CN111220714A - Method for detecting chlorobenzene and toluene chloride in textiles, leather and toys - Google Patents
Method for detecting chlorobenzene and toluene chloride in textiles, leather and toys Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to the technical field of chemical detection, and particularly relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys. The method for detecting chlorobenzene and toluene chloride in textiles, leather and toys specifically comprises the following steps: A. preparing a standard solution; B. pretreating a sample; C. and carrying out gas chromatography-mass spectrometry detection on the sample to be detected. The beneficial effects are as follows: the method for detecting the chlorobenzene and the toluene chloride in the textiles, the leather and the toys has the advantages of wide linear range, high recovery rate and good precision, the detection limit meets the limit value of an Oeko-Tex _ Standard _100 regulation, and the method is economical, efficient, easy to popularize and use in laboratories and well applicable to detection of the chlorobenzene and the toluene chloride in the textiles, the leather and the toys.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and particularly relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys.
Background
As is known, the colorful and various functional textiles need to be treated by chemical dyes, and polyester fibers have quite compact supermolecular structure and no active groups on chain segments, and must be dyed at high temperature and high pressure when dyed by disperse dyes. Research shows that most dyeing carriers have potential teratogenicity and carcinogenicity to human body, are not easy to decompose and are very harmful to environment, and the European Union currently limits the total amount of residual quantity of the dyeing carriers in textiles to be not more than 1.0PPM. Therefore, the organic chlorine carrier in the textile is increasingly becoming the focus of people's attention and scientific research as an important item of the standard detection system of the ecological textile. At present, for the detection of the project, domestic and foreign standards are numerous, the cost and the effect of the method are different, and the seeking of a uniform, accurate, rapid and low-cost detection method is a necessary trend of the industry.
Disclosure of Invention
The invention provides a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys in order to make up for the defects of the prior art.
The invention relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys, which comprises the following steps:
A. preparing a standard solution:
preparing standard substances of chlorobenzene and toluene chloride and standard stock solution of internal standard: weighing a certain amount of standard substance and an internal standard substance, and respectively dissolving HPLC-grade dichloromethane in 9-11mL volumetric flasks to prepare 800-1100mg/L stock solution;
preparation of standard working solution: accurately transferring a proper amount of standard stock solution, and preparing linear standard working solution of 0.02mg/L, 0.1mg/L and 1mg/L by using HPLC-grade dichloromethane;
B. sample pretreatment:
accurately weighing 1-3 g of the pretreated sample, placing the sample in a 40-60mL glass reaction bottle, adding an organic solvent, carrying out ultrasonic extraction for 30-60min at normal temperature, cooling to room temperature, filtering the extracting solution by using a 0.45 mu m PTFE (polytetrafluoroethylene) microporous filter membrane, and taking the filtrate as a sample to be detected;
C. carrying out gas chromatography-mass spectrometry detection on a sample to be detected:
the gas chromatography conditions were: a chromatographic column: HP-5 MS; column temperature conditions: initial temperature is 30-50 deg.C, maintaining for 0-2min, then raising to 250-280 deg.C at rate of 10-25 deg.C/min, and maintaining for 0-2 min; the temperature of a sample inlet is 250-300 ℃; and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1-2 μ L; carrier gas: high purity helium, purity >99.999%, flow: 1-2 ml/min;
the mass spectrum conditions are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃;
interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 3-5 min;
an acquisition mode: qualitative full ion scan, quantitative selective ion scan.
In some embodiments, in the step B, the ultrasonic temperature is 30 ℃ and the ultrasonic extraction time is 30 min; the organic solvent was dichloromethane, the internal standard was 2,4,5, 6-tetrachloro-m-xylene, and the concentration was 1.0mg/L, which was optimal for the choice of sonication temperature and time, as is evident from the example results.
In some of these embodiments, the solid sample is pre-treated in step B by shearing the sample to a size of 1mm x 1mm, which increases the surface area in contact with the extraction solvent to facilitate adequate extraction.
In some examples, 2.0g of the pretreated sample is accurately weighed in step B and placed in a 40mL glass reaction flask, the organic solvent is dichloromethane, the addition amount is 10mL, and the addition amount of the internal standard is 1.0 mg/L. 2.0g of sample is selected, the amount of the used extraction reagent is moderate, the volume concentration of the extracted detection object can meet the sensitivity requirement, and the response ratio of the internal standard response and the linear concentration of 1.0mg/L is proper, thereby being beneficial to quantification.
In some of these embodiments, the gas chromatography conditions in step C are: a chromatographic column: HP-5 MS; column temperature conditions: the initial temperature is 50 ℃, the temperature is kept for 0min, and then the temperature is increased to 270 ℃ at the speed of 11 ℃/min and the temperature is kept for 0 min; the temperature of a sample inlet is 250 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 2 mu L of the solution; carrier gas: high purity helium, purity >99.999%, flow: 1.0 ml/min. These parameters were selected by the inventors based on experience and a number of tests, and were obtained by taking into account the lifetime of the column, the sensitivity of the sample, the time of analysis, and the like.
The mass spectrum conditions are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃; interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 4.0 min; an acquisition mode: qualitative full ion scan, quantitative selective ion scan. The parameters of the electron energy, the ion source temperature and the chromatography-mass spectrometry interface temperature are considered to be optimal parameters by experiments of the inventor, and are particularly applied to Agilent equipment; the solvent delay of 4.0min is selected to firstly enable the detected substances to flow out, and secondly prevent the substances containing more impurities before 4.0min from entering the mass spectrum, thereby protecting the instrument.
In some embodiments, the specification parameter 30m 0.25mm of the chromatographic column in step C is selected to achieve the purpose, mainly from the viewpoint of cost, so that the cost can be effectively reduced.
The detection method uses dichloromethane as an extraction solvent, ultrasonically extracts chlorobenzene chloride and toluene chloride in textiles, leather and toys, then selects the type of a chromatographic column, optimizes extraction conditions, establishes the gas-mass combined detection method through mutual close cooperation of the aspects, and proves accurate and practical effects through verification experiments such as linearity, recovery rate, precision and the like.
The detection method is simple, convenient and quick, has high sensitivity, is in a linear relation within the range of 0.02-1 mg/L, has a correlation coefficient of 0.9995, has a detection limit of 0.05mg/L, has a standard addition recovery rate of 89-108 percent, has a Relative Standard Deviation (RSD) (n =7) of less than 10 percent, and meets the standard specified in the industry: the correlation coefficient is 0.99, the detection limit of the method is 0.1mg/L, the adding standard recovery rate and RSD are related to the adding standard concentration, and compared with the requirements that the adding standard recovery rate of the detection limit concentration is 80-120% and the RSD is less than 20%, the accuracy of the detection method can meet the requirements of analysis and detection, and even exceeds the standard value on three results of the correlation coefficient, the detection limit, the adding standard recovery rate and the RSD, so that the detection method is proved to have remarkable effect and can be well applied to detection of chlorobenzene and toluene chloride in textiles, leather and toys.
The invention has the beneficial effects that: the method for detecting the chlorobenzene and the toluene chloride in the textiles, the leather and the toys has the advantages of wide linear range, high recovery rate and good precision, the detection limit meets the limit value of an Oeko-Tex _ Standard _100 regulation, and the method is economical, efficient, easy to popularize and use in laboratories and well applicable to detection of the chlorobenzene and the toluene chloride in the textiles, the leather and the toys.
Drawings
FIG. 1 is a chromatogram of chlorinated benzenes and chlorinated toluenes in the examples, wherein the abscissa is retention time and the ordinate is signal intensity;
FIG. 2 is a standard working curve of pentachlorobenzene, a representative material of chlorinated benzenes and chlorinated toluenes in the examples;
FIG. 3 is a graph showing the recovery rate of the extraction results in example 4 at different ultrasonic temperatures and times.
Detailed Description
Specific examples of the present invention are given below to further explain the constitution of the present invention.
All instruments, reagents included in the following examples:
1. instrument for measuring the position of a moving object
GCMS-7890B/5977B gas chromatography-mass spectrometry combined instrument;
KQ-500DE type ultrasonic generator;
HP-5MS (30 m 0.25 mm) chromatography column;
0.45 μm PTFE filter head.
2. Reagent
And (3) standard substance: 1, 2-dichlorobenzene, 1, 3-dichlorobenzene, 1, 4-dichlorobenzene, 1,2, 3-trichlorobenzene, 1,2, 4-trichlorobenzene, 1,3, 5-trichlorobenzene, 1,2,3, 4-tetrachlorobenzene, 1,2,3, 5-tetrachlorobenzene, 1,2,4, 5-tetrachlorobenzene, pentachlorobenzene, hexachlorobenzene, 2-chlorotoluene, 3-chlorotoluene, 4-chlorotoluene, 2, 3-dichlorotoluene, 2, 4-dichlorotoluene, 2, 5-dichlorotoluene, 2, 6-dichlorotoluene, 3, 4-dichlorotoluene, 2,3, 6-trichlorotoluene, 2,4, 5-trichlorotoluene, tetrachlorotoluene, 2,3,4,5, 6-pentachlorotoluene, 2,4,5, 6-tetrachloro-m-xylene, dichloromethane.
Example 1
The invention relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys, which comprises the following steps:
A. preparing a standard solution:
preparing standard substances of chlorobenzene and toluene chloride and standard stock solution of internal standard: weighing a certain amount of standard substance and an internal standard substance, and respectively dissolving HPLC-grade dichloromethane in 9mL volumetric flasks to prepare 800mg/L stock solution;
preparation of standard working solution: accurately transferring a proper amount of standard stock solution, and preparing linear standard working solution of 0.02mg/L, 0.1mg/L and 1mg/L by using HPLC-grade dichloromethane;
B. sample pretreatment:
accurately weighing 1g of the pretreated sample, placing the sample in a 40mL glass reaction bottle, adding an organic solvent, carrying out ultrasonic extraction for 30min, cooling to room temperature, filtering the extracting solution by using a 0.45-micron PTFE (polytetrafluoroethylene) microporous filter membrane, and taking the filtrate as a sample to be detected;
C. carrying out gas chromatography-mass spectrometry detection on a sample to be detected:
the gas chromatography conditions were: a chromatographic column: HP-5 MS; column temperature conditions: the initial temperature is 30 ℃, the temperature is kept for 0min, then the temperature is increased to 250 ℃ at the speed of 10 ℃/min, and the temperature is kept for 0 min; the temperature of a sample inlet is 250 ℃; and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1 mu L of the solution; carrier gas: high purity helium, purity >99.999%, flow: 1 ml/min;
the mass spectrum conditions are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃;
interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 3 min;
an acquisition mode: qualitative full ion scan, quantitative selective ion scan.
Example 2
The invention relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys, which comprises the following steps:
A. preparing a standard solution:
preparing standard substances of chlorobenzene and toluene chloride and standard stock solution of internal standard: weighing a certain amount of standard substance and an internal standard substance, and respectively dissolving HPLC-grade dichloromethane in 10mL volumetric flasks to prepare 1000mg/L stock solution;
preparation of standard working solution: accurately transferring a proper amount of standard stock solution, and preparing linear standard working solution of 0.02mg/L, 0.1mg/L and 1mg/L by using HPLC-grade dichloromethane;
B. sample pretreatment:
accurately weighing 2g of the pretreated sample, placing the sample in a 50mL glass reaction bottle, adding an organic solvent, carrying out ultrasonic extraction for 50min at normal temperature, cooling to room temperature, filtering the extracting solution by using a 0.45-micron PTFE microporous filter membrane, and taking the filtrate as a sample to be detected;
C. carrying out gas chromatography-mass spectrometry detection on a sample to be detected:
the gas chromatography conditions were: a chromatographic column: HP-5 MS; column temperature conditions: the initial temperature is 40 ℃, the temperature is kept for 1min, then the temperature is increased to 260 ℃ at the speed of 120 ℃/min, and the temperature is kept for 1 min; the sample inlet temperature is 280 ℃; and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1.5 mu L; carrier gas: high purity helium, purity >99.999%, flow: 1.5 ml/min;
the mass spectrum conditions are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃;
interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 4 min;
an acquisition mode: qualitative full ion scan, quantitative selective ion scan.
Example 3
The invention relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys, which comprises the following steps:
A. preparing a standard solution:
preparing standard substances of chlorobenzene and toluene chloride and standard stock solution of internal standard: weighing a certain amount of standard substance and an internal standard substance, and respectively dissolving HPLC-grade dichloromethane in 11mL volumetric flasks to prepare 1100mg/L stock solution;
preparation of standard working solution: accurately transferring a proper amount of standard stock solution, and preparing linear standard working solution of 0.02mg/L, 0.1mg/L and 1mg/L by using HPLC-grade dichloromethane;
B. sample pretreatment:
accurately weighing 3g of the pretreated sample, placing the sample in a 60mL glass reaction bottle, adding an organic solvent, carrying out ultrasonic extraction at normal temperature for 60min, cooling to room temperature, filtering the extracting solution by using a 0.45-micron PTFE microporous filter membrane, and taking the filtrate as a sample to be detected;
C. carrying out gas chromatography-mass spectrometry detection on a sample to be detected:
the gas chromatography conditions were: a chromatographic column: HP-5 MS; column temperature conditions: the initial temperature is 50 ℃, the temperature is kept for 2min, then the temperature is raised to 280 ℃ at the speed of 25 ℃/min, and the temperature is kept for 2 min; the temperature of a sample inlet is 300 ℃; and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 2 mu L of the solution; carrier gas: high purity helium, purity >99.999%, flow: 2 ml/min;
the mass spectrum conditions are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃;
interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 5 min;
an acquisition mode: qualitative full ion scan, quantitative selective ion scan.
Example 4
The invention relates to a method for detecting chlorobenzene and toluene chloride in textiles, leather and toys, which comprises the following steps:
A. standard solution preparation
Preparing standard substances of chlorobenzene and toluene chloride and standard stock solution of internal standard: weighing a certain amount of standard substance and internal standard substance, and respectively dissolving in 10mL volumetric flasks with HPLC-grade dichloromethane to prepare 1000mg/L stock solution.
Preparation of standard working solution: accurately transferring a proper amount of standard stock solution, and preparing linear standard working solution (the internal standard is 1.0 mg/L) of 0.02mg/L, 0.1mg/L and 1mg/L by using HPLC-grade dichloromethane;
B. sample pretreatment
Sampling: a representative sample is taken, cut to a size of about 1mm by 1mm, and 2.0g (to the nearest degree) is accurately weighed
0.001 g) of the reaction solution, and placing the reaction solution in a 40mL glass reaction bottle; adding an extracting agent: adding 10mL of dichloromethane into a glass reaction bottle, plugging and sealing; ultrasonic extraction: placing the reaction bottle in an ultrasonic generator, and carrying out ultrasonic extraction at 30 ℃ for 30min, wherein the temperature and the time are optimal as can be seen from a graph of the extraction results under different ultrasonic temperatures and times in the step A in the embodiment shown in FIG. 3; and (3) filtering: filtering the extractive solution with 0.45 μm PTFE microporous membrane, and collecting filtrate as sample to be tested.
C. And (3) analyzing a sample to be detected by using a gas chromatography-mass spectrometer (GC-MS), and performing qualitative retention time and quantitative standard curve internal standard method.
Gas chromatography conditions:
a chromatographic column: HP-5MS (30 m 0.25 mm);
column temperature conditions: the initial temperature is 50 ℃, the temperature is kept for 0min, and then the temperature is increased to 270 ℃ at the speed of 11 ℃/min and the temperature is kept for 0 min;
sample inlet temperature: 250 ℃;
and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 2 mu L of the solution;
carrier gas: high purity helium (> 99.999%) flow: 1.0 ml/min;
mass spectrum conditions:
an ionization mode: electron Impact (EI) ionization, electron energy 70 eV;
ion source temperature: 230 ℃;
interface temperature of chromatography-mass spectrometry: 300 ℃;
solvent retardation: 4.0 min;
an acquisition mode: total ion SCAN (SCAN) qualitative, selective ion SCAN (SIM) quantitative.
The retention time and characteristic fragment ions of the target substance o-benzene in example 4 are shown in table 1, and the chromatogram of the chlorinated benzene and the chlorinated toluene in example 4 is shown in fig. 1, wherein the abscissa is the retention time, and the ordinate is the signal intensity;
TABLE 1 retention time, characteristic fragment ion and abundance ratio of target
| Name of substance | Retention time/min | Characteristic fragment ion/amu | Abundance ratio |
| 2&3&4-chlorotoluene | 4.890 | 91,126,63 | 100,38.5,10.4 |
| 1, 3-dichlorobenzene | 5.540 | 146,148,111 | 100,57.8,30.9 |
| 1, 4-dichlorobenzene | 5.620 | 146,148,111 | 100,61.5,34.9 |
| 1, 2-dichlorobenzene | 5.941 | 146,148,111 | 100,64.4,38.2 |
| 2,4&2,5&2, 6-dichlorotoluene | 7.108 | 125,160,89 | 100,44.0,31.7 |
| 1,3, 5-trichlorobenzene | 7.278 | 180,182,145 | 100,95.2,27.6 |
| 2,3&3, 4-Dichlorotoluene | 7.500 | 125,160,89 | 100,40.5,24.5 |
| 1,2, 4-trichlorobenzene | 7.884 | 180,182,145 | 100,96.1,28.5 |
| 1,2, 3-trichlorobenzene | 8.374 | 180,182,145 | 100,96.0,30.0 |
| 2,4, 5-trichlorotoluene | 9.414 | 159,194,123 | 100,47.2,26.6 |
| 2,3, 6-trichlorotoluene | 9.568 | 159,194,123 | 100,53.0,39.2 |
| 1,2,3,5&1,2,4, 5-tetrachlorobenzene | 9.849 | 216,214,218 | 100,78.1,47.7 |
| 1,2,3, 4-tetrachlorobenzene | 10.467 | 216,214,218 | 100,78.1,48.0 |
| Pentachlorobenzene | 12.125 | 250,252,215 | 100,64.1,21.2 |
| 2,3,4,5, 6-pentachlorotoluene | 13.825 | 229,264,193 | 100,66.3,27.7 |
| Hexachlorobenzene | 14.190 | 284,286,282 | 100,80.1,50.7 |
| Tetrachlorotoluene | 10.566 | 193,195,123 | 100,84.5,25.7 |
As is clear from table 1 and fig. 1, the target substance was separated well under the detection conditions of example 4.
The linear relationship is:
under the optimized detection condition, the standard solution is detected in the concentration range of 0.02-0.5 mg/L, the standard working curve is shown in figure 2, as can be seen from figure 2, the concentration and the response value have a good linear relation, and the correlation coefficient R2= 0.9997.
Detection limit:
under the optimized detection condition, standard samples with different concentrations are analyzed and detected, and the lowest detected concentration (S/N > 3) of the chlorobenzene and the toluene chloride is 0.02 mg/L. The Oeko-Tex _ Standard-100 regulation has a limit value of 0.1mg/kg for organic substances.
Precision degree
Under the optimized detection condition, the standard sample of 0.5mg/L is continuously detected for 7 times, and the result is shown in Table 2, and the relative standard deviation RSD is 3.2-10.2%, so that the precision can meet the requirement of analysis and detection under the condition of the detection method.
TABLE 2 precision experiment of o-benzene
And (3) recovery rate:
under the optimized detection condition, the target substances with different levels are added into the sample without the target substances, the sample is pretreated according to the method of the embodiment 4, the standard addition recovery rate of the detected target substances is performed, each level is performed for 3 times, the result is shown in the table 3, the recovery rate of the obtained o-benzene is between 94 and 109 percent, and the accuracy of the method can meet the requirement of analysis and detection.
TABLE 3 phthalic acid standard recovery experiment
As can be seen from examples 1 to 4, the detection method of the present invention has a wide linear range, high recovery rate, good precision, and a detection limit satisfying the limit value of the Oeko-Tex _ Standard-100 regulation. The detection method is economical and efficient, is easy to popularize and use in laboratories, and can be well applied to detection of chlorobenzene and toluene chloride in textiles, leather and toys.
The present invention is not limited to the above embodiments, and any technical solutions similar or identical to the present invention, which are made in the light of the present invention, are within the scope of the present invention.
Claims (7)
1. A method for detecting chlorobenzene and toluene chloride in textiles, leather and toys is characterized by comprising the following steps:
A. preparing a standard solution:
preparing standard substances of chlorobenzene and toluene chloride and standard stock solution of internal standard: weighing a certain amount of standard substance and an internal standard substance, and respectively dissolving HPLC-grade dichloromethane in 9-11mL volumetric flasks to prepare 800-1100mg/L stock solution;
preparation of standard working solution: accurately transferring a proper amount of standard stock solution, and preparing linear standard working solution of 0.02mg/L, 0.1mg/L and 1mg/L by using HPLC-grade dichloromethane;
B. sample pretreatment:
accurately weighing 1-3 g of the pretreated sample, placing the sample in a 40-60mL glass reaction bottle, adding an organic solvent, carrying out ultrasonic extraction for 30-60min at normal temperature, cooling to room temperature, filtering the extracting solution by using a 0.45 mu m PTFE (polytetrafluoroethylene) microporous filter membrane, and taking the filtrate as a sample to be detected;
C. carrying out gas chromatography-mass spectrometry detection on a sample to be detected:
the gas chromatography conditions were: a chromatographic column: HP-5 MS; column temperature conditions: initial temperature is 30-50 deg.C, maintaining for 0-2min, then raising to 250-280 deg.C at rate of 10-25 deg.C/min, and maintaining for 0-2 min; the temperature of a sample inlet is 250-300 ℃; and (3) sample introduction mode: no shunt sampling;
sample introduction amount: 1-2 μ L; carrier gas: high purity helium, purity >99.999%, flow: 1-2 ml/min;
the mass spectrum conditions are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃;
interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 3-5 min;
an acquisition mode: qualitative full ion scan, quantitative selective ion scan.
2. The method for detecting chlorobenzene and chlorotoluene in textiles, leather and toys as claimed in claim 1, wherein the method comprises the following steps: in the step B, the ultrasonic temperature is 30 ℃, and the ultrasonic extraction time is 30 min; the organic solvent is dichloromethane, the internal standard is 2,4,5, 6-tetrachloro-m-xylene, and the concentration is 1.0 mg/L.
3. The method for detecting chlorobenzene and chlorotoluene in textiles, leather and toys as claimed in claim 1, wherein the method comprises the following steps: in the step B, the solid sample is preprocessed by cutting the sample into the size of 1mm multiplied by 1mm, and the size of the sample can increase the surface area contacted with the extraction solvent and is beneficial to full extraction.
4. The method for detecting chlorobenzene and chlorotoluene in textiles, leather and toys as claimed in claim 1, wherein the method comprises the following steps: and B, accurately weighing 2.0g of the pretreated sample in the step B, placing the sample in a 40mL glass reaction bottle, wherein the organic solvent is dichloromethane, the adding amount is 10mL, the added internal standard is 1.0mg/L, selecting 2.0g of the sample, the amount of the used extraction reagent is moderate, the volume concentration of the extracted detection object can meet the sensitivity requirement, and the response ratio of the internal standard of 1.0mg/L to the linear concentration is proper, so that the quantification is facilitated.
5. The method for detecting chlorobenzene and chlorotoluene in textiles, leather and toys as claimed in claim 1, wherein the method comprises the following steps: the gas chromatography conditions in the step C are as follows: a chromatographic column: HP-5 MS; column temperature conditions: the initial temperature is 50 ℃, the temperature is kept for 0min, and then the temperature is increased to 270 ℃ at the speed of 11 ℃/min and the temperature is kept for 0 min; the temperature of a sample inlet is 250 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 2 mu L of the solution; carrier gas: high purity helium, purity >99.999%, flow: 1.0 ml/min.
6. The method for detecting chlorobenzene and chlorotoluene in textiles, leather and toys as claimed in claim 1, wherein the method comprises the following steps: the mass spectrum conditions in the step C are as follows: an ionization mode: electron bombardment ionization, wherein the electron energy is 70 eV; ion source temperature: 230 ℃; interface temperature of chromatography-mass spectrometry: 300 ℃; solvent retardation: 4.0 min; an acquisition mode: and (3) all-ion scanning is qualitative, ion scanning is quantitative, 4.0min of solvent delay is selected, firstly, a detected substance can flow out, and secondly, a substance containing more impurities before 4.0min can be prevented from entering a mass spectrum, so that an instrument is protected.
7. The method for detecting chlorobenzene and chlorotoluene in textiles, leather and toys as claimed in claim 1, wherein the method comprises the following steps: the column in step C has a specification parameter of 30m 0.25 mm.
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| 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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| CN115184524A (en) * | 2022-08-22 | 2022-10-14 | 普研（上海）标准技术服务有限公司 | Method for detecting content of 1,3, 5-trichlorobenzene in soil |
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