometric hyphenated technique
The quick selective mechanisms method of acid esters poisonous and harmful substance.This method is simple to operate, utilizes Thermal desorption-gas phase-mass spectrometry skill
In textile three (2- chloroethyls) phosphates are used for quickly detecting by art.Can it is sensitive, accurately and efficiently in textile three
(2- chloroethyls) phosphate carries out qualitative and half-quantitative detection, high with the rate of recovery, favorable reproducibility, the advantages of sensitivity is high.
Detection method：
(1) preparation of samples：Textile to be measured is ground into fritter, 10-20mg one-piece sample is weighed, sample is loaded and split
The cracking tube stage casing of instrument probe is solved, and fixation is clogged with silica wool；
(2) sample dissociation：Thermal cracking instrument probe final temperature：270℃-300℃；Programming rate：20℃/
millisecond；Pyrolysis time is 40s；Preferably thermal cracking instrument probe final temperature：290℃.
(3) GC analysis conditions：Chromatographic column：30m*0.25mm*0.25 μm of quartz capillary column；Injector temperature：280℃；
Carrier gas：Helium, purity >=99.999%, flow velocity 1.8mL/min, split ratio 100:1；GC/MS temperature programmings：90 DEG C of initial temperature, is protected
Temperature 1 minute.320 DEG C are warming up to 20 DEG C/min, 5.5 minutes are incubated；
(4) Mass Spectrometry Conditions：Chromatography-mass spectroscopy interface temperature：320℃；Ionization mode：EI；Ionization voltage： 70eV；Ion gun
Temperature：300℃；Transmission line temperature：280℃；Solvent-free delay；Mensuration mode：Total ion chromatogram (TIC) is qualitative, quality
Scanning range：M/Z=33~1000, selection ion detection (SIM) is quantitative；Select ion：Quota ion (m/z：249) it is, qualitative
Ion (m/z：143,205,223)；Determine whether thermal decomposition product is object by retention time and mass spectrometric data library searching.
The detection method of the present invention, using Thermal desorption method, makes (2- chloroethyls) phosphate three in textile fully discharge,
And Thermal desorption product is detected by gas phase-mass spectrometry so that conclude three in textile the composition of (2- chloroethyls) phosphate and
Content.
In the description of this specification, the description of term " one embodiment " etc. means that combining the embodiment or example describes
Specific features, structure, material or feature be contained in the present invention at least one embodiment or example in.In this manual,
Identical embodiment or example are not necessarily referring to the schematic representation of above-mentioned term.Moreover, the specific features of description, knot
Structure, material or feature can in an appropriate manner be combined in any one or more embodiments or example.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (2)
1. a kind of quick selective mechanisms method of (2- chloroethyls) phosphate three in textile, it is characterised in that；Comprise the following steps,
(1) preparation of samples：Textile to be measured is ground into fritter, sample is loaded to the cracking tube stage casing for cracking instrument probe；
(2) sample dissociation：Thermal cracking instrument probe final temperature：270℃-300℃；Programming rate：20℃/millisecond；Heat
The solution time is 40s；
(3) GC analysis conditions：Chromatographic column：30m*0.25mm*0.25 μm of quartz capillary column；Injector temperature：280℃；Carrier gas：
Helium, purity >=99.999%, flow velocity 1.8mL/min, split ratio 100:1；GC/MS temperature programmings：90 DEG C of initial temperature, is incubated 1 point
Clock；320 DEG C are warming up to 20 DEG C/min, 5.5 minutes are incubated；
(4) Mass Spectrometry Conditions：Chromatography-mass spectroscopy interface temperature：320℃；Ionization mode：EI；Ionization voltage：70eV；Ion source temperature：
300℃；Transmission line temperature：280℃；Solvent-free delay；Mensuration mode：Total ion chromatogram (TIC) is qualitative, mass scanning model
Enclose：M/Z=33~1000, selection ion detection (SIM) is quantitative；Select ion：Quota ion (m/z：249), qualitative ion (m/
z：143,205,223)；Determine whether thermal decomposition product is object by retention time and mass spectrometric data library searching.
2. the quick selective mechanisms method of (2- chloroethyls) phosphate three in textile according to claim 1, its feature exists
In；Thermal cracking instrument probe final temperature is 290 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710453262.7A CN107290449B (en) | 2017-06-15 | 2017-06-15 | Rapid screening and detecting method for tris (2-chloroethyl) phosphate in textile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710453262.7A CN107290449B (en) | 2017-06-15 | 2017-06-15 | Rapid screening and detecting method for tris (2-chloroethyl) phosphate in textile |
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| Publication Number | Publication Date |
|---|---|
| CN107290449A true CN107290449A (en) | 2017-10-24 |
| CN107290449B CN107290449B (en) | 2020-09-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710453262.7A Active CN107290449B (en) | 2017-06-15 | 2017-06-15 | Rapid screening and detecting method for tris (2-chloroethyl) phosphate in textile |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112858537A (en) * | 2021-04-14 | 2021-05-28 | 上海市质量监督检验技术研究院 | Rapid detection method for permethrin in anti-mosquito fabric |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776663A (en) * | 2010-02-05 | 2010-07-14 | 谱尼测试科技（北京）有限公司 | Method for determining content of tris (2-chloroethyl) phosphate |
| CN102288690A (en) * | 2011-05-12 | 2011-12-21 | 通标标准技术服务(上海)有限公司 | Method for determining content of tri (2-chloroethyl) phosphate |
| CN106770820A (en) * | 2016-12-12 | 2017-05-31 | 谱尼测试科技(天津)有限公司 | Three kinds of detection methods of phosphorus flame retardant in a kind of polyurethane foam product |
-
2017
- 2017-06-15 CN CN201710453262.7A patent/CN107290449B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776663A (en) * | 2010-02-05 | 2010-07-14 | 谱尼测试科技（北京）有限公司 | Method for determining content of tris (2-chloroethyl) phosphate |
| CN102288690A (en) * | 2011-05-12 | 2011-12-21 | 通标标准技术服务(上海)有限公司 | Method for determining content of tri (2-chloroethyl) phosphate |
| CN106770820A (en) * | 2016-12-12 | 2017-05-31 | 谱尼测试科技(天津)有限公司 | Three kinds of detection methods of phosphorus flame retardant in a kind of polyurethane foam product |
Non-Patent Citations (2)
| Title |
|---|
| KRZYSZTOF LANIEWSKI等: "Pyrolysis–gas chromatography of chloroorganic compounds in precipitation", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| NATHALIE HAYECK等: "Validation of thermodesorption method for analysis of semi-volatile organic compounds adsorbed on wafer surface", 《TALANTA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112858537A (en) * | 2021-04-14 | 2021-05-28 | 上海市质量监督检验技术研究院 | Rapid detection method for permethrin in anti-mosquito fabric |
| CN112858537B (en) * | 2021-04-14 | 2023-09-05 | 上海市质量监督检验技术研究院 | Quick detection method for permethrin in anti-mosquito fabric |
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| CN107290449B (en) | 2020-09-18 |
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