CN112710760A - Method for determining chlorine organic pollutants in textile solid waste through multi-method combination - Google Patents
Method for determining chlorine organic pollutants in textile solid waste through multi-method combination Download PDFInfo
- Publication number
- CN112710760A CN112710760A CN202011526187.0A CN202011526187A CN112710760A CN 112710760 A CN112710760 A CN 112710760A CN 202011526187 A CN202011526187 A CN 202011526187A CN 112710760 A CN112710760 A CN 112710760A
- Authority
- CN
- China
- Prior art keywords
- extraction
- organic pollutants
- solid waste
- chlorine
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for determining chlorine organic pollutants in textile solid waste by combining a multi-method combined method, which combines an accelerated solvent extraction method and a solid-phase extraction method, extracts, purifies and concentrates the chlorine organic pollutants in the textile solid waste, and qualitatively and quantitatively determines the chlorine organic pollutants by a gas-mass combined method. Including S1: standard solution preparation, S2: establishment of a gas chromatography-mass spectrometry method, S3: sample preparation, S4: ASE extraction, S5: SPE clean and S6: and (5) performing on-machine detection and the like. The ASE extraction organic solvent has the advantages of small using amount, rapidness, small matrix influence, high repeatability and high automation degree, and the SPE has high purification selectivity and high recovery rate and can reduce the influence of interference impurities. The method combines the methods of accelerating solvent, solid phase extraction, chromatographic column temperature rise program, quality and simplicity detection ion scanning and the like, and the established ASE/SPE-GC/MS method has high sensitivity and is suitable for monitoring organic pollutants such as chlorobenzene and chlorobenzene in complex textile solid waste.
Description
Technical Field
The invention relates to a method for determining chlorine organic pollutants in textile solid waste by multi-method combination.
Technical Field
Chlorobenzene and chlorotoluene organic pollutants (CCBs) as one of the priority control pollutants mainly include chlorobenzene, dichlorobenzene, trichlorobenzene, tetrachlorobenzene, pentachlorobenzene, hexachlorobenzene, chlorotoluene, dichlorotoluene, trichlorotoluene, tetrachlorotoluene, pentachlorotoluene and isomers thereof and other more than 20 kinds of homologues. The chlorine organic pollutants are important organic solvents and widely exist in complex textile solid waste, and a large number of researches show that CCBs can migrate in the environment, are enriched in organisms and cause damage to human mucosa and internal organs, so that the method has important significance for quickly, accurately and sensitively detecting whether the textiles contain the CCBs.
At present, a plurality of extraction methods are commonly used for detecting harmful substances in textile solid waste, and the extraction methods comprise ultrasonic-assisted extraction, microwave extraction, liquid-liquid extraction, headspace extraction and the like. However, the methods have the defects of large organic solvent consumption, low extraction efficiency, large influence of matrix, difficulty in fully extracting target components of chlorobenzene and chlorotoluene organic pollutants in complex textile solid waste, low recovery rate, easiness in impurity interference, great influence on later analysis results and incapability of accurately measuring the content of CCBs in the textile solid waste.
Therefore, the pretreatment method which is high in selectivity, high in recovery rate, free of impurity interference, small in organic solvent consumption, rapid, small in matrix influence, high in reproducibility and high in automation degree is established, and the method has very important significance for detecting organic pollutants such as chlorobenzene and chlorobenzene in textile solid waste.
Disclosure of Invention
Aiming at the existing problems, the invention provides a method for determining chlorine organic pollutants in textile solid waste by multi-method combination, which combines an accelerated solvent extraction method and a solid phase extraction method, is used for a pretreatment method for extracting, purifying and concentrating CCBs in the textile solid waste, and carries out qualitative and quantitative determination on 17 CCBs by a gas chromatography-mass spectrometry (GC/MS). The specific technical scheme is as follows:
a method for measuring chlorine organic pollutants in textile solid waste by multiple methods is characterized in that an accelerated solvent extraction method and a solid phase extraction method are combined, the chlorine organic pollutants in the textile solid waste are extracted, purified and concentrated, and the chlorine organic pollutants are qualitatively and quantitatively measured by a gas-mass combination method.
The method for the multi-process combined determination of the chlorine organic pollutants in the textile solid waste according to claim 1, comprising the following steps:
s1: preparing a standard solution: preparing a chlorine organic pollutant standard substance into a standard stock solution with the concentration of 500 mug/mL, then diluting the standard stock solution into a mixed standard solution with different concentrations again for later use, and storing the mixed standard solution in a refrigerator at-4 ℃ for later use;
s2: the gas chromatography-mass spectrometry method comprises the following steps: performing solid phase extraction on the mixed standard solution prepared in the step S1 through a chromatographic column temperature-raising program, and then performing ion scanning through a mass spectrum detector to obtain a total ion current chromatogram of the mixed standard solution;
s3: sample preparation: shearing a representative sample to be detected into fragments, and uniformly mixing for later use;
s4: ASE extraction: accurately weighing 1.0g of the mixed sample prepared in the step S1, adding 0.3 mu g/mL of standard working solution, placing the mixture into an accelerated solvent extraction stainless steel pool for extraction, and transferring the extract into a sealed glass container to be purified after the extraction is finished;
s5: SPE purification: pouring the extraction liquid extracted by ASE in the step S4 into a solid phase column, eluting, finally blowing and concentrating elution liquid nitrogen to 5 mu L, and fixing the volume to 1mL by using dichloromethane for detection;
s6: and (3) computer detection: and (4) detecting the eluent purified in the step S5 by the gas chromatography-mass spectrometry method established in the step S2 to obtain the type and content of the chlorine organic pollutants in the sample to be detected.
In the foregoing method for determining chlorine-containing organic pollutants in textile solid waste by multiple methods, in step S1, the standard chlorine-containing organic pollutants include 17 kinds of chlorine-containing organic matters with purity of 99% or more, which are respectively: 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%); the solvents used for preparing the standard stock solution and the mixed standard solution are dichloromethane; the concentration of the standard stock solution is 500 mug/mL; the concentration of the mixed standard solution is 0.01-2 mg/mL.
In the method for measuring chlorine organic pollutants in textile solid waste by multi-method combination, in step S2, the chromatographic column used for solid phase extraction is an active 19091N-133 type HP-inowax chromatographic column, the specification of which is 30m × 250mm, and the film thickness is 0.25 μm; the temperature of the solid phase extraction sample inlet is 250 ℃, the flow rate is 1.0mL/min, the split-flow sample introduction is not carried out, and the sample introduction amount is 1 mu L; the carrier gas is nitrogen with the purity of more than 99.999 percent; the temperature rising procedure of solid phase extraction 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 mass spectrum detector is an EI source, the temperature of an ion source is 250 ℃, the temperature of a quadrupole rod is 150 ℃, and the solvent delay is 5min during ion scanning.
In the method for measuring chlorine organic pollutants in textile solid waste by multi-process combination, in step S3, the representative samples are a healed yellow plain polyester waste fabric, a white polyester fabric, a white nylon fabric and a bamboo fiber fabric; the size of the cut pieces is 5mm × 5mm or less.
In the foregoing method for determining chlorine-containing organic pollutants in textile solid waste by using multiple methods, in step S4, the ASE extraction conditions are as follows: fixing the heating time for 5min, static extraction time for 5min, elution volume for 60%, and purging time for 30 s; the extraction solvent is a dichloromethane and acetone compound solvent; the extraction temperature is 80-120 ℃; the extraction pressure is 8-11 Mpa; the static cycle extraction times are 1-5. Preferably, the volume ratio of the extraction solvent dichloromethane to acetone is 1: 3; the extraction temperature is 110 ℃; the extraction pressure is 11 Mpa; the number of static cycle extractions was 3.
In step S5, the SPE purification uses a silica gel column or a florisil column, which is activated by 5mL of n-hexane, ethyl acetate, acetone, dichloromethane, methanol, chloroform, or acetonitrile before use, and is eluted by 15mL of n-hexane, ethyl acetate, acetone, dichloromethane, methanol, chloroform, or acetonitrile as an eluting solvent after the sample extract to be purified is poured. Preferably, the SPE purification adopts silica gel column, and the elution solvent is dichloromethane.
The invention has the beneficial effects that:
the invention combines an accelerated solvent extraction method and a solid phase extraction method, carries out extraction, purification and concentration treatment on chlorine organic pollutants in textile solid waste, and carries out qualitative and quantitative treatment on the chlorine organic pollutants by a gas-mass combination method. The added Accelerated Solvent Extraction (ASE) is different from the conventional extraction method for detecting harmful substances in textile solid waste, is a treatment method with small organic solvent dosage, rapidness, small matrix influence, high reproducibility and high automation degree, and is a treatment method for keeping the extraction temperature at 80-120 ℃ and the extraction pressure at 8-11 Mpa by pressurizing and heating the extraction solvent, so that the extraction solvent still keeps a liquid state at the temperature higher than the boiling point, the solubility of chlorine organic pollutants is higher than that of a gas state, the interaction force between a target substance and the matrix can be effectively reduced by increasing the temperature, and the target substance in the textile solid waste can be fully extracted by performing static cycle extraction for 1-5 times. Experiments show that when acetone is selected: dichloromethane (1:3, v/v) is used as an extracting agent, the temperature of 110 ℃ is used as ASE extraction temperature, 11MPa is used as ASE extraction pressure, and the best extraction effect is achieved by 3 times of static circulation extraction. The SPE purification is a solid phase extraction method which integrates extraction, separation and concentration, and has the advantages of high selectivity, high recovery rate, reduction of the influence of interfering impurities and the like. Experiments show that the extraction rate is highest when a silica gel column is used as a solid phase extraction column and dichloromethane is used as eluent.
The method combines the methods of accelerating solvent, solid phase extraction, chromatographic column temperature rise program, quality and simplicity detection ion scanning and the like, and the established ASE/SPE-GC/MS method has high sensitivity and is suitable for monitoring organic pollutants such as chlorobenzene and chlorobenzene in complex textile solid waste.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments.
Example 1
The method combines an accelerated solvent extraction method and a solid phase extraction method, extracts, purifies and concentrates the chlorine organic pollutants in the textile solid waste, and qualitatively and quantitatively determines the chlorine organic pollutants by a gas-mass combination method. The method specifically comprises the following steps:
s1: preparing a standard solution: the standard substance is sequentially prepared into a standard stock solution with the concentration of 500ug/mL by using dichloromethane, then the standard stock solution is diluted into mixed standard solutions with different concentrations of 0.01-2 mg/mL again for later use, and the mixed standard solutions are stored in a refrigerator at the temperature of-4 ℃ for 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%).
S2: the gas chromatography-mass spectrometry method comprises the following steps: performing solid phase extraction on the mixed standard solution prepared in the step S1 through a chromatographic column temperature-rising program, and then performing ion scanning through a mass spectrum detector to obtain a total ion current chromatogram of the mixed standard solution, wherein a chromatographic column used for the solid phase extraction is an active 19091N-133 type HP-INNOWAX chromatographic column, the specification of the chromatographic column is 30m × 250mm, and the film thickness is 0.25 μm; the temperature of the solid phase extraction sample inlet is 250 ℃, the flow rate is 1.0mL/min, the split-flow sample introduction is not carried out, and the sample introduction amount is 1 mu L; the carrier gas is nitrogen with the purity of more than 99.999 percent; the temperature rising procedure of solid phase extraction 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 mass spectrum detector is an EI source, the temperature of an ion source is 250 ℃, the temperature of a quadrupole rod is 150 ℃, and the solvent delay is 5min during ion scanning.
S3: sample preparation: the representative sample to be tested was cut into pieces and mixed well for use. The representative samples are heald yellow plain polyester waste fabric, white polyester fabric, white nylon fabric and bamboo fiber fabric; the size of the cut pieces is 5mm × 5mm or less.
S4: ASE extraction: accurately weighing 1.0g of the mixed sample prepared in the step S1, adding 0.3 mu g/mL of standard working solution, placing the mixture in an accelerated solvent extraction stainless steel pool for extraction, and transferring the extract into a sealed glass container to be purified after the extraction is finished. The ASE extraction conditions are as follows: fixing the heating time for 5min, static extraction time for 5min, elution volume for 60%, and purging time for 30 s; the used extraction solvent is a dichloromethane and acetone compound solvent, preferably, the volume ratio of dichloromethane and acetone compound of the extraction solvent is 1: 3; the extraction temperature is 80-120 ℃, and preferably 110 ℃; the extraction pressure is 8-11 MPa, preferably 11 MPa; the static cycle extraction frequency is 1-5, and preferably 3.
S5: SPE purification: pouring the extract extracted by ASE in the step S4 into a solid phase column, eluting, and finally blowing and concentrating the elution liquid nitrogen to 5 mu L, and fixing the volume to 1mL by using dichloromethane for detection. And the SPE purification adopts a silica gel column or a Florisil column, 5mL of n-hexane, ethyl acetate, acetone, dichloromethane, methanol, trichloromethane or acetonitrile is used for activation before the SPE purification is used, and after the sample extract liquid to be purified is poured, 15mL of n-hexane, ethyl acetate, acetone, dichloromethane, methanol, trichloromethane or acetonitrile is used as an elution solvent for elution. Preferably, the SPE purification adopts silica gel column, and the elution solvent is dichloromethane.
S6: and (3) computer detection: and (4) detecting the eluent purified in the step S5 by the gas chromatography-mass spectrometry method established in the step S2 to obtain the type and content of the chlorine organic pollutants in the sample to be detected.
Example 2
In this example, the method for determining the chlorine-containing organic pollutants in the textile solid waste by the multi-method combination described in example 1 was verified for sensitivity, accuracy, precision, reliability and practicability
The sensitivity verification method in this embodiment is as follows: a series of standard solutions of 0.01-2 mg/mL are prepared, according to the optimal experimental conditions described in example 1, the textile solid waste 1 is used as a blank sample, the concentration is used as an abscissa, the peak area is used as an ordinate, a standard curve is drawn, the detection limit is calculated by using the signal-to-noise ratio (S/N is 3), and the results of the obtained method, such as the correlation coefficient, the regression equation, the detection limit and the like, are shown in table 1.
TABLE 1 quantitative and qualitative ion, correlation coefficient, regression equation and detection limits for CCBs
The table shows that the correlation coefficients of the 17 CCBs are all larger than 0.997, and the detection limit is between 0.4-2.4 ug/mL, which indicates that the established ASE/SPE-GC/MS method is reasonable and effective and has higher sensitivity.
In this embodiment, the accuracy and precision verification method includes: 7 times of parallel standard addition experiments are carried out by adopting high, middle and low levels, under the screened optimal experiment conditions, the external standard method is used for quantification, and the measured standard addition recovery rate and relative deviation (RSD) results are shown in table 2.
TABLE 2 recovery, relative deviation of the process
The results show that the average recovery rates of 17 CCBs were: 80 to 97.8 percent, 81.7 to 103.5 percent and 82.4 to 99.8 percent; RSD is less than 5.5 percent and is far lower than the highest content requirement specified in China, so that the method is proved to have higher accuracy and precision and can meet the detection of 17 CCBs in the actual textile solid waste.
The reliability and practicability verification method in the embodiment comprises the following steps: selecting 2-4 textile solid wastes as sample matrix fabrics, adding 0.3mg/mL standard mixed solution into an experimental sample, and performing experiments according to the optimal experimental conditions to obtain that the recovery rates of CCBs are 85.3-101.4%, 88.5-90.4%, 80.5-105.4% and RSD are less than 8% respectively; the method is proved to be reliable.
The invention utilizes accelerated solvent extraction and solid phase extraction for purification and concentration, and establishes an analysis method for simultaneously determining 17 chlorobenzene organic pollutants by using ASE/SPE-GC/MS through quantitative and qualitative GC/MS methods. The result shows that the method has the advantages of high sensitivity and high accuracy, the measured recovery rate of the textile solid waste is up to more than 80%, the detection limit is 0.4-2.4 ug/mL, and the method is suitable for detecting organic pollutants such as chlorobenzene and chlorobenzene in the textile solid waste.
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 (10)
1. A method for measuring chlorine organic pollutants in textile solid waste by multiple methods is characterized in that: the method combines an accelerated solvent extraction method and a solid phase extraction method, carries out extraction, purification and concentration treatment on chlorine organic pollutants in textile solid waste, and carries out qualitative and quantitative treatment on the chlorine organic pollutants by a gas-mass combination method.
2. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 1, is characterized in that: the method comprises the following steps:
s1: preparing a standard solution: preparing a chlorine organic pollutant standard substance into a standard stock solution with the concentration of 500 mug/mL, then diluting the standard stock solution into a mixed standard solution with different concentrations again for later use, and storing the mixed standard solution in a refrigerator at-4 ℃ for later use;
s2: the gas chromatography-mass spectrometry method comprises the following steps: performing solid phase extraction on the mixed standard solution prepared in the step S1 through a chromatographic column temperature-raising program, and then performing ion scanning through a mass spectrum detector to obtain a total ion current chromatogram of the mixed standard solution;
s3: sample preparation: shearing a representative sample to be detected into fragments, and uniformly mixing for later use;
s4: ASE extraction: accurately weighing 1.0g of the mixed sample prepared in the step S1, adding 0.3 mu g/mL of standard working solution, placing the mixture into an accelerated solvent extraction stainless steel pool for extraction, and transferring the extract into a sealed glass container to be purified after the extraction is finished;
s5: SPE purification: pouring the extraction liquid extracted by ASE in the step S4 into a solid phase column, eluting, finally blowing and concentrating elution liquid nitrogen to 5 mu L, and fixing the volume to 1mL by using dichloromethane for detection;
s6: and (3) computer detection: and (4) detecting the eluent purified in the step S5 by the gas chromatography-mass spectrometry method established in the step S2 to obtain the type and content of the chlorine organic pollutants in the sample to be detected.
3. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 2, is characterized in that: in step S1, the standard substance of chlorine-containing organic pollutants includes: 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; the purity of 17 kinds of the Chinese medicinal composition is over 99 percent.
4. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 2, is characterized in that: in step S1, the solvents used for preparing the standard stock solution and the mixed standard solution are both dichloromethane; the concentration of the standard stock solution is 500 mug/mL; the concentration of the mixed standard solution is 0.01-2 mg/mL.
5. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 2, is characterized in that: in step S2, the column used for the solid phase extraction is an agent 19091N-133 type HP-INNOWAX column, the specification of which is 30m × 250mm, and the film thickness is 0.25 μm; the temperature of the solid phase extraction sample inlet is 250 ℃, the flow rate is 1.0mL/min, the split-flow sample introduction is not carried out, and the sample introduction amount is 1 mu L; the carrier gas is nitrogen with the purity of more than 99.999 percent; the temperature rising procedure of solid phase extraction 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 mass spectrum detector is an EI source, the temperature of an ion source is 250 ℃, the temperature of a quadrupole rod is 150 ℃, and the solvent delay is 5min during ion scanning.
6. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 2, is characterized in that: in step S3, the representative samples are a healed yellow plain polyester waste fabric, a white polyester fabric, a white nylon fabric and a bamboo fiber fabric; the size of the cut pieces is 5mm × 5mm or less.
7. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 2, is characterized in that: in step S4, the ASE extraction conditions are: fixing the heating time for 5min, static extraction time for 5min, elution volume for 60%, and purging time for 30 s; the extraction solvent is a dichloromethane and acetone compound solvent; the extraction temperature is 80-120 ℃; the extraction pressure is 8-11 Mpa; the static cycle extraction times are 1-5.
8. The method for determining the chlorine-type organic pollutants in textile solid waste by multi-method combination according to claim 7, which is characterized in that: the volume ratio of the extraction solvent dichloromethane to acetone is 1: 3; the extraction temperature is 110 ℃; the extraction pressure is 11 Mpa; the number of static cycle extractions was 3.
9. The multi-process combination method for determining chlorine-type organic pollutants in textile solid waste, according to claim 2, is characterized in that: in step S5, the SPE purification is performed using a silica gel column or florisil column, which is activated with 5mL of n-hexane, ethyl acetate, acetone, dichloromethane, methanol, chloroform, or acetonitrile before use, and after pouring the sample extract to be purified, the sample extract is eluted with 15mL of n-hexane, ethyl acetate, acetone, dichloromethane, methanol, chloroform, or acetonitrile as an eluting solvent.
10. The method for determining the chlorine-type organic pollutants in textile solid waste by multi-method combination according to claim 9, which is characterized in that: the SPE purification adopts a silica gel column, and the elution solvent is dichloromethane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011526187.0A CN112710760B (en) | 2020-12-22 | 2020-12-22 | Method for determining chlorine organic pollutants in textile solid waste through multi-method combination |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011526187.0A CN112710760B (en) | 2020-12-22 | 2020-12-22 | Method for determining chlorine organic pollutants in textile solid waste through multi-method combination |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112710760A true CN112710760A (en) | 2021-04-27 |
| CN112710760B CN112710760B (en) | 2022-11-25 |
Family
ID=75545036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011526187.0A Active CN112710760B (en) | 2020-12-22 | 2020-12-22 | Method for determining chlorine organic pollutants in textile solid waste through multi-method combination |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112710760B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001124748A (en) * | 1999-10-27 | 2001-05-11 | Mitsubishi Electric Corp | Method and apparatus for high-speed analysis of chlorobenzene |
| CN110749678A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Method for measuring organic volatile substances in soil by using gas chromatography-mass spectrometry-headspace |
| 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 |
-
2020
- 2020-12-22 CN CN202011526187.0A patent/CN112710760B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001124748A (en) * | 1999-10-27 | 2001-05-11 | Mitsubishi Electric Corp | Method and apparatus for high-speed analysis of chlorobenzene |
| CN110749678A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Method for measuring organic volatile substances in soil by using gas chromatography-mass spectrometry-headspace |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| V. LOPEZ-AVILA 等: "Evaluation of Fused-Silica Capillary Columns for GC/ECD Analysis of Chlorinated Hydrcbcarbons Listed in EPA Method 8120", 《JOURNAL OF HIGH RESOLUTION CHROMATOGRAPHY & CHROMATOGRAPHY COMMUNICATIONS》 * |
| 卫敏: "气质联用法测定纺织助剂中有机氯载体的含量", 《质量技术监督研究》 * |
| 施玉格 等: "加速溶剂萃取-气相色谱-质谱法测定土壤中半挥发性有机物的残留量", 《干旱环境监测》 * |
| 郎印海 等: "固相流体热萃取-GC/MS分析土壤中氯苯类有机污染物", 《分析试验室》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112710760B (en) | 2022-11-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | Headspace liquid-phase microextraction of trihalomethanes in drinking water and their gas chromatographic determination | |
| Xiao et al. | Analysis of PBDEs in soil, dust, spiked lake water, and human serum samples by hollow fiber-liquid phase microextraction combined with GC-ICP-MS | |
| Mei et al. | Simultaneous determination of bisphenols and alkylphenols in water by solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry | |
| Kawaguchi et al. | Determination of 4-nonylphenol and 4-tert.-octylphenol in water samples by stir bar sorptive extraction and thermal desorption–gas chromatography–mass spectrometry | |
| Devos et al. | A new validated analytical method for the determination of tributyltin in water samples at the quantification level set by the European Union | |
| Wu et al. | Determination of secondary and tertiary amines as N-nitrosamine precursors in drinking water system using ultra-fast liquid chromatography–tandem mass spectrometry | |
| Chen et al. | Cold on-column injection coupled with gas chromatography/mass spectrometry for determining halonitromethanes in drinking water | |
| CN112730662B (en) | Method for simultaneously determining two plasticizers, i.e. phthalate and adipate in textile solid waste | |
| Zhao et al. | Optimization of nonequilibrium liquid-phase microextraction for the determination of nitrobenzenes in aqueous samples by gas chromatography-electron capture detection | |
| CN112710760B (en) | Method for determining chlorine organic pollutants in textile solid waste through multi-method combination | |
| CN111220722B (en) | Method for simultaneously determining 8 p-hydroxybenzoate compounds in soil | |
| CN112526030B (en) | Analysis method of diallyl trisulfide in food industry wastewater | |
| Farahani et al. | Liquid‐phase microextraction by solidification of floating organic microdrop and GC‐MS detection of trihalomethanes in drinking water | |
| CN113109460B (en) | Method for analyzing high-boiling-point solvent residue in OLED material | |
| Chen et al. | Analyses of nitrobenzene, benzene and aniline in environmental water samples by headspace solid phase microextraction coupled with gas chromatography-mass spectrometry | |
| US9207220B1 (en) | Fully automated analytical method for determination of chloroethers in water and urine sample | |
| Yu et al. | Simultaneous determination of six earthy–musty smelling compounds in water by headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry | |
| Yang et al. | Enantioselective determination of trantinterol in rat plasma by ultra performance liquid chromatography–electrospray ionization mass spectrometry after derivatization | |
| Yu et al. | Trace analysis of phenolic compounds in water by in situ acetylation coupled with purge and trap-GC/MS | |
| CN106124672A (en) | The enrichment method of organic fluoride in a kind of water sample based on fluorine solid phase extraction techniques | |
| CN112710761B (en) | Method for determining chlorine organic pollutants in textile raw material solid waste | |
| LU501359B1 (en) | Method for analyzing difenoconazole and pyraclostrobin in litchi flowers by high performance liquid chromatography-tandem mass spectrometry | |
| CN114910588B (en) | Synchronous detection method for couchgrass, dicamba, penta-nitrophenol, fenpyroxim and penconazole in tea | |
| CN115184499B (en) | Synergistic detection method of organic chlorine pesticide, halogenated flame retardant and organic phosphate and application | |
| JP2005055205A (en) | Analytical method of polychlorinated biphenyls |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |