CN112710761B - Method for determining chlorine organic pollutants in textile raw material solid waste - Google Patents
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Abstract
The invention discloses a method for determining chlorine organic pollutants in textile raw material solid waste, which comprises the steps of extracting and purifying the chlorine organic pollutants in a textile raw material solid waste sample to be detected by adopting an ultrasonic-assisted extraction/solid-phase extraction-gas chromatography-mass spectrometry method, and then determining the type and the content of the chlorine organic pollutants in the textile raw material solid waste sample to be detected by GC/MS detection. The method comprises the steps of establishing pretreatment conditions and detecting a sample; the method comprises the steps of preparing a standard solution of chlorine organic pollutants, carrying out GC/MS test on the standard solution, determining the type and characteristic ions of a target substance, and further carrying out experimental test on a sample. The method has the advantages of high sensitivity, good recovery rate and strong accuracy, and can meet the requirement of detecting the chlorine organic pollutants in the textile raw material solid waste. The method provides technical support for fighting the adulteration and smuggling of textiles, and national textile raw material import and export control, negotiation, risk analysis and the like; meanwhile, the method has important significance for comprehensive utilization of waste textile raw materials.
Description
Technical Field
The invention relates to a method for determining chlorine organic pollutants in textile raw material solid waste.
Technical Field
Chlorobenzene and chlorotoluene compounds are important organic solvents, chemical raw materials and intermediates, can be accumulated in organisms through the migration modes of respiration, skin contact, drinking water and the like, have the effects of carcinogenesis, carcinogenesis and teratogenesis, and are listed as one of the priority control pollutants in many countries and organizations.
Therefore, in order to forbid trade fraud behaviors such as 'adulterated toxic textiles', 'smuggled textiles' and the like, technical support is provided for national excellent in and out, regulation of textile raw material import, international negotiation, risk analysis and the like; in addition, in order to meet the requirements of 'detected, fast detected and accurate detected' major customs work, the waste textile raw materials which are safe, sanitary and environment-friendly are comprehensively utilized according to the development concept of domestic circular economy and the principle of 'harmlessness, reduction and recycling' of wastes, and the establishment of the detection technology of the chlorine organic pollutants in the solid wastes of the textile raw materials has important significance.
The ultrasonic extraction method is different from pretreatment technologies such as accelerated solvent extraction, solid phase extraction, microwave extraction, liquid-liquid extraction, headspace extraction and the like, is a low-cost, rapid and time-saving pretreatment method, is widely applied to detection of chlorine organic pollutants in the fields of environment, biology and the like, but has not been reported at home and abroad for detection of chlorine organic pollutants in textile raw material solid waste by applying the ultrasonic extraction method. And because the matrix of the textile raw material solid waste is complex, and the target object is not easy to obtain an accurate and stable result, a method for quickly and accurately measuring the chlorine organic pollutants in the textile raw material solid waste is urgently needed.
Disclosure of Invention
In order to solve the problems and achieve the purpose, the invention provides a method for determining chlorine organic pollutants in textile raw material solid waste, which adopts ultrasonic-assisted extraction and solid-phase extraction to carry out extraction and purification pretreatment on the chlorine organic pollutants in the textile raw material solid waste, and uses gas chromatography-tandem mass spectrometry to carry out quantification and qualitative analysis, thereby establishing a simple, efficient and accurate analysis method suitable for the chlorine organic pollutants in the textile raw material solid waste. The specific technical scheme is as follows:
a method for determining chlorine organic pollutants in textile raw material solid waste adopts an ultrasonic-assisted extraction/solid-phase extraction-gas chromatography-mass spectrometry method to extract and purify the chlorine organic pollutants in a sample of the textile raw material solid waste to be detected, and then determines the type and content of the chlorine organic pollutants in the sample of the textile raw material solid waste to be detected through GC/MS detection.
The method for determining the chlorine organic pollutants in the textile raw material solid waste comprises the steps of establishing a pretreatment condition and detecting a sample; the method comprises the steps of preparing a standard solution of chlorine organic pollutants, carrying out GC/MS test on the standard solution, determining the type and characteristic ions of a target substance, and further carrying out experimental test on a sample.
The establishing of the pretreatment condition specifically comprises the following steps:
s1-1: preparing a single-component standard stock solution: accurately weighing a proper amount of chlorine organic pollutant standard substances respectively, dissolving and diluting the chlorine organic pollutant standard substances to a constant volume by using dichloromethane, oscillating the chlorine organic pollutant standard substances on a vortex machine to fully dissolve the chlorine organic pollutant standard substances, preparing a single-component standard stock solution with the concentration of 1000mg/L, and storing the single-component standard stock solution at the temperature of minus 4 ℃ for later use;
s1-2: preparing a mixed standard working solution: respectively and accurately measuring the single-component standard stock solutions prepared in the step S1-1, mixing the single-component standard stock solutions in a volumetric flask, using dichloromethane to fix the volume, and preparing each single-component standard stock solution into a mixed standard working solution with a certain concentration;
s1-3: ion detection: performing ion full scanning on the mixed standard working solution prepared in the step S1-2 through a chromatographic column temperature-raising program to obtain a total ion current chromatogram of a target substance;
s1-4: determining the species and the characteristic ions: determining the peak-appearing time of each chlorine organic pollutant standard substance in the mixed standard stock solution according to the chromatogram obtained by ion scanning in the step S1-3, and determining the types and characteristic ions of the fragment ions according to the mass spectrogram, thereby establishing the pretreatment condition of the GC/MS-SIM method.
In step S1-1, the standard substance for chlorine-based organic pollutants includes: chlorobenzene (99.9%), 1, 2-dichlorobenzene (99.8%), 1, 3-dichlorobenzene (99.7%), 1, 4-dichlorobenzene (99.9%), 1,2, 3-trichlorobenzene (99.9%), 2, 5-dichlorotoluene (99.9%), 2, 4-dichlorotoluene (99.1%), 2, 3-dichlorotoluene (99.4%), 1,3, 5-trichlorobenzene (99.9%), 2, 6-dichlorotoluene (99.6%), 1,2, 4-trichlorobenzene (99.6%), 1,2,4, 5-tetrachlorobenzene (99.4%), 1,2,3, 5-tetrachlorobenzene (99.0%), a, a, a-trichlorotoluene (99.6%), a, a, a-2-tetrachlorotoluene (99.5%), pentachlorobenzene (98.1%), hexachlorobenzene (99.9%), 17 kinds of chlorine-based organic contaminants.
Preferably, in step S1-2, the concentration of the mixed standard working solution is 40 mg/L.
In a preferred technical scheme, in step S1-3, the chromatographic column used for ion detection is an active 19091N-133 type HP-inowax chromatographic column, the specification of which is 30m × 250mm × 0.25 μm, the injection port temperature is 250 ℃, the flow rate is 1.0mL/min, the sample is injected without split flow, the sample injection amount is 1 μ L, the carrier gas is nitrogen, and the spacer purge flow is 3 mL/min; the temperature raising procedure is as follows: the initial temperature is 45 ℃, the temperature is kept for 2min, the temperature is raised to 230 ℃ at the speed of 20 ℃/min, the temperature is kept for 5min, the temperature is raised to 250 ℃ at the speed of 15 ℃/min, and the temperature is kept for 2 min; the chromatogram is measured by using an EI source mass spectrometer, and the ion source temperature is 250 ℃, and the quadrupole rod temperature is 150 ℃; the full scan solvent delay was 5 min.
The experimental test of the sample specifically comprises the following steps:
s2-1: ultrasonic extraction: cutting a textile solid waste sample to be detected into fragments, uniformly mixing the fragments with a certain amount of standard mixed standard solution, and standing for 1 h; placing the mixed sample in an ultrasonic cleaner, extracting by using an ultrasonic extraction solvent in a water bath, filtering, and transferring the extract liquor to be purified;
s2-2: SPE purification: pouring the extract liquid obtained by ultrasonic extraction in the step S2-1 into a solid phase extraction column, eluting by using a solid phase extraction eluent, carrying out blow concentration on the elution liquid nitrogen, and fixing the volume to 1m by using dichloromethane for GC/MS (gas chromatography/mass spectrometry) machine detection;
s2-3: ion detection: scanning the eluent subjected to solid phase extraction in the step S2-2 by adopting an HP-INNOWAX chromatographic column temperature-rising program to obtain an ion current chromatogram of a target substance contained in the eluent;
s2-4: determining the target substance: and (4) analyzing the ion current chromatogram in the step S2-3, determining the types and characteristic ions according to the total ion current chromatogram of the mixed standard working solution, and simultaneously determining the chlorine organic pollutants contained in the textile solid waste sample to be detected.
In a preferred technical scheme, in the step S2-1, the sample is cut to a specification of 5mm × 5 mm; the ultrasonic extraction solvent is n-hexane, acetone or dichloromethane, preferably dichloromethane; the ultrasonic extraction time is 10-50min, preferably 30 min; the filtration is performed by a polytetrafluoroethylene membrane filter head, and the specification of the filtration is preferably 0.2 mu m.
In a preferred embodiment, in step S2-2, the solid phase extraction column is a Florisil solid phase extraction column; the SPE purification method comprises the following steps: the Florisil solid phase extraction column was activated with 10mL of n-hexane, ethyl acetate, acetone, dichloromethane and methanol, and the liquid to be measured was poured into the solid phase column, and then eluted with 15mL of n-hexane, ethyl acetate, acetone, dichloromethane and methanol, respectively, or eluted with acetone solution alone.
The invention has the beneficial effects that:
the method adopts an ultrasonic-assisted extraction method and a solid-phase extraction method to carry out extraction and purification pretreatment on chlorine organic pollutants in the textile raw material solid waste, establishes an analysis method of UAV/SPE-GC/MS, and then detects and analyzes the chlorine organic pollutants in the textile raw material solid waste to be detected by using the method. The method has the advantages of high sensitivity, good recovery rate and strong accuracy, and can meet the detection requirement of the chlorine organic pollutants in the textile raw material solid waste.
In the method, because the polarity of the chlorine organic pollutants is mostly nonpolar or weakly polar, according to the similar compatibility principle, the extraction effect is better by nonpolar or medium polar normal hexane, acetone and dichloromethane, and the dichloromethane extraction effect is best through inspection. In addition, in the aspect of grasping the extraction time, when the extraction is carried out for 30min, the extraction efficiency of the 17 chlorine organic pollutants basically reaches more than 80%, the extraction rate is basically not obviously increased along with the extension of time, and when the extraction time is extended to 50min, the recovery rate of part of the chlorine organic matters is reduced on the contrary. Considering the high efficiency of the actual operation, 30min was selected as the ultrasonic extraction time.
Due to the complex matrix of textile raw material solid waste, and the difficulty in obtaining accurate and stable results from a target object, the invention establishes an analysis method of UAV/SPE-GC/MS by optimizing the extraction conditions of ultrasonic-assisted extraction and solid-phase extraction on a sample and applying selective ion scanning of GC/MS. Technical support is provided for banning trade fraud behaviors such as 'adulterated toxic textiles' and 'smuggling textiles', and for national excellence in and out, regulation and control of textile raw material import, international negotiation, risk analysis and the like; meanwhile, in order to meet the large-pass work requirements of 'detected, detected quickly and detected accurately', the comprehensive utilization of the waste textile raw materials which accord with safety, sanitation and environmental protection is significant according to the development concept of domestic circular economy and the principle of 'harmlessness, reduction and recycling' of wastes.
Drawings
FIG. 1 is a total ion current chromatogram of a mixed standard working solution of the method for simultaneously determining chlorine organic pollutants in textile raw material solid waste.
In the figure: no. 1-17 are sequentially as follows: chlorobenzene, 1, 2-dichlorobenzene, 1, 3-dichlorobenzene, 1, 4-dichlorobenzene, 1,2, 3-trichlorobenzene, 2, 5-dichlorotoluene, 2, 4-dichlorotoluene, 2, 3-dichlorotoluene, 1,3, 5-trichlorobenzene, 2, 6-dichlorotoluene, 1,2, 4-trichlorobenzene, 1,2,4, 5-tetrachlorobenzene, 1,2,3, 5-tetrachlorobenzene, a, a, a-trichlorotoluene, a, a, a-2-tetrachlorotoluene, pentachlorobenzene, hexachlorobenzene.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments and the accompanying drawings.
Example 1
The embodiment is a method for determining chlorine organic pollutants in textile raw material solid waste, which comprises the steps of extracting and purifying the chlorine organic pollutants in a textile raw material solid waste sample to be detected by adopting an ultrasonic-assisted extraction/solid-phase extraction-gas chromatography-mass spectrometry method, and then determining the type and the content of the chlorine organic pollutants in the textile raw material solid waste sample to be detected by GC/MS detection. The method has the advantages of high sensitivity, good recovery rate and strong accuracy, and can meet the detection requirement of the chlorine organic pollutants in the textile raw material solid waste.
The method for determining the chlorine organic pollutants in the textile raw material solid waste comprises the steps of establishing a pretreatment condition and detecting a sample; the method comprises the steps of preparing a standard solution of chlorine organic pollutants, carrying out GC/MS test on the standard solution, determining the type and characteristic ions of a target substance, and further carrying out experimental test on a sample.
The establishing pretreatment condition specifically comprises the following steps:
s1-1: preparing a single-component standard stock solution: respectively and accurately weighing 0.01g (accurate to 0.0001g) of a proper amount of standard chlorine organic pollutant, placing the standard chlorine organic pollutant in a 25mL volumetric flask, dissolving and diluting the volumetric flask with dichloromethane to a constant volume, shaking the volumetric flask on a vortex machine to fully dissolve the standard chlorine organic pollutant, and placing the prepared standard stock solution with the concentration of 1000mg/L and single component in a refrigerator for storage at-4 ℃ for later use, wherein the validity period is 3 months. The standard substance of the chlorine organic pollutants comprises: chlorobenzene (99.9%), 1, 2-dichlorobenzene (99.8%), 1, 3-dichlorobenzene (99.7%), 1, 4-dichlorobenzene (99.9%), 1,2, 3-trichlorobenzene (99.9%), 2, 5-dichlorotoluene (99.9%), 2, 4-dichlorotoluene (99.1%), 2, 3-dichlorotoluene (99.4%), 1,3, 5-trichlorobenzene (99.9%), 2, 6-dichlorotoluene (99.6%), 1,2, 4-trichlorobenzene (99.6%), 1,2,4, 5-tetrachlorobenzene (99.4%), 1,2,3, 5-tetrachlorobenzene (99.0%), a, a, a-trichlorotoluene (99.6%), a, a, a-2-tetrachlorotoluene (99.5%), pentachlorobenzene (98.1%), hexachlorobenzene (99.9%), and the like.
S1-2: preparing a mixed standard working solution: respectively and accurately measuring 2mL of the single-component standard stock solution prepared in the step S1-1, placing the single-component standard stock solution into a 50mL volumetric flask, and using dichloromethane to fix the volume to prepare a mixed standard working solution with the concentration of 40 mg/L.
S1-3: ion detection: performing ion full scanning on the mixed standard working solution prepared in the step S1-2 through a chromatographic column temperature-raising program to obtain a total ion current chromatogram of the target substance, as shown in FIG. 1; the chromatographic column adopted by the ion detection is an active 19091N-133 type HP-INNOWAX chromatographic column, the specification of the chromatographic column is 30m multiplied by 250mm multiplied by 0.25 mu m, the temperature of a sample inlet is 250 ℃, the flow rate is 1.0mL/min, the sample is not split and is injected, the sample injection amount is 1uL, the carrier gas is nitrogen, and the purging flow of a spacer is 3 mL/min; the temperature raising procedure is as follows: the initial temperature is 45 deg.C, holding for 2min, heating to 230 deg.C at 20 deg.C/min, holding for 5min, heating to 250 deg.C at 15 deg.C/min, and holding for 2 min; the chromatogram is measured by using an EI source mass spectrum detector, and the ion source temperature is 250 ℃, and the quadrupole rod temperature is 150 ℃; the full scan solvent delay was 5 min.
S1-4: determining the type and characteristic ions: determining the peak-appearing time of each chlorine organic pollutant standard substance in the mixed standard stock solution according to the chromatogram obtained by ion scanning in the step S1-3, and determining the types and characteristic ions of the fragment ions according to the mass spectrogram, thereby establishing the pretreatment condition of the GC/MS-SIM method.
In this embodiment, the experimental testing of the sample specifically includes the following steps:
s2-1: ultrasonic extraction: cutting a textile solid waste sample to be detected into fragments with the size of 5mm multiplied by 5mm, uniformly mixing the fragments with a certain amount of standard mixed standard solution, and standing for 1 h; 1.0g (to the nearest 0.01g) of the mixed sample was placed in an ultrasonic cleaner, extracted with an ultrasonic extraction solvent in a water bath, passed through a 0.2 μm Teflon membrane filter head, and the extract was transferred to be purified.
S2-2: SPE purification: respectively activating a Florisil column with 10mL of n-hexane, ethyl acetate, acetone, dichloromethane and methanol, pouring the extract obtained by ultrasonic extraction in the step S2-1 into a solid phase extraction column, respectively eluting with 15mL of the 5 solvents or acetone alone, blowing and concentrating the elution liquid nitrogen, and metering the volume to 1m with dichloromethane for GC/MS machine detection.
S2-3: ion detection: and (4) scanning the eluent of the solid phase extraction in the step S2-2 by using the HP-INNOWAX chromatographic column temperature-rising program in the step S1-3 to obtain an ion current chromatogram of the target substance contained in the eluent.
S2-4: determining the target substance: and analyzing the ion current chromatogram in the step S2-3, and simultaneously determining the chlorine organic pollutants contained in the textile solid waste sample to be detected according to the standard working solution mixed in the step S1-2 and the types and characteristic ions determined by the total ion current chromatogram in the step S1-3.
Example 2
In this example, the method for determining chlorine-containing organic pollutants in textile raw material solid waste described in example 1 was subjected to correlation and detection limit verification, and simultaneously, sensitivity and accuracy verification were performed.
In this embodiment, the correlation and detection limit verification method includes: a series of mixed standard working nights of 17 chlorine organic pollutants are respectively configured, a working curve is drawn by taking the mass concentration as a horizontal coordinate and taking the peak area as a vertical coordinate, and the linear equation, the linear range and the correlation coefficient of the 17 chlorine organic pollutants are shown in Table 1.
TABLE 1.17 Linear correlation coefficient, Linear Range and detection Limit for chlorine-based organic contaminants
As can be seen from the table above, the linear correlation coefficient R of the detection method is more than or equal to 0.997, and the detection limit is 0.02-1.34 mug/g, which shows that the detection result is effective, the detection limit is wide, and the detection method is suitable for detecting the chlorine organic pollutants.
The verification of sensitivity and accuracy in this embodiment is: high, medium and low 3 levels of positive samples are prepared, and 7 parallel experiments are carried out under the screened optimal experimental conditions, and the measured recovery rate and relative deviation (RSD) results are shown in table 2.
TABLE 2.17 sample recoveries and relative deviations (RSD) of chlorine-based organic contaminants
As can be seen from the above table, the recovery rates of the 17 chlorine-containing organic pollutants are respectively as follows: 80% -107.6%; the RSD is 1.0% -6.5%, which shows that the method has better sensitivity and accuracy.
Because the matrix of the textile raw material solid waste is complex, and a target object is generally difficult to obtain an accurate and stable result, the UAV/SPE-GC/MS analysis method is established by optimizing the extraction conditions of an ultrasonic-assisted extraction method and a solid-phase extraction method for a sample and applying selective ion scanning of GC/MS, and the UAV/SPE-GC/MS analysis method is high in sensitivity, good in recovery rate and strong in accuracy, and meets the requirement for detecting chlorine organic pollutants in the textile raw material solid waste. Technical support is provided for banning trade fraud behaviors such as 'adulterated toxic textiles' and 'smuggling textiles', and for national excellence in and out, regulation and control of textile raw material import, international negotiation, risk analysis and the like; meanwhile, in order to meet the large-pass work requirements of 'detected, detected quickly and detected accurately', the comprehensive utilization of the waste textile raw materials which accord with safety, sanitation and environmental protection is significant according to the development concept of domestic circular economy and the principle of 'harmlessness, reduction and recycling' of wastes.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. Furthermore, it should be understood that although the present specification describes embodiments, these embodiments are not intended to be included solely, and such description is for clarity only, and those skilled in the art will be able to make the present specification as a whole, and the embodiments of the present invention may be appropriately combined to form other embodiments understood by those skilled in the art.
Claims (5)
1. A method for measuring chlorine organic pollutants in textile raw material solid waste is characterized by comprising the following steps: the method comprises the steps of adopting an ultrasonic-assisted extraction/solid-phase extraction-gas chromatography-mass spectrometry method to extract and purify chlorine organic pollutants in a textile raw material solid waste sample to be detected, and then determining the types and the contents of the chlorine organic pollutants in the textile raw material solid waste sample to be detected through GC/MS detection; the method comprises the following steps of preparing a standard solution of chlorine organic pollutants, performing GC/MS (gas chromatography/mass spectrometry) test on the standard solution, determining the type and characteristic ions of a target substance, and further performing experimental test on a sample, wherein the pre-established treatment conditions specifically comprise the following steps:
s1-1: preparing a single-component standard stock solution: accurately weighing a proper amount of chlorine organic pollutant standard substances respectively, dissolving and diluting the chlorine organic pollutant standard substances to a constant volume by using dichloromethane, oscillating the chlorine organic pollutant standard substances on a vortex machine to fully dissolve the chlorine organic pollutant standard substances, preparing a single-component standard stock solution with the concentration of 1000mg/L, and storing the single-component standard stock solution at the temperature of minus 4 ℃ for later use;
s1-2: preparing a mixed standard working solution: respectively and accurately measuring the single-component standard stock solutions prepared in the step S1-1, mixing the single-component standard stock solutions in a volumetric flask, using dichloromethane to fix the volume, and preparing the single-component standard stock solutions into mixed standard working solution with the concentration of 40 mg/L;
s1-3: ion detection: performing ion full scanning on the mixed standard working solution prepared in the step S1-2 through a chromatographic column temperature-raising program to obtain a total ion current chromatogram of a target substance;
s1-4: determining the type and characteristic ions: determining the peak-appearing time of each chlorine organic pollutant standard substance in the mixed standard stock solution according to the chromatogram obtained by ion scanning in the step S1-3, and determining the type and characteristic ions of fragment ions in the mass spectrogram, thereby establishing a pretreatment condition of a GC/MS-SIM method, wherein in the step S1-1, the chlorine organic pollutant standard substance comprises: chlorobenzene, 1, 2-dichlorobenzene, 1, 3-dichlorobenzene, 1, 4-dichlorobenzene, 1,2, 3-trichlorobenzene, 2, 5-dichlorotoluene, 2, 4-dichlorotoluene, 2, 3-dichlorotoluene, 1,3, 5-trichlorobenzene, 2, 6-dichlorotoluene, 1,2, 4-trichlorobenzene, 1,2,4, 5-tetrachlorobenzene, 1,2,3, 5-tetrachlorobenzene, a, a, a-trichlorotoluene, a, a, a-2-tetrachlorotoluene, pentachlorobenzene and hexachlorobenzene 17 kinds of chlorine organic pollutants, wherein in the step S1-3, the chromatographic column used for ion detection is an Aglient19091N-133 type HP-INWAX chromatographic column with the specification of 30m x 250mm x 0.25 μm, the injection inlet temperature is 250 ℃ and the flow rate is 1.0mL/min, sampling without shunting, wherein the sampling amount is 1uL, the carrier gas is nitrogen, and the purging flow of the isolation pad is 3 mL/min; the temperature-raising program is as follows: the initial temperature is 45 ℃, the temperature is kept for 2min, the temperature is raised to 230 ℃ at the speed of 20 ℃/min, the temperature is kept for 5min, the temperature is raised to 250 ℃ at the speed of 15 ℃/min, and the temperature is kept for 2 min; the chromatogram is measured by using an EI source mass spectrometer, and the ion source temperature is 250 ℃, and the quadrupole rod temperature is 150 ℃; the solvent delay for the full scan was 5 min.
2. The method for determining chlorine-based organic contaminants in textile raw material-based solid waste according to claim 1, wherein: the experimental test of the sample specifically comprises the following steps:
s2-1: ultrasonic extraction: cutting a textile solid waste sample to be detected into fragments, uniformly mixing the fragments with a certain amount of standard mixed standard solution, and standing for 1 h; placing the mixed sample in an ultrasonic cleaner, extracting by an ultrasonic extraction solvent in a water bath, filtering, and transferring the extract liquor to be purified;
s2-2: SPE purification: pouring the extract liquid obtained by ultrasonic extraction in the step S2-1 into a solid phase extraction column, eluting by using a solid phase extraction eluent, blowing and concentrating the elution liquid nitrogen, and fixing the volume to 1mL by using dichloromethane for detecting on a GC/MS machine;
s2-3: ion detection: scanning the eluent extracted from the solid phase in the step S2-2 by adopting an HP-INNOWAX chromatographic column temperature-rising program to obtain an ion current chromatogram of a target substance contained in the eluent;
s2-4: determining the target substance: and (4) analyzing the ion current chromatogram in the step S2-3, determining the types and characteristic ions according to the total ion current chromatogram of the mixed standard working solution, and simultaneously determining the chlorine organic pollutants contained in the textile solid waste sample to be detected.
3. The method for determining chlorine-based organic contaminants in textile raw material-based solid waste according to claim 2, wherein: in step S2-1, the cutting specification of the sample is 5mm multiplied by 5 mm; the solvent for ultrasonic extraction is n-hexane, acetone or dichloromethane; the ultrasonic extraction time is 10-50 min; the filtration is performed by a 0.2 mu m polytetrafluoroethylene membrane filter head.
4. The method for determining chlorine-based organic contaminants in textile raw material-based solid waste according to claim 3, wherein: the ultrasonic extraction solvent is dichloromethane; the ultrasonic extraction time is 30 min; the specification of the polytetrafluoroethylene membrane filter head which passes through the filtration is 0.2 mu m.
5. The method for determining chlorine-based organic contaminants in textile raw material-based solid waste according to claim 4, wherein: in step S2-2, the solid phase extraction column is a Florisil solid phase extraction column; the SPE purification method comprises the following steps: the Florisil solid phase extraction column was activated with 10mL of n-hexane, ethyl acetate, acetone, dichloromethane and methanol, respectively, and the test solution was poured into the solid phase column and eluted with acetone solution only.
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