CN106770703A - The method that GC-MS determines chlorobenzene class organic pollution in leather - Google Patents
The method that GC-MS determines chlorobenzene class organic pollution in leather Download PDFInfo
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- CN106770703A CN106770703A CN201611018069.2A CN201611018069A CN106770703A CN 106770703 A CN106770703 A CN 106770703A CN 201611018069 A CN201611018069 A CN 201611018069A CN 106770703 A CN106770703 A CN 106770703A
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- G—PHYSICS
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- 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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Abstract
The invention discloses a kind of method that GC-MS determines chlorobenzene class organic pollution in leather, comprise the following steps：The preparation of testing sample, sample extraction, the configuration of standard working solution and the detection of testing sample solution, the method combination ultrasonic extraction GC-MS, chlorobenzene class organic pollution in leather can be simultaneously measured, the method have the advantages that accurately, quick, sensitivity it is high, for the quick detection of leather provides reliable detection method support.
Description
Technical field
The invention belongs to leather detection field, it is related to gas chromatography-mass spectrography (GC-MS), specifically refers to a kind of gas phase color
The method of chlorobenzene class organic pollution, is particularly suited for leather in spectrum-mass spectrometric determination leather.
Background technology
With the improvement of people ' s living standards with the enhancing of environmental consciousness, green consumption has become a kind of trend.Carrier
Dyeing is the dyeing commonly used in leather conduct industry.Carrier dyeing is conducive to disperse dyes right under the conditions of boiling dyeing at normal pressure
Leather product are dyeed.Some cheap chloride aromatic compounds, such as dichloro-benzenes, trichloro-benzenes, tetrachlorobenzene are efficient dyeing
Carrier.These chlorobenzene carriers are used in leather product dyeing course, the infiltration for contributing to fibre structure expanded with dyestuff.But it is domestic
Outer research indicates that chlorobenzene compound chemical property is sufficiently stable, is not easy to decompose under field conditions (factors), and Long Term Contact can cause
It is allergic, the central nervous system of people is influenceed, then the body to people has potential teratogenesis and carcinogenicity.
But research both domestic and external indicates that chlorobenzene compound chemical property is sufficiently stable, is not easy under field conditions (factors) point
Solution, Long Term Contact can cause allergic, influence the central nervous system of people, and then the body to people has potential teratogenesis and cause
It is carcinous.Shoes manufacturing enterprise of the country of China generally refers to light industry standard on footwear standard, mainly into footwear outward appearance and physics
Mechanical performance has more detailed requirement, and is not strict with then in terms of poisonous and harmful substance limitation, with EU criteria phase
Difference is very remote, such as China's state compulsion standard GB20400-2006《Leather and fur limits of harmful substances》Also specify only free
The poisonous and harmful substance limitation of formaldehyde and forbidding azo dyes this two major classes, this directly results in China's footwear because of foreign technology
The loss of barrier is every year more than up to 20,000,000,000 RMB.
Therefore, set up and accurately and reliably determine 1,3- dichloro-benzenes, Isosorbide-5-Nitrae-dichloro-benzenes, 1,2- dichloro-benzenes, 1,3 in leather product,
5- trichloro-benzenes, 1,2,4- trichloro-benzenes, 1,2,3- trichloro-benzenes, 1,2,3,5- tetrachlorobenzenes, 1,2,4,5- tetrachlorobenzenes, 1,2,3,4- tetrachloros
The content of 11 kinds of chlorobenzene class organic pollutions such as benzene, pentachlorobenzene, hexachloro-benzene is extremely important.
At present, conventional analysis method can be divided into qualitative analysis, quantitative analysis and qualitative and quantitative analysis technology.Quantitative analysis
Typically using chromatographic technique and hydrolysis and condensation, chromatographic technique has the methods such as gas-chromatography and liquid chromatogram, chromatogram matter
Spectrum GC-MS has the methods such as liquid chromatograph mass spectrography and gas chromatography-mass spectrography；Qualitative and quantitative analysis will then have two concurrently
The technology of kind is integrated, and testing result will simultaneously provide the structural information and quantity information of object.
Therefore, it is necessary to 1,3- dichloro-benzenes, Isosorbide-5-Nitrae-dichloro-benzenes, 1,2- dichloro-benzenes, 1,3,5- trichloro-benzenes, 1 in leather product,
2,4- trichloro-benzenes, 1,2,3- trichloro-benzenes, 1,2,3,5- tetrachlorobenzenes, 1,2,4,5- tetrachlorobenzenes, 1,2,3,4- tetrachlorobenzenes, pentachlorobenzene,
The detection method of 11 kinds of chlorobenzene class organic pollutions such as hexachloro-benzene is studied, so as to be carried out to chlorobenzene compound in leather product
Monitoring, at the same for the light industrial goods export enterprises such as domestic leather product to European Union etc. it is regional when, can provide and meet Chinese and EU etc.
The detection data of the regulation of national standard.
The content of the invention
In order to overcome the deficiencies in the prior art, the invention provides chlorobenzene in a kind of Gas Chromatography-Mass Spectrometry leather
The method of class organic pollution, the method combination ultrasonic extraction-gas chromatography-mass spectrography can be organic to chlorobenzene class in leather
Pollutant is measured simultaneously, the method have the advantages that accurately, quick, sensitivity it is high, for the quick detection of leather is provided
Reliable detection method is supported.
The method that the present invention provides chlorobenzene class organic pollution in a kind of Gas Chromatography-Mass Spectrometry leather, including with
Lower step：
The preparation of step one, testing sample, takes appropriate leather sample, and sample is shredded, sample size scope less than 20mm ×
20mm, and sample after shredding is well mixed；
Step 2, sample extraction, weigh 0.70-1.30g samples, are placed in reaction bulb, 30mL dichloromethane liquid are added, in room
Carried out under the conditions of temperature 25 ~ 35min of ultrasonic wave extraction obtain ultrasonic extract, filter ultrasonic extract and concentrate acquisition 1 ~
2mL concentrates, concentrate is transferred in evaporation tube, and nitrogen is blown to 1mL, adds 2, the 4,5,6- tetra- of the μ g/mL of 0.01mL 100
Dimethyl benzene phenol solution between chlorine, described 2, dimethyl benzene phenol solution is inner mark solution between 4,5,6- tetrachloros, it is uniform mix after obtain
Testing sample solution；
The configuration of step 3, standard working solution, prepares ladder concentration and is respectively 0.1 μ g/mL, 0.5 μ g/mL, 2.0 μ g/mL's
Chlorobenzene titer, and xylenol is mixed to form standard as internal standard compound between 2,4,5,6- tetrachloros are added in chlorobenzene titer
Solubility of the xylenol in standard working solution is 1.0 μ g/mL between working solution, the tetrachloro of the internal standard compound 2,4,5,6-；
The detection of step 4, testing sample solution, by the testing sample solution and standard working solution in step 2 in gas phase color
Sample introduction is distinguished on spectrum-mass spectrograph, is obtained with chlorobenzene class organic pollution in standard working solution and the tetrachloro of internal standard compound 2,4,5,6-
Between the concentration ratio of xylenol be abscissa, then with chlorobenzene class organic pollution in standard working solution and internal standard compound 2,4,5,
The peak area ratio of xylenol is the working curve of ordinate between 6- tetrachloros, and chlorobenzene class is organic in obtaining each standard working solution
The peak area ratio of xylenol and the organic dirt of chlorobenzene class in standard working solution between pollutant and the tetrachloro of internal standard compound 2,4,5,6-
The linear relation of the concentration ratio of xylenol between dye thing and the tetrachloro of internal standard compound 2,4,5,6-, by the chromatogram of testing sample solution
Figure measures the peak area ratio of testing sample solution, and peak area ratio substitution linear relation is drawn into chlorobenzene in testing sample solution
Concentration, and with 2, xylenol is calculated for internal standard compound using internal standard method between 4,5,6- tetrachloros, obtains testing sample solution
Middle chlorobenzene class organic pollution concentration, wherein quantitatively computing formula is：X=cv/m
X represents the content of chlorobenzene in testing sample solution in formula, and unit is milligrams per kilogram (mg/kg)；
C represents the concentration of chlorobenzene in testing sample solution, and unit is micrograms per millilitre (μ g/mL)；
V represents testing sample solution cumulative volume, and unit is milliliter (mL)；
M represents sample mass, and unit is gram (g).
So set beneficial effect be：Using such scheme, using such scheme, the present invention is by adding dichloromethane
Ultrasonic extraction is carried out to leather sample, pretreatment process is simple, convenient, fast.
Secondly, the present invention is by gas phase for the qualitative and quantitative detection analysis of chlorobenzene class Components of Organic Pollutants in leather
Chromatography-mass spectroscopy instrument (GC-MS) is analyzed.One group of step-like standard working solution is first configured, then by standard working solution and to be checked
Liquid distinguishes sample introduction on gas chromatograph-mass spectrometer.The chromatographic peak retention time occurred in liquid to be checked is consistent with standard working solution,
Tolerance is less than ± 2.5 %, the relative abundance of the mass spectrometry ion corresponding to the chromatographic peak standard work suitable with concentration
The relative abundance for making solution is consistent, and relative abundance deviation is no more than regulation, then to can determine that and contain chlorobenzene class in the liquid to be checked
Compound.
Finally, this method carries out quantitative calculating using internal standard method, and v is that volume after testing sample solution nitrogen blows is in formula
1ml；M is the quality that style is weighed；C is calculated by the linear relationship for drawing in working curve, internal standard compound in linear relationship
Between 2,4,5,6- tetrachloros the concentration of xylenol be 1.0 μ g/mL, its log-of-ratio value without influence, only influence unit, specifically
Calculation, first by the peak area in reading testing sample solution in chromatogram, 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 with convincingness.
The extracting mode that the present invention is further arranged in the step 2 is ultrasonic extraction, and Extraction solvent is dichloromethane
Alkane.
So set beneficial effect be：Using such scheme, dichloromethane has splendid molten to Chlorobenzene compounds
Xie Xing, is easy to concentrate Chlorobenzene compounds in style, is easy to follow-up detection.
The present invention is further arranged in the step 2 use Rotary Evaporators to the concentration of ultrasonic extract, sets
Thickening temperature is 40 ± 5 DEG C.
So set beneficial effect be：Using such scheme, temperature rationally will not when Chlorobenzene compounds decompose,
Ensure the accuracy of experiment, at the same it is fast using this Rotary Evaporators concentration speed, improve experimental work efficiency.
The present invention is further arranged to also include extracting bearing ultrasonic using dichloromethane liquid in the step 2
The washing of the reagent bottle of liquid simultaneously obtains cleaning solution, cleaning solution is mixed with concentrate and is blown while carrying out nitrogen.
So set beneficial effect be：Using such scheme, using dichloromethane to reprinting ultrasonic extract
Sample bottle carries out once washing, and is merged with ultrasonic extract, effectively to remaining in the ultrasonic wave extraction in sample bottle
Liquid is collected, and together carries out the operation and detection of next step, effectively increases the precision of inspection, it is ensured that test knot
The accuracy of fruit.
The present invention is further arranged to the chlorobenzene titer includes 1,3- dichloro-benzenes titer, 1,4- dichloro-benzenes standards
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- tetrachlorobenzenes titer, 1,2,4,5- tetrachlorobenzenes titer, 1,2,3,4- tetrachlorobenzenes titer, pentachlorobenzene titer,
Hexachloro-benzene titer.
The detection parameter of gas chromatograph-mass spectrometer is in step 4 of the present invention：
Chromatographic condition：HP-35 MS (30 m × 0.25 mm × 0.25 μm) capillary column；Using temperature programming, initial temperature
It is 100 °C, keeps 1min, be then warming up to 240 °C with 15 °C/min, keeps 3 min；260 °C of injector temperature, carrier gas is
High-pure helium, the mL/min of flow 1.0, pulse Splitless injecting samples, sample size is 2.0 μ 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 of the drawings
Fig. 1 is the 1,3- dichloro-benzenes chemical structural formulas in the specific embodiment of the invention；
Fig. 2 is the 1,4- dichloro-benzenes chemical structural formulas in the specific embodiment of the invention；
Fig. 3 is the 1,2- dichloro-benzenes chemical structural formulas in the specific embodiment of the invention；
Fig. 4 is the 1,3,5- trichloro-benzenes chemical structural formulas in the specific embodiment of the invention；
Fig. 5 is the 1,2,4- trichloro-benzenes chemical structural formulas in the specific embodiment of the invention；
Fig. 6 is the 1,2,3- trichloro-benzenes chemical structural formulas in the specific embodiment of the invention；
Fig. 7 is the 1,2,3,5- tetrachlorobenzene chemical structural formulas in the specific embodiment of the invention；
Fig. 8 is the 1,2,4,5- tetrachlorobenzene chemical structural formulas in the specific embodiment of the invention；
Fig. 9 is the 1,2,3,4- tetrachlorobenzene chemical structural formulas 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 hexachloro-benzene chemical structural formula in the specific embodiment of the invention；
Figure 12 is 11 kinds of chlorobenzene compound standard liquid (2.0 μ g/mL) MRM chromatograms in the specific embodiment of the invention；
Figure 13 is blank leather sample figure A in the specific embodiment of the invention
Figure 14 is blank leather sample marked graph B in the specific embodiment of the invention；
Figure 15 is 1,3- dichloro-benzenes, the 1,4- dichloro-benzenes standard working curves in the specific embodiment of the invention；
Figure 16 is the 1,2- dichloro-benzenes standard working curves in the specific embodiment of the invention；
Figure 17 is the 1,3,5- trichloro-benzenes standard working curves in the specific embodiment of the invention；
Figure 18 is the 1,2,4- trichloro-benzenes standard working curves in the specific embodiment of the invention；
Figure 19 is the 1,2,3- trichloro-benzenes standard working curves in the specific embodiment of the invention；
Figure 20 is 1,2,3,5- tetrachlorobenzenes, the 1,2,4,5- tetrachlorobenzene standard working curves in the specific embodiment of the invention；
Figure 21 is the 1,2,3,4- tetrachlorobenzene standard working curves 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 hexachloro-benzene standard working curve in the specific embodiment of the invention.
Specific embodiment
It is the organic dirt of chlorobenzene class in Gas Chromatography-Mass Spectrometry leather shown in specific implementation such as Fig. 1-2 3 of the invention
The method for contaminating thing, it is comprised the following steps：
The preparation of step one, testing sample, takes appropriate leather sample, and sample is shredded, sample size scope less than 20mm ×
20mm, and sample after shredding uniformly mixes；
Step 2, sample extraction, weigh 1.00g samples, are placed in 40 mL reaction bulbs, 30 mL dichloromethane are added, in room temperature
Under the conditions of the min of ultrasonic wave extraction 30 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 concentrates, concentrate is transferred in evaporation tube, and
Boiling flask is cleaned with a small amount of dichloromethane, merging is transferred to evaporation tube, and nitrogen is blown to 1 mL.Plus 0.01 mL, 100 μ g/mL's is interior
Mark solution, obtains testing sample solution after mixing；
The configuration of step 3, standard working solution, prepares ladder concentration and is respectively 0.1 μ g/mL, 0.5 μ g/mL, 2.0 μ 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 standards
Liquid, 1,2,4,5- tetrachlorobenzene titers, 1,2,3,4- tetrachlorobenzene titers, pentachlorobenzene titer, hexachloro-benzene titer, and in chlorine
Xylenol is mixed to form standard working solution, the internal standard as internal standard compound between 2,4,5,6- tetrachloros are added in benzene titer
Solubility of the xylenol in standard working solution is 1.0 μ g/mL between the tetrachloro of thing 2,4,5,6-；
The detection of step 4, testing sample solution, by the testing sample solution and standard working solution in step 2 in gas phase color
Sample introduction is distinguished on spectrum-mass spectrograph, chromatographic condition and Mass Spectrometry Conditions are respectively,
Chromatographic condition：HP-35 MS (30 m × 0.25 mm × 0.25 μm) capillary column；Using temperature programming, initial temperature
It is 100 °C, keeps 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, the mL/min of flow 1.0, pulse Splitless injecting samples, and sample size is 2.0 μ 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
It it is 300 °C, the solvent delay time is 7 min, data acquisition scheme SIM.
Obtain with the concentration of xylenol between chlorobenzene pollutant in standard working solution and the tetrachloro of internal standard compound 2,4,5,6-
Than being abscissa, then with xylenol between chlorobenzene class organic pollution in standard working solution and the tetrachloro of internal standard compound 2,4,5,6-
Peak area ratio be the working curve of ordinate, and obtain chlorobenzene class organic contamination in 11 kinds of standard working solutions as shown in table 2
The peak area ratio of xylenol and chlorobenzene class organic pollution in standard working solution between thing and the tetrachloro of internal standard compound 2,4,5,6-
The linear relation of the concentration ratio of xylenol between the tetrachloro of internal standard compound 2,4,5,6-,
Table 2-11 kinds of linear equation, coefficient correlation, quantitative limits of chlorobenzene
The peak area ratio of testing sample solution is measured by the chromatogram of testing sample solution, peak area ratio is substituted into linear relation
The concentration of chlorobenzene in testing sample solution is drawn, and with 2, xylenol is entered for internal standard compound using internal standard method between 4,5,6- tetrachloros
Row is calculated, and chlorobenzene class organic pollution concentration in testing sample solution is obtained, wherein quantitatively computing formula is：X=cv/m
X represents the content of chlorobenzene in testing sample solution in formula, and unit is milligrams per kilogram (mg/kg)；
C represents the concentration of chlorobenzene in testing sample solution, and unit is micrograms per millilitre (μ 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 Capsuls 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
Implement of the invention with using other various specific embodiments, or it is every using design structure of the invention and thinking, do
Simple change or change, both fall within protection scope of the present invention.
Claims (6)
1. in a kind of Gas Chromatography-Mass Spectrometry leather chlorobenzene class organic pollution method, it is characterised in that including following
Step：
The preparation of step one, testing sample, takes appropriate leather sample, and sample is shredded, sample size scope less than 20mm ×
20mm, and sample after shredding is well mixed；
Step 2, sample extraction, weigh 0.70-1.30g samples, are placed in reaction bulb, 30mL dichloromethane liquid are added, in room
Carried out under the conditions of temperature 25 ~ 35min of ultrasonic wave extraction obtain ultrasonic extract, filter ultrasonic extract and concentrate acquisition 1 ~
2mL concentrates, concentrate is transferred in evaporation tube, and nitrogen is blown to 1mL, adds 2, the 4,5,6- tetra- of the μ g/mL of 0.01mL 100
Dimethyl benzene phenol solution between chlorine, described 2, dimethyl benzene phenol solution is inner mark solution between 4,5,6- tetrachloros, it is uniform mix after obtain
Testing sample solution；
The configuration of step 3, standard working solution, prepares ladder concentration and is respectively 0.1 μ g/mL, 0.5 μ g/mL, 2.0 μ g/mL's
Chlorobenzene titer, and xylenol is mixed to form standard as internal standard compound between 2,4,5,6- tetrachloros are added in chlorobenzene titer
Solubility of the xylenol in standard working solution is 1.0 μ g/mL between working solution, the tetrachloro of the internal standard compound 2,4,5,6-；
The detection of step 4, testing sample solution, by the testing sample solution and standard working solution in step 2 in gas phase color
Sample introduction is distinguished on spectrum-mass spectrograph, is obtained with chlorobenzene class organic pollution in standard working solution and the tetrachloro of internal standard compound 2,4,5,6-
Between the concentration ratio of xylenol be abscissa, then with chlorobenzene class organic pollution in standard working solution and internal standard compound 2,4,5,
The peak area ratio of xylenol is the working curve of ordinate between 6- tetrachloros, and chlorobenzene class is organic in obtaining each standard working solution
The peak area ratio of xylenol and the organic dirt of chlorobenzene class in standard working solution between pollutant and the tetrachloro of internal standard compound 2,4,5,6-
The linear relation of the concentration ratio of xylenol between dye thing and the tetrachloro of internal standard compound 2,4,5,6-, by the chromatogram of testing sample solution
Figure measures the peak area ratio of testing sample solution, and peak area ratio substitution linear relation is drawn into chlorobenzene in testing sample solution
Concentration, and with 2, xylenol is calculated for internal standard compound using internal standard method between 4,5,6- tetrachloros, obtains testing sample solution
Middle chlorobenzene class organic pollution concentration, wherein quantitatively computing formula is：X=cv/m
X represents the content of chlorobenzene in testing sample solution in formula, and unit is milligrams per kilogram (mg/kg)；
C represents the concentration of chlorobenzene in testing sample solution, and unit is micrograms per millilitre (μ 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 Gas Chromatography-Mass Spectrometry leather according to claim 1 chlorobenzene class organic pollution method, it is special
Levy and be：Extracting mode in the step 2 is ultrasonic extraction, and Extraction solvent is dichloromethane.
3. in Gas Chromatography-Mass Spectrometry leather according to claim 1 chlorobenzene class organic pollution method, it is special
Levy and be：Concentration in the step 2 to ultrasonic extract uses Rotary Evaporators, and it is 40 ± 5 DEG C to set thickening temperature.
4. in Gas Chromatography-Mass Spectrometry leather according to claim 1 chlorobenzene class organic pollution method, it is special
Levy and be：Also include using dichloromethane liquid is to the washing of the reagent bottle of bearing ultrasonic extract solution and obtains in the step 2
Cleaning solution is obtained, cleaning solution is mixed with concentrate and is blown while carrying out nitrogen.
5. in Gas Chromatography-Mass Spectrometry leather according to claim 1 chlorobenzene class organic pollution method, it is special
Levy and be：The chlorobenzene titer include 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- tetrachlorobenzene standards
Liquid, 1,2,4,5- tetrachlorobenzenes titer, 1,2,3,4- tetrachlorobenzenes titer, pentachlorobenzene titer, hexachloro-benzene titer.
6. in a kind of leather according to claim 1 chloro- benzenes contamination thing detection method, it is characterised in that：Described step
The detection parameter of gas chromatograph-mass spectrometer is in rapid four：
Chromatographic condition：HP-35 MS (30 m × 0.25 mm × 0.25 μm) capillary column；Using temperature programming, initial temperature
It is 100 °C, keeps 1min, be then warming up to 240 °C with 15 °C/min, keeps 3 min；260 °C of injector temperature, carrier gas is
High-pure helium, the mL/min of flow 1.0, pulse Splitless injecting samples, sample size is 2.0 μ 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
It it is 300 °C, the solvent delay time is 7 min, data acquisition scheme SIM.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044509A (en) * | 2019-12-24 | 2020-04-21 | 北京建工环境修复股份有限公司 | Method for quickly identifying chlorobenzene pollutants in soil and evaluating concentration of chlorobenzene pollutants |
| CN111044508A (en) * | 2019-12-24 | 2020-04-21 | 北京建工环境修复股份有限公司 | Method for rapidly evaluating pollution level of chlorobenzene substances in water body |
| CN111796040A (en) * | 2020-07-14 | 2020-10-20 | 南京海关工业产品检测中心 | Method for separating isomeride chlorobenzene and toluene chloride by adopting gas chromatography-mass spectrometry |
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| CN111044509A (en) * | 2019-12-24 | 2020-04-21 | 北京建工环境修复股份有限公司 | Method for quickly identifying chlorobenzene pollutants in soil and evaluating concentration of chlorobenzene pollutants |
| CN111044508A (en) * | 2019-12-24 | 2020-04-21 | 北京建工环境修复股份有限公司 | Method for rapidly evaluating pollution level of chlorobenzene substances in water body |
| CN111796040A (en) * | 2020-07-14 | 2020-10-20 | 南京海关工业产品检测中心 | Method for separating isomeride chlorobenzene and toluene chloride by adopting gas chromatography-mass spectrometry |
| CN111796040B (en) * | 2020-07-14 | 2021-03-16 | 南京海关工业产品检测中心 | Method for separating isomeride chlorobenzene and toluene chloride by adopting gas chromatography-mass spectrometry |
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