CN111812229A - Analysis method for measuring 2-methylbenzothiazole in soil/sediment through gas chromatography-mass spectrometry - Google Patents
Analysis method for measuring 2-methylbenzothiazole in soil/sediment through gas chromatography-mass spectrometry Download PDFInfo
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Abstract
The invention discloses an analysis method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry. The method comprises the following steps: sample pretreatment, extracting solution treatment and standard curve preparation, then the sample is detected by a gas chromatography-mass spectrometer, and quantitative detection is carried out by adopting an external standard method to obtain a quantitative detection result. The invention establishes a quantitative analysis method of 2-methylbenzothiazole in soil/sediment by using a Soxhlet extraction-silica gel purification-gas chromatography mass spectrometry method for the first time, the detection method is simple and easy to operate, the detection result is accurate, the detection is limited in land, the method is suitable for analyzing samples in batch soil/sediment in actual analysis and detection, and the analysis result can be used for soil pollution degree evaluation.
Description
Technical Field
The invention relates to the technical field of detection and analysis, and particularly relates to an analysis method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry.
Background
Benzothiazole and derivatives thereof have strong molecular science and technology conversion rate, are correspondingly sensitive to external fields, can greatly shift the spectral response range to a long-wave region, are important functional compounds, and are widely applied to nonlinear optics, electroluminescence and light quality change materials and medicine. Are commonly added to various types of products as preservatives, refrigerants, bactericides, cancer agents, photosensitizers and rubber agents. 2-methylbenzothiazole is the most important raw material for benzothiazole derivatives, and therefore, it is widely produced and used in industrial production. For example, the 2-methylbenzothiazole catalyzed and oxidized by metalloporphyrin can be used for preparing benzothiazole-2-formic acid which is an important organic medical intermediate, can be widely applied to the fields of medicines, pesticides, medicines and optical materials, can also be used for synthesizing a dipeptide protease inhibitor, effectively inhibits the activity of severe acute respiratory syndrome virus (SARS-CoV 3CL), and can also be used for synthesizing medicaments for resisting cancers, diminishing inflammation and treating neurocardiovascular diseases or disorders. Meanwhile, the 2-methylbenzothiazole can be used as a raw material to synthesize (E) -2- (4-formylstyryl) benzothiazole, and the latter has good bacteriostatic action on streptomyces microflavus and beer yeast. For example, 2-methylbenzothiazole and 3-carboxymethyl rhodanine are used as raw materials, a novel cyanine spectrum sensitizing dye 3-carboxymethyl-5- [ 3-carboxymethyl-5- (3-ethyl-2-benzothiazoleethylidene) -4-oxothiazole ] -4-oxo-2-thiothiazole bistriacetamine salt with a bridged chain containing rhodanine nucleus can be synthesized, and the dye is used in a laser image film emulsion, has stable sensitizing performance, obvious effect and ideal aging resistance, particularly has little residual color after development processing of a film, and can be widely applied to raw materials for synthesizing various functional compounds.
Meanwhile, 2-methylbenzothiazole is a colorless oily liquid. The melting point is 14 ℃. Boiling point 238 deg.C, 150 deg.C and 151 deg.C (2.0 kPa). Relative density 1.173. Refractive index 1.6170. Flash point 102 ℃. Is soluble in ethanol and hydrochloric acid, is insoluble in water, has pyridine smell, has toxicity, and can cause skin anaphylaxis. Industrial and medical wastewater contain this contaminant due to its wide use, but there is no report on a method for detecting this substance. Particularly, for chemical enterprises taking 2-methylbenzothiazole as a raw material, the 2-methylbenzothiazole can enter plant soil in the storage and production processes, and the 2-methylbenzothiazole in the soil can be polluted. However, the compound is not involved in technical specifications such as technical guidelines for evaluating risks of contaminated sites (HJ-25.3-2014) issued by Ministry of environmental protection, and soil pollution risk control standards (trial) for soil environmental quality construction sites (GB 36600-2018). Thus, when investigating and evaluating contaminated land areas when land properties are changed or moved, the risk of contamination may be underestimated.
Although patent 201910912024.7 discloses a method for detecting substances such as sodium benzothiazole-2-sulfinate in wastewater, the detection target does not include 2-methylbenzothiazole, and the sample to be detected is waste liquid, not soil or sediment. Therefore, there is a need to develop a quantitative analysis method for 2-methylbenzothiazole in soil/sediments, which is rapid, convenient and easy to operate.
Disclosure of Invention
The invention aims to provide an analysis method for measuring 2-methylbenzothiazole in soil/sediment by using gas chromatography-mass spectrometry, aiming at the problem that the prior art has no reported defects about a detection method of 2-methylbenzothiazole in soil/sediment. The invention adopts a Soxhlet extraction-silica gel chromatographic column purification-gas chromatography mass spectrometry quantitative method to establish a pretreatment and quantitative analysis method which is simple and quick and is suitable for 2-methylbenzothiazole in soil/sediments and saves solvent, has simple detection process and accurate detection result, is suitable for analyzing and detecting 2-methylbenzothiazole in soil/sediments, can investigate and evaluate the pollution degree of soil and reduces the risk of soil pollution.
The above object of the present invention is achieved by the following scheme:
an analytical method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry, which comprises the following steps:
s1, sample pretreatment: removing foreign matters from a soil sample, air-drying and grinding the soil sample into powder, and then extracting the powder by a Soxhlet extraction method to obtain an extracting solution;
s2, treating an extracting solution: replacing the solvent of the additional extracting solution obtained in the step S1 with n-hexane, eluting the replaced sample through a silica gel column, wherein the eluent is n-hexane and dichloromethane, and collecting the eluent;
s3, making a standard curve, carrying out constant volume on the eluent in the step S2, detecting by a gas chromatography-mass spectrometer, and carrying out quantitative detection by adopting an external standard method, wherein the specific detection conditions are as follows: the chromatographic column is HP-5MS, and the temperature is raised in a programmed temperature raising mode, wherein the temperature range is 100-300 ℃; mass spectrometry was performed using a full scan mode.
Preferably, the specific chromatographic conditions are: sample inlet temperature: at 280 ℃, no flow splitting is carried out; column temperature: keeping at 100 deg.C for 0 min; raising the temperature to 300 ℃ at the speed of 20 ℃/min, and keeping the temperature for 0 min;
the mass spectrum conditions are as follows: ion source temperature: 230 ℃ and interface temperature: 290 ℃, quadrupole temperature: 150 ℃, scan mode: full scan mode.
Preferably, in step S1, the soxhlet extraction method uses dichloromethane and acetone as extraction solvents, and the heating temperature is 72 ℃.
Preferably, the volume ratio of the extraction solvents dichloromethane and acetone of the soxhlet extraction method is 1: 1.
Preferably, in the soxhlet extraction process, the soil sample is wrapped by a glass fiber filter membrane; in the extraction process, the heating reflux speed is 4-6 times/h, and the extraction time is 18 h.
Preferably, the glass fiber filter membrane has a diameter of 90mm and a pore diameter of 0.45 μm, and is baked in a muffle furnace at 400 ℃ for more than 4h before use, and is sealed and stored after cooling.
Preferably, during the Soxhlet extraction, the soil sample has a mass of 10g and the extract is mentioned as 100 mL.
More preferably, the soxhlet extraction process is: wrapping a soil sample by using a glass fiber filter membrane, putting the wrapped soil sample into a Soxhlet extraction reflux pipe, adding a mixed solution of dichloromethane and acetone in a volume ratio of 1:1 into a flat-bottomed flask, heating the mixture in a water bath at 72 ℃, controlling the reflux speed of a solvent to be 4-6 times/h, controlling the extraction time to be 18h, finishing extraction, and collecting an extracting solution.
Preferably, in step S2, the solvent replacement process is: concentrating the extractive solution at 40 deg.C, adding n-hexane solution, and concentrating; and the solvent replacement is carried out for 1-3 times.
Preferably, the volume of n-hexane added during the solvent replacement is 5 times of the volume of the concentrated extract.
More preferably, the process of solvent replacement is: concentrating the collected extracting solution under the conditions of low pressure and low temperature, wherein the temperature is lower than 40 ℃, and the vacuum degree is kept to be more than 260 Pa; when the concentration was about 2mL, 10mL of n-hexane was added to replace the solvent, and the concentration was continued to about 1.0 mL.
Preferably, in step S2, the silica gel column elution process is: before elution, anhydrous sodium sulfate was filled in the top of the silica gel column and rinsed with n-hexane, and then the sample after solvent exchange was loaded and eluted with n-hexane and dichloromethane.
Preferably, the volume ratio of the n-hexane and the dichloromethane of the mobile phase eluted by the silica gel column is 1: 1.
Preferably, the silica gel column is a commercially available silica SPE cartridge (500mg, 6mL/pcs, CNW) or a self-packed column with an inner diameter of 1.0cm packed with 3.0g silica (100-200 mesh).
Preferably, the filler in the silica gel column is 100-200 mesh silica gel, the silica gel column is ultrasonically cleaned in methanol for 3 times before use, then ultrasonically cleaned for 3 times by dichloromethane, naturally dried, dried in an oven at 180 ℃, cooled and then hermetically stored.
Preferably, the silica gel column elution process is: before elution, the silica gel column is rinsed by 10mL of n-hexane; then transferring the concentrated solution to a purification column, rinsing with 2mL of n-hexane for 3 times, adding 30mL of mixed solvent of n-hexane and dichloromethane (volume ratio of 1:1) to rinse the purification column, and collecting eluate
Preferably, after the eluate collected in step S2 is concentrated, the volume is determined by n-hexane, and then the detection in step S3 can be performed.
Preferably, the detection in step S3 is carried out using a 7890B-5977B gas chromatography mass spectrometer (Agilent, USA) with a HP-5MS column of 30 m.times.0.25. mu.m.times.0.25 mm.
Preferably, in step S3, the sample size of the gas chromatograph: 1.0 μ L, column flow: 1.0 mL/min.
Compared with the prior art, the invention has the following beneficial effects:
the invention establishes a quantitative analysis method of 2-methylbenzothiazole in soil/sediment by using a Soxhlet extraction-silica gel purification-gas chromatography mass spectrometry method for the first time, the detection method is simple and easy to operate, the detection result is accurate, the detection is limited in land, the method is suitable for analyzing samples in batch soil/sediment in actual analysis and detection, and the analysis result can be used for soil pollution degree evaluation.
Drawings
FIG. 1 is a graph showing the effect of different leachates on the recovery efficiency of 2-methylbenzothiazole in example 3.
FIG. 2 is the result of recovery of spiked samples for the white spiked and matrix spiked groups in example 4.
Detailed Description
The present invention is further described in detail below with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention. The test methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are, unless otherwise specified, commercially available reagents and materials.
Example 1
An analysis method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry comprises the following specific steps:
1. sample preparation
The collected soil or sediment sample is placed in an enamel or glass tray, and foreign matters such as branches, leaves, stones and the like are removed. And naturally drying and grinding, and weighing 10.0g of the dried sample to be tested.
Wherein the determination of the soil sample moisture is performed according to HJ613, and the determination of the sediment sample moisture content is performed according to GB 17378.5.
2. Preparation of Standard samples
Standard solution: 2-methylbenzothiazole (CAS number 120-75-2, 98% purity, 5g mass) was a pure liquid standard, commercially available as certified standard, J & K.
Weighing 0.1000g of standard solution into a 10mL volumetric flask, diluting with acetone to a constant volume to a scale, preparing 10000mg/L of standard stock solution, diluting the standard stock solution, and preparing a series of standard curve concentrations, wherein the concentrations of all points are 0.1, 0.5, 1, 2, 5 and 10mg/L respectively.
3. Sample processing
(1) Wrapping the weighed sample with a glass fiber filter membrane, putting the wrapped sample into a reflux pipe of a Soxhlet extractor, adding 100mL of a dichloromethane and acetone mixed solvent (volume ratio is 1:1) into a flat-bottomed flask, heating the mixture in a water bath (set temperature is 70 ℃), connecting a condensation pipe through a circulating condensation pump, controlling the reflux speed of the solvent, controlling the reflux speed to be 4-6 times per hour, extracting for 18 hours, and collecting an extracting solution.
The glass fiber filter membrane used in the above process has a diameter of 90mm and a pore diameter of 0.45 μm, and is baked in a muffle furnace at 400 deg.C for more than 4h before use, and sealed for storage after cooling.
(2) Concentrating the collected extractive solution with rotary evaporator, setting heating temperature below 40 deg.C, and maintaining vacuum degree at above 260 Pa. When the concentration was about 2mL, 10mL of n-hexane was added to replace the solvent, and the concentration was continued to about 1.0 mL.
(3) The concentrate was transferred to a purification column. The column was packed with 3g of silica gel and 0.5g of anhydrous sodium sulfate, and the column was rinsed with 10mL of n-hexane before transfer. Then transferring the concentrated solution to a purification column, rinsing the purification column with 2mL of n-hexane for 3 times, adding 30mL of a mixed solvent of n-hexane and dichloromethane (volume ratio is 1:1), rinsing the purification column, and collecting the rinsing liquid.
A commercially available silica SPE cartridge (500mg, 6mL/pcs, CNW) or self-packed chromatography column with an inner diameter of 1.0cm packed with 3.0g silica (100-200 mesh).
The silica gel filler required in the process is 100-200 meshes of silica gel, the silica gel is ultrasonically cleaned in methanol for 3 times before use, then ultrasonically cleaned for 3 times by using dichloromethane, and naturally dried and then placed in an oven for 180 timesOC, baking for 24 hours, cooling, sealing and storing.
(4) And concentrating the purified test solution again according to the nitrogen blowing concentration or rotary evaporation concentration step, metering the volume to 1.0mL by using normal hexane, transferring the test solution into a sample injection bottle, and testing to be tested.
4. Qualitative and quantitative detection
An analytical instrument: 7890B-5977B gas chromatography-mass spectrometer (Agilent, USA)
An extraction instrument: soxhlet extraction device
A chromatographic column: HP-5MS, 30 m.times.0.25. mu.m.times.0.25 mm
Chromatographic conditions are as follows:
sample inlet temperature: at 280 ℃, no flow splitting is carried out;
sample introduction amount: 1.0 μ L, column flow: 1.0 mL/min;
column temperature: keeping at 100 deg.C for 0 min; raising the temperature to 300 ℃ at the speed of 20 ℃/min, and keeping the temperature for 0min
Mass spectrum reference conditions:
ion source temperature: 230 deg.C
Interface temperature: 290 deg.C
Quadrupole temperature: 150 ℃ C
Scanning mode: full scan mode.
Quantitative method: and (4) an external standard method.
The method can be used for rapidly and accurately detecting the content of the 2-methylbenzothiazole in the soil and can be used for evaluating the soil pollution.
Example 2 investigation of soil sample pretreatment Process
In order to ensure the extraction effect of the 2-methylbenzothiazole in the soil sample, the influence of the extraction mode and the type of a solvent is researched, and the specific process is as follows:
in order to determine the extraction efficiency of 2-methylbenzothiazole in soil by different extraction modes and extraction solvents, 4 treatment schemes (table 1) are specially set, wherein the scheme 1 and the scheme 2 adopt a traditional Soxhlet extraction mode, namely heating in a water bath, and the extraction process is as follows: wrapping the weighed sample with a glass fiber filter membrane, putting the wrapped sample into a Soxhlet extraction reflux pipe, adding 100mL of an extraction solvent into a flat-bottomed flask, heating the flat-bottomed flask in a water bath (the set temperature is 72 ℃), connecting a condenser pipe through a circulating condensation pump, controlling the reflux speed of the solvent, controlling the reflux speed to be 4-6 times per hour, extracting for 18 hours, finishing extraction, and collecting an extracting solution. Scheme 1 adopts a mixed solvent of acetone and dichloromethane (volume ratio is 1:1) as an extraction solvent, and scheme 2 adopts acetone as an extraction solvent.
Scheme 3 and scheme 4 full-automatic soxhlet extraction mode, its extraction process is: wrapping the weighed sample with a glass fiber filter membrane, putting the wrapped sample into a reflux pipe of a Soxhlet extractor, adding 100mL of an extraction solvent into a flat-bottomed flask, heating the mixture in a water bath kettle (the set temperature is 70 ℃), connecting a condensation pipe through a circulating condensation pump, controlling the reflux speed of the solvent, controlling the reflux speed to be 4-6 times per hour, extracting for 18 hours, finishing extraction, and collecting an extracting solution.
TABLE 1 Effect of different treatment protocols on the extraction efficiency of 2-methylbenzothiazole in soil
| Scheme(s) | Extraction mode | Extraction solvent | Extraction efficiency (%) |
| 1 | Conventional extraction | Acetone + dichloromethane (1:1, volume ratio) | 92.0±9.8 |
| 2 | Conventional extraction | Acetone (II) | 102±15.0 |
| 3 | Full-automatic Soxhlet extraction | Acetone + dichloromethane (1:1, volume ratio) | 80±20.2 |
| 4 | Full-automatic Soxhlet extraction | Acetone (II) | 86.3±12 |
The results are shown in table 1, where the extraction efficiency of the conventional soxhlet extraction is higher than that of the fully automatic soxhlet extraction, so the conventional soxhlet extraction was selected in this study; in addition, when the extraction solvent is acetone, although the extraction efficiency is high, the relative standard deviation is large, dichloromethane is convenient to concentrate during concentration after extraction, and acetone is an easily toxic chemical, so after comprehensive consideration, a mixed solvent (1:1) of acetone and dichloromethane is selected as an extraction liquid, and the traditional Soxhlet extraction is adopted to extract the 2-methylbenzothiazole in the soil.
Example 3
In order to optimize the experimental conditions of the purification process, on the premise of ensuring the best recovery efficiency, the method is energy-saving and environment-friendly, reduces the usage amount of toxic reagents, and totally sets 3 different leacheate elution chromatographic column experimental treatments, and the specific scheme is as follows: transferring a standard solution containing 1000ppb in 1mL of n-hexane to a 3.0g silica gel chromatographic column, eluting the chromatographic column by respectively using 30mL of a mixed solvent of n-hexane and dichloromethane (volume ratio is 1:1), 30mL of dichloromethane, 30mL of a mixed solvent of dichloromethane and acetone (volume ratio is 1:1), collecting eluent, concentrating to constant volume, and measuring by a computer, wherein each treatment is carried out for 3 times in parallel.
The results are shown in fig. 1, wherein the recovery rate of the target compound is (95.1 ± 3.2)%, the recovery rate obtained by eluting the chromatographic column with the mixed solvent of n-hexane and dichloromethane (volume ratio 1:1) is (89.6 ± 12)%, and the recovery rate of the target compound obtained by eluting the chromatographic column with the mixed solvent of dichloromethane and acetone (volume ratio 1:1) is (97.2 ± 6.6)%, so that it can be seen that the recovery rate obtained by using dichloromethane alone as the eluting solution is the lowest, the recovery rate obtained with the mixed solvent of dichloromethane and acetone (volume ratio 1:1) is the highest, but the ideal recovery effect can also be obtained with the mixed solvent of n-hexane and dichloromethane (volume ratio 1: 1). As acetone is an easily toxic chemical and is expensive, a mixed solvent of normal hexane and dichloromethane (the volume ratio is 1:1) is selected as the eluent at the later stage of the experiment.
Example 4
1. The method is used for researching the accuracy and comprises the following specific processes:
quartz sand is taken to respectively carry out a blank experiment and a blank marking experiment, a soil sample of a certain farmland in Bozhou city is selected to carry out an actual sample, the soil sample is simultaneously used as a matrix marking, and the blank marking and the matrix marking are both 1000 ppb.
Pretreatment was performed according to the best protocol in examples 2 and 3, and all experiments were performed in 3 replicates. Wherein 2-methylbenzothiazole was not detected in 3 blank experiments and 3 matrix blank samples. The recovery rate of the three blank standard additions was (93.7 + -9.0)%, and the recovery rate of the three substrate standard additions was (91.8 + -8.9)%, as shown in FIG. 2. Therefore, both the extraction efficiency and the recovery efficiency can reach the analysis and test standard, and better recovery efficiency can be obtained on the premise of the influence of the soil matrix. The analysis results of 3 agricultural actual soil samples show that no 2-methylbenzothiazole is detected.
2. Detection limit of method
Make and detect 7 LowThe Standard Deviation (SD) of the measurement results of 7 replicates was calculated for the concentration sample (0.1 μ g/mL), the detection limit of the sample solution was calculated (D.L-3.143 SD), and the mass m of the sample and the volume V were determined from the basis of the sample mass m and the volume V1Conversion method detection limit (MDL D.L V)1/m)。
TABLE 17 detection results of low concentration samples, standard deviation, detection limits of sample solutions and detection limits of method
| Serial number | Detecting the concentration | Unit of |
| 1 | 0.062 | μg/mL |
| 2 | 0.067 | μg/mL |
| 3 | 0.064 | μg/mL |
| 4 | 0.065 | μg/mL |
| 5 | 0.062 | μg/mL |
| 6 | 0.064 | μg/mL |
| 7 | 0.065 | μg/mL |
| Standard Deviation (SD) | 0.002 | μg/mL |
| Sample solution detection Limit (D.L) | 0.005 | μg/mL |
| Method Detection Limit (MDL) | 0.525 | μg/kg |
Taking 10g of sample, concentrating to 1mL, and calculating the lowest detection limit as follows: 0.525. mu.g/kg.
It should be finally noted that the above examples are only intended to illustrate the technical solutions of the present invention, and not to limit the scope of the present invention, and that other variations and modifications based on the above description and thought may be made by those skilled in the art, and that all embodiments need not be exhaustive. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. An analysis method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry is characterized by comprising the following steps:
s1, sample pretreatment: removing foreign matters from a soil sample, air-drying and grinding the soil sample into powder, and then extracting the powder by a Soxhlet extraction method to obtain an extracting solution;
s2, treating an extracting solution: replacing the solvent of the additional extracting solution obtained in the step S1 with n-hexane, eluting the replaced sample through a silica gel column, wherein the eluent is n-hexane and dichloromethane, and collecting the eluent;
s3, making a standard curve, carrying out constant volume on the eluent in the step S2, detecting by a gas chromatography-mass spectrometer, and carrying out quantitative detection by adopting an external standard method, wherein the specific detection conditions are as follows: the chromatographic column is HP-5MS, and the temperature is raised in a programmed temperature raising mode, wherein the temperature range is 100-300 ℃; mass spectrometry was performed using a full scan mode.
2. The analysis method for the gas chromatography-mass spectrometry to determine the 2-methylbenzothiazole in the soil/sediment according to claim 1, wherein the specific chromatographic conditions are as follows: sample inlet temperature: at 280 ℃, no flow splitting is carried out; column temperature: keeping at 100 deg.C for 0 min; raising the temperature to 300 ℃ at the speed of 20 ℃/min, and keeping the temperature for 0 min;
the mass spectrum conditions are as follows: ion source temperature: 230 ℃ and interface temperature: 290 ℃, quadrupole temperature: 150 ℃, scan mode: full scan mode.
3. The analytical method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry as claimed in claim 2, wherein in step S1, the solvent for extraction used in the soxhlet extraction method is dichloromethane and acetone in a volume ratio of 1:1, and the heating temperature is 72 ℃.
4. The analytical method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry as claimed in claim 1, wherein in the process of the soxhlet extraction method, the soil sample is wrapped by a glass fiber filter membrane; in the extraction process, the heating reflux speed is 4-6 times/h, and the extraction time is 18 h.
5. The analytical method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry as claimed in claim 1, wherein during the soxhlet extraction process, the mass of a soil sample is 10g, and the volume of an extraction solvent is 100 mL.
6. The analytical method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry as claimed in claim 1, wherein in the step S2, the process of solvent replacement is as follows: concentrating the extractive solution at 40 deg.C, adding n-hexane, and concentrating; and the solvent replacement is carried out for 1-3 times.
7. The analytical method for 2-methylbenzothiazole measurement of soil/sediment by gas chromatography-mass spectrometry as set forth in claim 6, wherein the volume of n-hexane added during the solvent replacement is 5 times the volume of the extract after concentration.
8. The analytical method for measuring 2-methylbenzothiazole in soil/sediment by gas chromatography-mass spectrometry as claimed in claim 1, wherein in the step S2, the elution process of the silica gel column is as follows: before elution, anhydrous sodium sulfate was filled in the top of the silica gel column and rinsed with n-hexane, and then the sample after solvent exchange was loaded and eluted with n-hexane and dichloromethane.
9. The analytical method for the gas chromatography-mass spectrometry detection of 2-methylbenzothiazole in soil/sediment according to claim 8, wherein the volume ratio of mobile phase n-hexane and dichloromethane eluted by the silica gel column is 1: 1.
10. The analysis method for determining 2-methylbenzothiazole in soil/sediment through gas chromatography-mass spectrometry as claimed in claim 8, wherein the filler in the silica gel column is 100-200 mesh silica gel, the silica gel column is ultrasonically cleaned in methanol for 3 times before use, then ultrasonically cleaned for 3 times by using dichloromethane, naturally dried in the air, dried in an oven at 180 ℃, cooled, and then hermetically stored.
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| CN112326841A (en) * | 2020-11-26 | 2021-02-05 | 安徽工和环境监测有限责任公司 | Detection and analysis method of halogenated carbazole in water body sediment |
| CN113495108A (en) * | 2021-07-09 | 2021-10-12 | 生态环境部华南环境科学研究所 | Method for simultaneously detecting 63 persistent organic pollutants in soil |
| CN115078577A (en) * | 2022-06-14 | 2022-09-20 | 国网河北省电力有限公司电力科学研究院 | Method for detecting petroleum hydrocarbon in soil |
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