CN106018588A - Method for measuring bis(4-bromophenyl)ether in textiles - Google Patents
Method for measuring bis(4-bromophenyl)ether in textiles Download PDFInfo
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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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas 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
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- G01N2030/062—Preparation extracting sample from raw material
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Abstract
A method for measuring bis(4-bromophenyl)ether in textiles comprises the steps that a proper solvent is selected to perform extraction on a sample, and bis(4-bromophenyl)ether in the sample is extracted into a solution; then, a gas chromatograph-mass spectrometer (GC-MS) is used for analyzing whether bis(4-bromophenyl)ether is contained in the sample or not and analyzing the content of bis(4-bromophenyl)ether. The method is easy and convenient to implement, and a large amount of research shows that the method is high in accuracy and excellent in repeatability and reproducibility.
Description
Technical field
The invention belongs to textile inspection field, particularly in a kind of textile 4, the survey of 4 '-dibromo diphenyl ester
Determine method.
Background technology
Along with constantly expanding and demand increasing of textile application field, the textile fire caused
Calamity is also continuously increased.According to statistics, textile the fire caused accounts for more than half of fire sum, especially
Being building home fire, textile fire spread and is caused the ratio shared by fire bigger, bedding and indoor
Decorative textile product is main cause on fire.Therefore, developed country is the most right as far back as the 60-70 age in 20th century
Textile proposes flame-retardancy requirements, and has formulated flame-retardant standard and the regulation of all kinds of textile.
The flame treatment of textile is that some precursor (such as terylene, cotton synthetic fibre, acrylon) being flammable itself are added certain
Plant fire retardant so that it is the free radical in suppression combustion process；Or the thermal decomposition process of change fiber, promote
Dehydration carbonization；Some is then to make fire retardant decomposition discharge non-flammable compressive gas to cover at fiber surface, plays isolation sky
Gas effect.Wherein add fire retardant textile carrying out flame treatment is a kind of relatively conventional method.At present,
China has developed the BACN of a series of great variety of goods, excellent performance.
Textile is commonly used fire retardant and is divided into by contained ignition-proof element: halogen containing flame-retardant, in pyrolytic process, decomposes
X and HX, HX that go out capture transmission burning free radical can dilute the fuel gas produced when fiber cracks,
Or cut off and the contacting of air；Phosphonium flame retardant, produces phosphoric anhydride or phosphoric acid, promotes weaving in combustion process
Product dehydration carbonization, stops or reduces fuel gas producing, additionally, phosphoric anhydride forms similar glass when pyrolysis
The fused mass of shape covers on fabric, promotes its oxidation to generate carbon dioxide, plays fire retardation；Nitrogenous resistance
Combustion agent, nitrogen compound can promote to interlink into charcoal with cellulose effect, reduce the decomposition temperature of fabric, produce
Raw non-flammable compressive gas, plays the effect of dilution fuel gas.
4,4 '-dibromo diphenyl ester is then a kind of BACN, is applied to the resistance of textile frequently as fire retardant
Combustion processes.But human contact can cause skin irritation to 4,4 '-dibromo diphenyl ester, cause gi system
And respiratory tract disease, severe patient can cause body dead.Accordingly, it would be desirable to strictly control 4,4 '-dibromo hexichol
Ester content in textile, and the most accurately detecting its content is to realize accurately controlling it to contain in textile
The key factor of amount.But, the most not yet find detection 4,4 '-dibromo diphenyl ester content in textile
The relevant report of method.
Summary of the invention
An object of the present invention is to provide the assay method of 4,4 '-dibromo diphenyl ester in a kind of textile.
The method of the present invention by select suitable solvent by sample extraction so that it is in 4,4 '-dibromo diphenyl ester extract
Take to solution, then be analyzed in sample whether containing with gas chromatograph-mass spectrometer (GC-MS) (GC-MS)
4,4 '-dibromo diphenyl ester and content thereof.The method of the present invention is easy, and shows through numerous studies, the present invention's
Method accuracy is high, repeated and repeatability is excellent.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
In a kind of textile 4, the assay method of 4 '-dibromo diphenyl ester, comprise the steps:
A sample treatment is become every arbitrary dimension less than 10mm, such as 2mm, 5mm, 8mm by ()
Deng granule；
Sample b step (a) is processed by () after puts into sealing in organic solvent, extraction；Sample and organic solvent
Ratio is 1:10-50g/mL, such as 1:12g/mL, 1:16g/mL, 1:19g/mL, 1:23g/mL, 1:29
G/mL, 1:35g/mL, 1:41g/mL, 1:48g/mL etc.；
C () has extracted after, with organic solvent constant volume used by step (b) after solution is concentrated；After described constant volume
Volume and sample quality are than for 5-20:1mL/g, such as 7:1mL/g, 11:1mL/g, 17:1mL/g etc.；
D solution after step (c) constant volume is carried out GC-MS analysis by ()；
Wherein the chromatographic column of GC-MS is DB-5MS；When GC-MS analyzes, the temperature programmed control of GC part sets
Being set to: initial temperature 100-120 DEG C, for example, 103 DEG C, 107 DEG C, 112 DEG C, 116 DEG C etc. keep 0.5-2min,
For example, 0.7min, 1.6min etc., with 20-40 DEG C/min, for example, 23 DEG C/min, 26 DEG C/min, 31 DEG C
/ min, 35 DEG C/min, 38 DEG C/min etc. rise to 230-270 DEG C, for example, 233 DEG C, 238 DEG C, 244 DEG C,
252 DEG C, 259 DEG C, 266 DEG C etc., keep more than 4min, for example, 4.5min, 5.5min, 8min etc.；
Injector temperature is 280-320 DEG C, for example, 283 DEG C, 288 DEG C, 295 DEG C, 301 DEG C, 307 DEG C, 313 DEG C,
317 DEG C etc..
The present invention uses organic solvent to extract textile samples, thickening filtration extract, uses gas chromatogram matter
Spectrum combined instrument detects.Qualitative analysis is carried out, by quota ion by chromatographic retention and mass spectrum
Intensity and standard solution contrast, and accurately calculate in sample 4, the content of 4 '-dibromo diphenyl ester.
The present invention by substantial amounts of determined use extraction then carry out GC-MS analyze can be accurate, can
Obtain in textile 4 leaned on, the content of 4 '-dibromo diphenyl ester, the solvent wherein extracted and the choosing of proportioning thereof
Taking the extraction completely to 4,4 '-dibromo diphenyl ester has important impact, solvent and proportioning thereof to select and chromatograph
The accuracy of analysis result and repeatability, repeatability are had a major impact by setting of condition.
As optimization technique method, assay method of the present invention, in step (a), sample treatment becomes every to appoint
Dimension is smaller in size than the granule of 6mm.
As optimization technique method, assay method of the present invention, organic solvent described in step (b) is two
Chloromethanes and/or acetone.
Preferably, described extraction uses ultrasonic extraction.
Preferably, the time of described extraction is more than 0.5h, for example, 0.7h, 1.1h, 1.5h, 2.4h
Deng, preferably 1-3h.
Preferably, the ratio of sample and organic solvent is 1:20-40g/mL, for example, 1:22g/mL, 1:26
G/mL, 1:31g/mL, 1:35g/mL, 1:38g/mL etc., preferably 30g/mL.
As optimization technique method, assay method of the present invention, step (c) is done blank experiment simultaneously.
Preferably, the volume after described constant volume and sample quality are than for 10:1mL/g.
As optimization technique method, assay method of the present invention, chromatographic column described in step (d) is
DB-5MS, preferably specification are 30m*0.25mm*0.25 μm.
Preferably, when GC-MS analyzes, carrier gas is high-purity helium, and post flow is 1.5-2.0ml/min, for example,
1.6ml/min, 1.8ml/min, 1.95ml/min etc., preferably 1.7ml/min.
Preferably, when GC-MS analyzes, the temperature programmed control of GC part is set to: initial temperature 110 DEG C holding
1min, rises to 250 DEG C with 30 DEG C/min, keeps 5min.
Preferably, when GC-MS analyzes, the condition setting of MS part is: ionization mode is electron impact ionization,
Ion source temperature 210-250 DEG C, for example, 212 DEG C, 219 DEG C, 225 DEG C, 234 DEG C, 247 DEG C etc., solvent
Postpone 2-4min, for example, 2.2min, 2.6min, 3.2min, 3.7min etc., makings interface temperature
255-290 DEG C, mode determination is for selecting ion scan pattern qualitative and quantitative analysis, sweep limits 40 to 500
amu；Being preferably ionization mode is electron impact ionization, ion source temperature 230 DEG C, solvent delay 3min,
Makings interface temperature 270 DEG C, mode determination is for selecting ion scan pattern qualitative and quantitative analysis, sweep limits
40 to 500amu.
When GC-MS analyzes, initially set up 4, the working curve of 4 '-dibromo diphenyl ester, try to achieve 4,4 '-dibromo
The regression equation of diphenyl ester concentration relationship；Draw sample and blank solution the most respectively, obtain 4,4 '-dibromo
The regression equation made by peak intensity substitution of diphenyl ester, finally tries to achieve in sample blank solution and test liquid
4, the concentration of 4 '-dibromo diphenyl ester, and then calculate in textile 4, the content of 4 '-dibromo diphenyl ester.
As preferably, assay method of the present invention, comprise the steps:
A sample treatment is become the every arbitrary dimension granule less than 10mm by ()；
Sample b step (a) is processed by () after puts into sealing in organic solvent, extraction；Sample and organic solvent
Ratio is 1:10-50g/mL；
C () has extracted after, with organic solvent constant volume used by step (b) after solution is concentrated；After described constant volume
Volume and sample quality are than for 5-20:1mL/g；Do blank experiment simultaneously；
D solution after step (c) constant volume is carried out GC-MS analysis by ()；
Wherein the chromatographic column of GC-MS is DB-5MS；When GC-MS analyzes, the temperature programmed control of GC part sets
It is set to: initial temperature 100-120 DEG C keeps 0.5-2min, rises to 230-270 DEG C with 20-40 DEG C/min, protects
Hold more than 4min；Injector temperature is 280-320 DEG C；
When in step (d), GC-MS analyzes, the condition setting of MS part is: ionization mode is electron bombardment electricity
From, ion source temperature 210-250 DEG C, solvent delay 2-4min, makings interface temperature 255-290 DEG C, measure
Pattern is for selecting ion scan pattern qualitative and quantitative analysis, sweep limits 40 to 500amu.
As preferably, assay method of the present invention, comprise the steps:
A sample treatment is become the every arbitrary dimension granule less than 6mm by ()；
Sample b step (a) is processed by () after puts into sealing in organic solvent, extraction；Sample and organic solvent
Ratio is 1:30g/mL；
C () has extracted after, with organic solvent constant volume used by step (b) after solution is concentrated；After described constant volume
Volume and sample quality are than for 10:1mL/g；Do blank experiment simultaneously；
D solution after step (c) constant volume is carried out GC-MS analysis by ()；
Wherein the chromatographic column of GC-MS is DB-5MS；When GC-MS analyzes, the temperature programmed control of GC part sets
It is set to: initial temperature 110 DEG C keeps 1min, rises to 250 DEG C with 30 DEG C/min, keeps 5min；Injection port
Temperature is 300 DEG C；
When in step (d), GC-MS analyzes, the condition setting of MS part is: ionization mode is electron bombardment electricity
From, ion source temperature 230 DEG C, solvent delay 3min, makings interface temperature 270 DEG C, mode determination is choosing
Select ion scan pattern qualitative and quantitative analysis, sweep limits 40 to 500amu.
In textile, the content of 4,4 '-dibromo diphenyl ester is calculated as follows:
In formula:
XiIn sample 4, the i content of 4 '-dibromo diphenyl ester, unit is mg/kg；
cI, sIn standard working solution 4, the concentration of 4 '-dibromo diphenyl ester i, unit mg/L；
The peak intensity of the i of 4,4 '-dibromo diphenyl ester in A test solution；
AI, bThe peak intensity of the i of 4,4 '-dibromo diphenyl ester in blank；
V test solution constant volume, unit is mL；
AI, sThe peak intensity of 4,4 '-dibromo diphenyl ester i in standard working solution；
M sample mass, unit g.
The detection method of the present invention is easy, and accuracy is high, repeated and repeatability is good.
Accompanying drawing explanation
Fig. 1 is 4,4 '-dibromo diphenyl ester total ion chromatogram；
Fig. 2 is the 4,4 '-dibromo diphenyl ester mass spectrum under SIM pattern；
Fig. 3 is peak intensity and the regression curve of concentration of 4,4 '-dibromo diphenyl ester.
Detailed description of the invention
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art it will be clearly understood that
Described embodiment is used only for help and understands the present invention, is not construed as the concrete restriction to the present invention.
Instrument and equipment in embodiment:
Gas chromatography mass spectrometry instrument GC/MS Japan Shimadzu SHIMADZU GCMS-QP2010 Plus, color
Spectrum post: Agilent company of U.S. DB-5MS, length 30m, internal diameter 0.25mm, thickness 0.25 μm,
Resistance to extreme temperature: 350 DEG C.
Agents useful for same in embodiment: dichloromethane
Specification Curve of Increasing
By the 4 of 20mg/L, the named A of 4 '-dibromo diphenyl ester standard substance, to make solvent, uses 1ml capacity
Bottle is prepared.Dilute according to table 1 below again:
Table 1
With A, five concentration point of A1, A2, A3, A4 do 4, the working curve of 4 '-dibromo diphenyl ester, working curve
Linear requirements more than 0.95.If the working curve of preparation is less than 0.95, then remove deflection curve bigger
A bit, again recall working curve, whether observe after adjusting linear coefficient more than 0.95, if linear coefficient
More than 0.95 use, otherwise, the most again prepare series concentration.
Fig. 3 is peak intensity and the regression curve of concentration of 4,4 '-dibromo diphenyl ester.
Embodiment 1
1, detecting step:
1) prepared by sample: what textile was cut into size 5 × 5 × 5mm treats test sample；
2) organic solvent extraction: weigh sample 1.0089g and treat test sample, be placed in ultrasonic extraction bottle, adds
Organic solvent 30mL, seals, and is placed in ultrasonic extraction instrument ultrasonic 1 hour, is extracted liquid；
3) concentrate: extracted by filtration liquid, rotary evaporation, be settled to 10ml and obtain liquid to be measured.Do blank real simultaneously
Test；
4) measure: drawing sample and blank solution respectively, obtain 4, the peak intensity of 4 '-dibromo diphenyl ester substitutes into
Made regression equation, tries to achieve in sample blank solution and test liquid 4, the concentration of 4 '-dibromo diphenyl ester,
And then calculate the content of 4,4 '-dibromo diphenyl ester in textile.
2, instrument condition and parameter:
GC conditions: carrier gas: high-purity helium, injector temperature: 300 DEG C, post flow: 1.7ml/min,
Temperature programming: 110 DEG C retain 1min, are warming up to 250 DEG C with 30 DEG C/min, 250 DEG C retain 5min.
Mass Spectrometry Conditions: ionization mode: electron impact ionization, ion source temperature: 230 DEG C, solvent delay 3min,
Makings interface temperature: 270 DEG C, mode determination: select ion scan pattern qualitative and quantitative analysis.
3, the qualitative and quantitative analysis of 4,4 '-dibromo diphenyl ester:
Under above-mentioned instrument condition and Parameter Conditions during the reservation of 4,4 '-dibromo diphenyl ester total ion chromatogram
Between be Rt=5.06min, select ion (SIM): m/z=140,168,221,328, wherein 328 be quantitative from
Son.
Fig. 1 is 4,4 '-dibromo diphenyl ester total ion chromatogram in the solution after the sample treatment of the present embodiment；
Fig. 2 is the 4,4 '-dibromo diphenyl ester mass spectrum under SIM pattern.
The calibration curve being used as, records in solution 4,4 '-dibromo diphenyl ester be concentration be 4.524mg/L, sample
In product, 4,4 '-dibromo diphenyl ester content is 44.841mg/kg.Take same sample 10 parts respectively through shredding, extracting
Take post analysis, obtain the content in final sample be respectively as follows: 44.341mg/kg, 43.891mg/kg, 43.807
mg/kg、43.998mg/kg、44.867mg/kg、44.793mg/kg、44.805mg/kg、43.902mg/kg、
44.245mg/kg, 44.918mg/kg, the relative standard deviation of ten test results is 1.018%, it is seen that this
The repeatability of method is very well.By 5 laboratorys, repeatability test result is carried out respectively for same sample divide
It is as follows: 42.007mg/g, 43.095mg/g, 43.911mg/g, 43.798mg/g, 44.442mg/g,
The relative standard deviation of the test result of 5 different experiments rooms is 2.161%, it is seen then that the test side of the present invention
Method also achieves extraordinary repeatability between different laboratorys.The test carrying out recovery of standard addition records
The response rate is between 96-102%, it is seen that the detection method of the present invention has higher accuracy.
Embodiment 2
1, detecting step:
1) prepared by sample: what textile was cut into size 10 × 10 × 10mm treats test sample；
2) organic solvent extraction: weigh sample 1.0111g and treat test sample, be placed in ultrasonic extraction bottle, adds
Organic solvent 50mL, seals, and is placed in ultrasonic extraction instrument ultrasonic 0.5 hour, is extracted liquid；
3) concentrate: extracted by filtration liquid, rotary evaporation, be settled to 5ml and obtain liquid to be measured.Do blank experiment simultaneously；
4) measure: drawing sample and blank solution respectively, obtain 4, the peak intensity of 4 '-dibromo diphenyl ester substitutes into
Made regression equation, tries to achieve in sample blank solution and test liquid 4, the concentration of 4 '-dibromo diphenyl ester,
And then calculate the content of 4,4 '-dibromo diphenyl ester in textile.
2, instrument condition and parameter:
GC conditions: carrier gas: high-purity helium, injector temperature: 280 DEG C, post flow: 1.5ml/min,
Temperature programming: 120 DEG C retain 0.5min, are warming up to 270 DEG C with 20 DEG C/min, retain 8min.
Mass Spectrometry Conditions: ionization mode: electron impact ionization, ion source temperature: 210 DEG C, solvent delay 4min,
Makings interface temperature: 290 DEG C, mode determination: select ion scan pattern qualitative and quantitative analysis.
3, the qualitative and quantitative analysis of 4,4 '-dibromo diphenyl ester:
Under above-mentioned instrument condition and Parameter Conditions during the reservation of 4,4 '-dibromo diphenyl ester total ion chromatogram
Between be Rt=5.19min, select ion (SIM): m/z=140,168,221,328, wherein 328 be quantitative from
Son.
The calibration curve being used as, records in solution 4,4 '-dibromo diphenyl ester be concentration be 1.421mg/L, sample
In product, 4,4 '-dibromo diphenyl ester content is 7.027mg/kg.Take same sample 10 parts respectively through shredding, extracting
Post analysis, obtain the content in final sample be respectively as follows: 7.127mg/kg, 7.214mg/kg, 7.153mg/kg,
7.047mg/kg、7.402mg/kg、7.318mg/kg、7.261mg/kg、7.094mg/kg、7.164mg/kg、
7.221mg/kg, the relative standard deviation of ten test results is 1.483%, it is seen that the repeatability of this method is very
Good.For same sample respectively by 5 laboratorys carried out the following 7.101mg/kg of repeatability test result,
7.214mg/kg, 7.156mg/kg, 7.029mg/kg, 7.521mg/kg, the test of 5 different experiments rooms
The relative standard deviation of result is 2.635%, it is seen then that the method for testing of the present invention is between different laboratorys
Also extraordinary repeatability is achieved.Carry out the test of recovery of standard addition and record the response rate between 96-102%,
The detection method of the visible present invention has higher accuracy.
Applicant states, person of ordinary skill in the field is on the basis of above-described embodiment, by above-mentioned reality
Execute the concrete content point value of example component, combined with the technical scheme of Summary, thus produce
New numerical range, is also one of the record scope of the present invention, the application for making description simple and clear, no longer sieve
Arrange these numerical rangies.
Applicant states, the present invention illustrates the processing technology of the present invention by above-described embodiment, but the present invention
It is not limited to above-mentioned making step, does not i.e. mean that the present invention has to rely on above-mentioned making step ability real
Execute.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to selected by the present invention
Replace and the interpolation of auxiliary element, concrete way choice etc. with the equivalence of raw material, all fall within the guarantor of the present invention
Within the scope of protecting scope and disclosure.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned enforcement
Detail in mode, in the technology concept of the present invention, can enter technical scheme
The multiple simple variant of row, these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention,
In the case of reconcilable, can be combined by any suitable means, in order to avoid unnecessary weight
Multiple, various possible compound modes are illustrated by the present invention the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is not
Running counter to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (9)
1. in a textile 4, the assay method of 4 '-dibromo diphenyl ester, comprise the steps:
A sample treatment is become the every arbitrary dimension granule less than 10mm by ()；
Sample b step (a) is processed by () after puts into sealing in organic solvent, extraction；Sample and organic solvent
Ratio is 1:10-50g/mL；
C () has extracted after, with organic solvent constant volume used by step (b) after solution is concentrated；After described constant volume
Volume and sample quality are than for 5-20:1mL/g；
D solution after step (c) constant volume is carried out GC-MS analysis by ()；
Wherein the chromatographic column of GC-MS is low pole chromatographic column；The program control of GC part when GC-MS analyzes
Temperature is set to: initial temperature 100-120 DEG C keeps 0.5-2min, rises to 230-270 DEG C with 20-40 DEG C/min,
Keep more than 4min；Injector temperature is 280-320 DEG C.
Assay method the most according to claim 1, it is characterised in that in step (a), sample treatment becomes every
The sheet arbitrary dimension granule less than 6mm.
Assay method the most according to claim 1 and 2, it is characterised in that organic described in step (b)
Solvent is dichloromethane and/or acetone；
Preferably, described extraction uses ultrasonic extraction；
Preferably, the time of described extraction is more than 0.5h, preferably 1-3h；
Preferably, the ratio of sample and organic solvent is 1:20-40g/mL, preferably 30g/mL.
4. according to the assay method described in any one of claim 1-3, it is characterised in that in step (c) simultaneously
Do blank experiment；
Preferably, the volume after described constant volume and sample quality are than for 10:1mL/g.
5. according to the assay method described in any one of claim 1-4, it is characterised in that described in step (d)
Chromatographic column be DB-5MS, preferably specification be 30m*0.25mm*0.25 μm；
Preferably, when GC-MS analyzes, carrier gas is high-purity helium, and post flow is 1.5-2.0ml/min, is preferably
1.7ml/min。
6. according to the assay method described in any one of claim 1-5, it is characterised in that GC-MS in step (d)
During analysis, the temperature programmed control of GC part is set to: initial temperature 110 DEG C keeps 1min, with 30 DEG C/min liter
To 250 DEG C, keep 5min.
7. according to the assay method described in any one of claim 1-6, it is characterised in that GC-MS in step (d)
During analysis, the condition setting of MS part is: ionization mode is electron impact ionization, ion source temperature
210-250 DEG C, solvent delay 2-4min, makings interface temperature 255-290 DEG C, mode determination is for selecting ion
Scan pattern qualitative and quantitative analysis, sweep limits 40 to 500amu；Being preferably ionization mode is that electronics bangs
Hit ionization, ion source temperature 230 DEG C, solvent delay 3min, makings interface temperature 270 DEG C, mode determination
For selecting ion scan pattern qualitative and quantitative analysis, sweep limits 40 to 500amu.
Assay method the most according to claim 1, it is characterised in that comprise the steps:
A sample treatment is become the every arbitrary dimension granule less than 10mm by ()；
Sample b step (a) is processed by () after puts into sealing in organic solvent, extraction；Sample and organic solvent
Ratio is 1:10-50g/mL；
C () has extracted after, with organic solvent constant volume used by step (b) after solution is concentrated；After described constant volume
Volume and sample quality are than for 5-20:1mL/g；Do blank experiment simultaneously；
D solution after step (c) constant volume is carried out GC-MS analysis by ()；
Wherein the chromatographic column of GC-MS is DB-5MS；When GC-MS analyzes, the temperature programmed control of GC part sets
It is set to: initial temperature 100-120 DEG C keeps 0.5-2min, rises to 230-270 DEG C with 20-40 DEG C/min, protects
Hold more than 4min；Injector temperature is 280-320 DEG C；
When in step (d), GC-MS analyzes, the condition setting of MS part is: ionization mode is electron bombardment electricity
From, ion source temperature 210-250 DEG C, solvent delay 2-4min, makings interface temperature 255-290 DEG C, measure
Pattern is for selecting ion scan pattern qualitative and quantitative analysis, sweep limits 40 to 500amu.
Assay method the most according to claim 1, it is characterised in that comprise the steps:
A sample treatment is become the every arbitrary dimension granule less than 6mm by ()；
Sample b step (a) is processed by () after puts into sealing in organic solvent, extraction；Sample and organic solvent
Ratio is 1:30g/mL；
C () has extracted after, with organic solvent constant volume used by step (b) after solution is concentrated；After described constant volume
Volume and sample quality are than for 10:1mL/g；Do blank experiment simultaneously；
D solution after step (c) constant volume is carried out GC-MS analysis by ()；
Wherein the chromatographic column of GC-MS is DB-5MS；When GC-MS analyzes, the temperature programmed control of GC part sets
It is set to: initial temperature 110 DEG C keeps 1min, rises to 250 DEG C with 30 DEG C/min, keeps 5min；Injection port
Temperature is 300 DEG C；
When in step (d), GC-MS analyzes, the condition setting of MS part is: ionization mode is electron bombardment electricity
From, ion source temperature 230 DEG C, solvent delay 3min, makings interface temperature 270 DEG C, mode determination is choosing
Select ion scan pattern qualitative and quantitative analysis, sweep limits 40 to 500amu.
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| CN102243221A (en) * | 2011-04-21 | 2011-11-16 | 郭会清 | Detection method for special fire retardant content in textile |
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