CN106404979A - Method using ultrasonic extraction-gas chromatography-mass spectrum to measure chlorobenzene compounds in textiles - Google Patents
Method using ultrasonic extraction-gas chromatography-mass spectrum to measure chlorobenzene compounds in textiles Download PDFInfo
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- CN106404979A CN106404979A CN201611015729.1A CN201611015729A CN106404979A CN 106404979 A CN106404979 A CN 106404979A CN 201611015729 A CN201611015729 A CN 201611015729A CN 106404979 A CN106404979 A CN 106404979A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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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Abstract
The invention discloses a method using ultrasonic extraction-gas chromatography-mass spectrum to measure chlorobenzene compounds in textiles. The method includes: preparing a to-be-measured sample, extracting the sample, preparing a standard work solution and detecting a to-be-measured sample solution. The method using ultrasonic extraction-gas chromatography-mass spectrum to measure the chlorobenzene compounds in the textiles has the advantages that the chlorobenzene organic pollutants in the textiles can be measured at the same time, the method is accurate, fast and high in sensitivity, and a reliable detecting method support is provided for the fast detection of the textiles.
Description
Technical field
The invention belongs to textile inspection field, it is related to gas chromatography-mass spectrography (GC-MS), specifically refer to a kind of ultrasonic
In extraction-gas chromatography-mass spectrometry textile, the method for chlorobenzene compound, is particularly suited for textile.
Background technology
Raising with people's living standard and the enhancing of environmental consciousness, green consumption has become as a kind of trend.Carrier
Dyeing is conventional dyeing in textile industry.Carrier dyeing is conducive to disperse dyes right under the conditions of boiling dyeing at normal pressure
Textile is dyeed.Some cheap chloride aromatic compounds, such as dichloro-benzenes, trichloro-benzenes, tetrachlorobenzene are efficient dyeing
Carrier.During these chlorobenzene carriers are used in textile dyeing, contribute to the expanded infiltration with dyestuff of fibre structure.
But research both domestic and external indicates, chlorobenzene compound chemical property is sufficiently stable, it is not easy under field conditions (factors) point
Solution, Long Term Contact can cause skin allergy, the central nervous system of impact people, then has potential teratogenesis and cause to the body of people
Carcinous.The Oeko-Tex Standard 100 being issued according to the research of international ecological textile and inspection association and country of China matter
The GB/T 18885-2009 that amount supervision and inspection quarantine general bureau issues《Ecological textile technical specification》Standard specifies, chlorobenzene is contained
The limit value of amount also all dictates it is stipulated that Limited Doses must not exceed 1.0 mg/kg.
Therefore, set up accurately and reliably measure textile in 1,3- dichloro-benzenes, Isosorbide-5-Nitrae-dichloro-benzenes, 1,2- dichloro-benzenes, 1,3,
5- trichloro-benzenes, 1,2,4- trichloro-benzenes, 1,2,3- trichloro-benzenes, 1,2,3,5- tetrachlorobenzene, 1,2,4,5- tetrachlorobenzene, 1,2,3,4- tetrachloro
The content of 11 kinds of chlorobenzene class organic pollutions such as benzene, pentachlorobenzene, Perchlorobenzene is extremely important.
At present, conventional analysis method can be divided into qualitative analyses, quantitative analyses and qualitative and quantitative analysis technology.Quantitative analyses
Typically adopt chromatographic technique and hydrolysis and condensation, chromatographic technique has the methods such as gas chromatogram and liquid chromatograph, chromatograph matter
Spectrum multiple techniques has the methods such as liquid chromatograph mass spectrography and gas chromatography-mass spectrography；Qualitative and quantitative analysis then will have two concurrently
The technology of kind is integrated, and testing result will provide structural information and the quantity information of object simultaneously.
Therefore, it is necessary to 1,3- dichloro-benzenes in textile, Isosorbide-5-Nitrae-dichloro-benzenes, 1,2- dichloro-benzenes, 1,3,5- trichloro-benzenes, 1,
2,4- trichloro-benzenes, 1,2,3- trichloro-benzenes, 1,2,3,5- tetrachlorobenzene, 1,2,4,5- tetrachlorobenzene, 1,2,3,4- tetrachlorobenzene, pentachlorobenzene,
The detection method of 11 kinds of chlorobenzene class organic pollutions such as Perchlorobenzene is studied, thus carrying out to chlorobenzene compound in textile
Monitoring, when simultaneously for the area such as light industrial goods export enterprise such as domestic textile to European Union, can provide and meet Chinese and EU etc.
The detection data of the regulation of national standard.
Content of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of ultrasonic extraction-gas chromatography-mass spectrometry weaving
The method of chlorobenzene compound in product, the method combines ultrasonic extraction-gas chromatography-mass spectrography, can be to chlorobenzene in textile
Class organic pollution is measured simultaneously, and that the method has the advantages that is accurate, quick, sensitivity is high, is the quick inspection of textile
Survey provides reliable detection method and supports.
The method that the present invention provides chlorobenzene compound in a kind of ultrasonic extraction-gas chromatography-mass spectrometry textile, bag
Include following steps：
Step one, the preparation of testing sample, take appropriate textile samples, sample are shredded, sample size scope be less than 20mm ×
20mm, and will be uniform for the sample mix after shredding；
Step 2, sample extraction, weigh 0.70-1.30g sample, are placed in reaction bulb, add 30mL dichloromethane liquid, in room
Carry out ultrasonic extraction 25 ~ 35min under the conditions of temperature and obtain ultrasonic extract, filter ultrasonic extract and concentrate acquisition 1 ~
2mL concentrated solution, concentrated solution is transferred in evaporation tube, and nitrogen is blown to 1mL, adds 2, the 4,5,6- tetra- of 0.01mL 100 g/mL
Dimethyl benzene phenol solution between chlorine, described 2, between 4,5,6- tetrachloros, dimethyl benzene phenol solution is inner mark solution, obtains after uniformly mixing
Testing sample solution；
Step 3, the configuration of standard working solution, prepare ladder concentration and are respectively 0.1 g/mL, 0.5 g/mL, 2.0 g/mL's
Chlorobenzene titer, and add xylenol between 2,4,5,6- tetrachloros to be mixed to form standard as internal standard substance in chlorobenzene titer
Working solution, between described internal standard substance 2,4,5,6- tetrachloro, solubility in standard working solution for the xylenol is 1.0 g/mL；
Step 4, the detection of testing sample solution, by the testing sample solution in step 2 and standard working solution in gas phase color
Difference sample introduction on spectrum-mass spectrograph, obtains with chlorobenzene class organic pollution in standard working solution and internal standard substance 2,4,5,6- tetrachloro
Between the concentration ratio of xylenol be abscissa, then with chlorobenzene class organic pollution in standard working solution and internal standard substance 2,4,5,
Between 6- tetrachloro, the peak area ratio of xylenol is the working curve of vertical coordinate, and it is organic to obtain chlorobenzene class in each standard working solution
The peak area ratio of xylenol and the organic dirt of chlorobenzene class in standard working solution between pollutant and internal standard substance 2,4,5,6- tetrachloro
The linear relation of the concentration ratio of xylenol between dye thing and internal standard substance 2,4,5,6- tetrachloro, by the chromatograph of testing sample solution
Figure measures the peak area ratio of testing sample solution, and peak area ratio substitution linear relation is drawn chlorobenzene in testing sample solution
Concentration, and with 2,4,5,6- tetrachloros between xylenol calculated using internal standard method for internal standard substance, obtain testing sample solution
Middle chlorobenzene class organic pollution concentration, wherein quantitative Analysis formula is：X=cv/m
In formula, X represents the content of chlorobenzene in testing sample solution, and unit is milligrams per kilogram (mg/kg)；
C represents the concentration of chlorobenzene in testing sample solution, and unit is micrograms per millilitre (g/mL)；
V represents testing sample solution cumulative volume, and unit is milliliter (mL)；
M represents sample mass, and unit is gram (g).
So setting beneficial effect be：Using such scheme, using such scheme, the present invention passes through to add dichloromethane
Ultrasonic extraction is carried out to textile samples, pretreatment process is simple, convenient, fast.
Secondly, the present invention is by gas for the qualitative and quantitative detection analysis of chlorobenzene class Components of Organic Pollutants in textile
Phase chromatography-mass spectroscopy instrument (GC-MS) is analyzed.First configure one group of step-like standard working solution, then by standard working solution and treating
Inspection liquid difference sample introduction on gas chromatograph-mass spectrometer.The chromatographic peak retention time occurring in liquid to be checked and standard working solution one
Cause it is allowed to deviation is less than ± 2.5 %, the relative abundance of the mass spectrometry ion corresponding to this chromatographic peak standard suitable with concentration
The relative abundance of working solution is consistent, and relative abundance deviation is less than regulation, then can determine that in this liquid to be checked and contain chlorobenzene
Class compound.
Finally, this method carries out quantitative Analysis using internal standard method, and in formula, v is that volume after testing sample solution nitrogen blows is
1ml；M is the quality that style weighs；C is calculated by the linear relationship drawing in working curve, internal standard substance in linear relationship
Between 2,4,5,6- tetrachloros, the concentration of xylenol is 1.0 g/mL, the no impact of its log-of-ratio value, only impact unit, specifically
Calculation, first by the peak area reading in chromatogram in testing sample solution, then brings the numerical value that linear relation draws c into；
Calculated by above-mentioned formula again, drawn testing result so that testing result is more accurate, more be there is cogency.
The extracting mode that the present invention is further arranged in described step 2 is ultrasonic extraction, and Extraction solvent is dichloromethane
Alkane.
So setting beneficial effect be：Using such scheme, dichloromethane has splendid molten to Chlorobenzene compounds
Xie Xing, is easy to Chlorobenzene compounds in style are concentrated, is easy to follow-up detection.
The present invention is further arranged to adopt Rotary Evaporators to the concentration of ultrasonic extract in described step 2, setting
Thickening temperature is 40 ± 5 DEG C.
So setting beneficial effect be：Using such scheme, temperature rationally will not when Chlorobenzene compounds decompose,
Guarantee the accuracy tested, adopt this Rotary Evaporators to concentrate speed soon simultaneously, improve experimental work efficiency.
The present invention is further arranged in described step 2 also include using dichloromethane liquid, bearing ultrasonic is extracted
Washing and obtaining cleaning mixture of the reagent bottle of liquid, cleaning mixture is mixed and carries out simultaneously nitrogen and blow with concentrated solution.
So setting beneficial effect be：Using such scheme, using dichloromethane to reprinting ultrasonic extract
Sample bottle carries out once washing, and merges with ultrasonic extract, effectively to the ultrasonic extraction remaining in sample bottle
Liquid is collected, and together carries out operation and the detection of next step, effectively increases the precision of inspection it is ensured that test is tied
The accuracy of fruit.
The present invention is further arranged to described chlorobenzene titer and includes 1,3- dichloro-benzenes titer, 1,4- dichloro-benzenes standard
Liquid, 1,2- dichloro-benzenes titer, 1,3,5- trichloro-benzenes titer, 1,2,4- trichloro-benzenes titer, 1,2,3- trichloro-benzenes titer,
1,2,3,5- tetrachlorobenzene titer, 1,2,4,5- tetrachlorobenzene titer, 1,2,3,4- tetrachlorobenzene titer, pentachlorobenzene titer,
Perchlorobenzene titer.
In step 4 of the present invention, the detection parameter of gas chromatograph-mass spectrometer is：
Chromatographic condition：HP-35 MS (30 m × 0.25 mm × 0.25 m) capillary column；Using temperature programming, initial temperature
For 100 °C, keep 1min, be then warming up to 240 °C with 15 °C/min, keep 3 min；260 °C of injector temperature, carrier gas is
High-pure helium, flow 1.0 mL/min, pulse Splitless injecting samples, sample size is 2.0 L.
Mass Spectrometry Conditions：Electron impact ion source (EI), ion source temperature is 230 °C, and level Four bar temperature is 150 °C, interface
Temperature is 300 °C, and the solvent delay time is 7 min, data acquisition scheme SIM.
With reference to embodiment, the invention will be further described.
Brief description
Fig. 1 is the 1,3- dichloro-benzenes chemical structural formula in the specific embodiment of the invention；
Fig. 2 is the 1,4- dichloro-benzenes chemical structural formula in the specific embodiment of the invention；
Fig. 3 is the 1,2- dichloro-benzenes chemical structural formula in the specific embodiment of the invention；
Fig. 4 is the 1,3,5- trichloro-benzenes chemical structural formula in the specific embodiment of the invention；
Fig. 5 is the 1,2,4- trichloro-benzenes chemical structural formula in the specific embodiment of the invention；
Fig. 6 is the 1,2,3- trichloro-benzenes chemical structural formula in the specific embodiment of the invention；
Fig. 7 is the 1,2,3,5- tetrachlorobenzene chemical structural formula in the specific embodiment of the invention；
Fig. 8 is the 1,2,4,5- tetrachlorobenzene chemical structural formula in the specific embodiment of the invention；
Fig. 9 is the 1,2,3,4- tetrachlorobenzene chemical structural formula in the specific embodiment of the invention；
Figure 10 is the pentachlorobenzene chemical structural formula in the specific embodiment of the invention；
Figure 11 is the Perchlorobenzene chemical structural formula in the specific embodiment of the invention；
Figure 12 is 11 kinds of chlorobenzene compound standard solution (2.0 g/mL) MRM chromatograms in the specific embodiment of the invention；
Figure 13 is specific embodiment of the invention empty textile samples figure A
Figure 14 is specific embodiment of the invention empty textile samples marked graph B；
Figure 15 is the 1,3- dichloro-benzenes in the specific embodiment of the invention, 1,4- dichloro-benzenes standard working curve；
Figure 16 is the 1,2- dichloro-benzenes standard working curve in the specific embodiment of the invention；
Figure 17 is the 1,3,5- trichloro-benzenes standard working curve in the specific embodiment of the invention；
Figure 18 is the 1,2,4- trichloro-benzenes standard working curve in the specific embodiment of the invention；
Figure 19 is the 1,2,3- trichloro-benzenes standard working curve in the specific embodiment of the invention；
Figure 20 is the 1,2,3,5- tetrachlorobenzene in the specific embodiment of the invention, 1,2,4,5- tetrachlorobenzene standard working curve；
Figure 21 is the 1,2,3,4- tetrachlorobenzene standard working curve in the specific embodiment of the invention；
Figure 22 is the pentachlorobenzene standard working curve in the specific embodiment of the invention；
Figure 23 is the Perchlorobenzene standard working curve in the specific embodiment of the invention.
Specific embodiment
Being embodied as of the present invention is for example a kind of ultrasonic extraction-gas chromatography-mass spectrometry textile shown in Fig. 1-2 3
The method of middle chlorobenzene compound, it comprises the following steps：
Step one, the preparation of testing sample, take appropriate textile samples, sample are shredded, sample size scope be less than 20mm ×
20mm, and the sample after shredding uniformly is mixed；
Step 2, sample extraction, weigh 1.00g sample, are placed in 40 mL reaction bulbs, add 30 mL dichloromethane, in room temperature
Under the conditions of ultrasonic extraction 30 min obtain ultrasonic extract.Ultrasonic extract is filtered to the boiling flask of 100 mL
In, concentrated under the conditions of 40 DEG C of temperature with Rotary Evaporators and obtain 1-2mL concentrated solution, concentrated solution is transferred in evaporation tube, and
Clean boiling flask with a small amount of dichloromethane, merge and proceed to evaporation tube, nitrogen is blown to 1 mL.Plus 0.01 mL, 100 g/mL's is interior
Mark solution, obtains testing sample solution after mixing；
Step 3, the configuration of standard working solution, prepare ladder concentration and are respectively 0.1 g/mL, 0.5 g/mL, 2.0 g/mL's
Chlorobenzene titer, chlorobenzene titer include 1,3- dichloro-benzenes titer, Isosorbide-5-Nitrae-dichloro-benzenes titer, 1,2- dichloro-benzenes titer,
1,3,5- trichloro-benzenes titer, 1,2,4- trichloro-benzenes titer, 1,2,3- trichloro-benzenes titer, 1,2,3,5- tetrachlorobenzene standard
Liquid, 1,2,4,5- tetrachlorobenzene titers, 1,2,3,4- tetrachlorobenzene titers, pentachlorobenzene titer, Perchlorobenzene titer, and in chlorine
Xylenol between 2,4,5,6- tetrachloros is added to be mixed to form standard working solution as internal standard substance in benzene titer, described internal standard
Thing 2,4, between 5,6- tetrachloros, solubility in standard working solution for the xylenol is 1.0 g/mL；
Step 4, the detection of testing sample solution, by the testing sample solution in step 2 and standard working solution in gas phase color
Difference sample introduction on spectrum-mass spectrograph, chromatographic condition and Mass Spectrometry Conditions are respectively,
Chromatographic condition：HP-35 MS (30 m × 0.25 mm × 0.25 m) capillary column；Using temperature programming, initial temperature
For 100 °C, keep 1min, be then warming up to 240 °C with 15 °C/min, retention time is as shown in table 1；260 ° of injector temperature
C, carrier gas is high-pure helium, flow 1.0 mL/min, pulse Splitless injecting samples, and sample size is 2.0 L；
1-11 kind of chlorobenzene GC-MS testing conditions of table
Mass Spectrometry Conditions：Electron impact ion source (EI), ion source temperature is 230 °C, and level Four bar temperature is 150 °C, interface temperature
For 300 °C, the solvent delay time is 7 min, data acquisition scheme SIM.
Obtain with xylenol between chlorobenzene class organic pollution in standard working solution and internal standard substance 2,4,5,6- tetrachloro
Concentration ratio be abscissa, then with diformazan between chlorobenzene class organic pollution in standard working solution and internal standard substance 2,4,5,6- tetrachloro
The peak area ratio of base phenol is the working curve of vertical coordinate, and obtains chlorobenzene class in the standard working solution of as shown in table 2 11 kind and have
Between organic pollutants and internal standard substance 2,4,5,6- tetrachloro, the peak area ratio of xylenol is organic with chlorobenzene class in standard working solution
The linear relation of the concentration ratio of xylenol between pollutant and internal standard substance 2,4,5,6- tetrachloro,
The linear equation of 2-11 kinds of chlorobenzenes of table, correlation coefficient, quantitative limit
Measured the peak area ratio of testing sample solution by the chromatogram of testing sample solution, peak area ratio is substituted into linear relation
Draw the concentration of chlorobenzene in testing sample solution, and with 2,4,5,6- tetrachloros between xylenol entered using internal standard method for internal standard substance
Row calculates, and obtains chlorobenzene class organic pollution concentration in testing sample solution, and wherein quantitative Analysis formula is：X=cv/m
In formula, X represents the content of chlorobenzene in testing sample solution, and unit is milligrams per kilogram (mg/kg)；
C represents the concentration of chlorobenzene in testing sample solution, and unit is micrograms per millilitre (g/mL)；
V represents testing sample solution cumulative volume, and unit is milliliter (mL)；
M represents sample mass, and unit is gram (g).
3-11 kinds of chlorobenzene TIANZHU XINGNAO Capsul of table, precision (n=6)
The present invention is not limited to above-mentioned specific embodiment, and persons skilled in the art, can according to present disclosure
To implement the present invention using other multiple specific embodiments, or the design structure of every employing present invention and thinking, do
Simple change or change, both fall within protection scope of the present invention.
Claims (6)
1. in a kind of ultrasonic extraction-gas chromatography-mass spectrometry textile chlorobenzene compound method it is characterised in that bag
Include following steps：
Step one, the preparation of testing sample, take appropriate textile samples, sample are shredded, sample size scope be less than 20mm ×
20mm, and will be uniform for the sample mix after shredding；
Step 2, sample extraction, weigh 0.70-1.30g sample, are placed in reaction bulb, add 30mL dichloromethane liquid, in room
Carry out ultrasonic extraction 25 ~ 35min under the conditions of temperature and obtain ultrasonic extract, filter ultrasonic extract and concentrate acquisition 1 ~
2mL concentrated solution, concentrated solution is transferred in evaporation tube, and nitrogen is blown to 1mL, adds 2, the 4,5,6- tetra- of 0.01mL 100 g/mL
Dimethyl benzene phenol solution between chlorine, described 2, between 4,5,6- tetrachloros, dimethyl benzene phenol solution is inner mark solution, obtains after uniformly mixing
Testing sample solution；
Step 3, the configuration of standard working solution, prepare ladder concentration and are respectively 0.1 g/mL, 0.5 g/mL, 2.0 g/mL's
Chlorobenzene titer, and add xylenol between 2,4,5,6- tetrachloros to be mixed to form standard as internal standard substance in chlorobenzene titer
Working solution, between described internal standard substance 2,4,5,6- tetrachloro, solubility in standard working solution for the xylenol is 1.0 g/mL；
Step 4, the detection of testing sample solution, by the testing sample solution in step 2 and standard working solution in gas phase color
Difference sample introduction on spectrum-mass spectrograph, obtains with chlorobenzene class organic pollution in standard working solution and internal standard substance 2,4,5,6- tetrachloro
Between the concentration ratio of xylenol be abscissa, then with chlorobenzene class organic pollution in standard working solution and internal standard substance 2,4,5,
Between 6- tetrachloro, the peak area ratio of xylenol is the working curve of vertical coordinate, and it is organic to obtain chlorobenzene class in each standard working solution
The peak area ratio of xylenol and the organic dirt of chlorobenzene class in standard working solution between pollutant and internal standard substance 2,4,5,6- tetrachloro
The linear relation of the concentration ratio of xylenol between dye thing and internal standard substance 2,4,5,6- tetrachloro, by the chromatograph of testing sample solution
Figure measures the peak area ratio of testing sample solution, and peak area ratio substitution linear relation is drawn chlorobenzene in testing sample solution
Concentration, and with 2,4,5,6- tetrachloros between xylenol calculated using internal standard method for internal standard substance, obtain testing sample solution
Middle chlorobenzene class organic pollution concentration, wherein quantitative Analysis formula is：X=cv/m
In formula, X represents the content of chlorobenzene in testing sample solution, and unit is milligrams per kilogram (mg/kg)；
C represents the concentration of chlorobenzene in testing sample solution, and unit is micrograms per millilitre (g/mL)；
V represents testing sample solution cumulative volume, and unit is milliliter (mL)；
M represents sample mass, and unit is gram (g).
2. in ultrasonic extraction according to claim 1-gas chromatography-mass spectrometry textile chlorobenzene compound side
Method it is characterised in that：Extracting mode in described step 2 is ultrasonic extraction, and Extraction solvent is dichloromethane.
3. in ultrasonic extraction according to claim 1-gas chromatography-mass spectrometry textile chlorobenzene compound side
Method it is characterised in that：In described step 2, the concentration of ultrasonic extract is adopted with Rotary Evaporators, setting thickening temperature is 40
±5℃.
4. in ultrasonic extraction according to claim 1-gas chromatography-mass spectrometry textile chlorobenzene compound side
Method it is characterised in that：Also include in described step 2 using dichloromethane liquid to the reagent bottle of bearing ultrasonic extracting solution
Wash and obtain cleaning mixture, cleaning mixture is mixed and carries out simultaneously nitrogen with concentrated solution and blow.
5. in ultrasonic extraction according to claim 1-gas chromatography-mass spectrometry textile chlorobenzene compound side
Method it is characterised in that：Described chlorobenzene titer includes 1,3- dichloro-benzenes titer, 1,4- dichloro-benzenes titer, 1,2- dichloro-benzenes
Titer, 1,3,5- trichloro-benzenes titer, 1,2,4- trichloro-benzenes titer, 1,2,3- trichloro-benzenes titer, 1,2,3,5- tetrachloro
Benzene titer, 1,2,4,5- tetrachlorobenzene titer, 1,2,3,4- tetrachlorobenzene titer, pentachlorobenzene titer, Perchlorobenzene titer.
6. in a kind of textile according to claim 1 chloro- benzenes contamination thing detection method it is characterised in that：Described
In step 4, the detection parameter of gas chromatograph-mass spectrometer is：
Chromatographic condition：HP-35 MS (30 m × 0.25 mm × 0.25 m) capillary column；Using temperature programming, initial temperature
For 100 °C, keep 1min, be then warming up to 240 °C with 15 °C/min, keep 3 min；260 °C of injector temperature, carrier gas is
High-pure helium, flow 1.0 mL/min, pulse Splitless injecting samples, sample size is 2.0 L；
Mass Spectrometry Conditions：Electron impact ion source (EI), ion source temperature is 230 °C, and level Four bar temperature is 150 °C, interface temperature
For 300 °C, the solvent delay time is 7 min, data acquisition scheme SIM.
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Cited By (6)
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| CN108152397A (en) * | 2017-12-14 | 2018-06-12 | 浙江工业大学 | Method for simultaneously detecting hexachlorobutadiene, pentachlorobenzene and hexachlorobenzene in waste incineration fly ash |
| CN108445132A (en) * | 2018-03-26 | 2018-08-24 | 安徽回车服装有限公司 | A kind of textile chemistry method for detecting residue |
| CN109975468A (en) * | 2019-02-15 | 2019-07-05 | 上海市质量监督检验技术研究院 | The detection method of mosquito repellent effective component in a kind of textile |
| CN111024830A (en) * | 2018-10-09 | 2020-04-17 | 江苏德旺化工工业有限公司 | Method for detecting organochlorine carrier in dye |
| CN113884454A (en) * | 2021-09-30 | 2022-01-04 | 浙江扬清芯片技术有限公司 | System and method for integrated textile ultrasonic extraction and detection |
| CN114002351A (en) * | 2021-10-27 | 2022-02-01 | 江苏新河农用化工有限公司 | Gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil |
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| CN109975468A (en) * | 2019-02-15 | 2019-07-05 | 上海市质量监督检验技术研究院 | The detection method of mosquito repellent effective component in a kind of textile |
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| CN114002351A (en) * | 2021-10-27 | 2022-02-01 | 江苏新河农用化工有限公司 | Gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil |
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