CN110441436A - The analysis method of aniline in a kind of measurement soil - Google Patents
The analysis method of aniline in a kind of measurement soil Download PDFInfo
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- CN110441436A CN110441436A CN201910826853.3A CN201910826853A CN110441436A CN 110441436 A CN110441436 A CN 110441436A CN 201910826853 A CN201910826853 A CN 201910826853A CN 110441436 A CN110441436 A CN 110441436A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
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- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- 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
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
It is disclosed by the invention to belong to measuring method technical field, the analysis method of aniline in specially a kind of measurement soil, the following steps are included: S1: sample acquisition: acquiring pedotheque in sampled point, impurity elimination, after freeze-drying, it is placed in grinding save set to be ground and save to be measured, grinding condition was 60 meshes, and storage temperature is -20 DEG C;S2: sample pre-treatments, this kind measures the analysis method of aniline in soil, the measuring method being concentrated using Gas chromatographyMass spectrometry combination Accelerate solvent extraction and rotary evaporation, pedotheque is concentrated by Accelerate solvent extraction and rotary evaporation, ion scan mode is selected with gas chromatography-mass spectrography, quantified by external standard method, stability is good, the rate of recovery is high, detection sensitivity is high, and for the rapid screening of aniline in soil, extraction time can be greatly shortened, the content of extract component is improved, and then improves the accuracy of detection.
Description
Technical field
The present invention relates to measuring method technical field, the analysis method of aniline in specially a kind of measurement soil.
Background technique
Aniline is one of most important intermediate in dyestuff work, can be used for Acid Ink Blue G, acidity in dye industry
Medium BS, acid light yellow, direct orange S, direct pink, indigo, disperse yellow brown, cationic pink fg;It is used in terms of organic pigment
In manufacture bronze red, bronze red g, pigment scarlet powder, the red, nigrosine of phenol cyanines etc..Dyestuff nigrosine is used in printing and dyeing industry;Aniline is
The important source material of rubber chemicals, for manufacture antioxidant A, antioxidant d, anti-aging agent RD and antioxidant 4010, captax,
808, D and CA etc.;Also it can be used as the raw material of medical sulfa drug, while being also the centre of production fragrance, plastics, varnish, film etc.
Body;And it can be used as the stabilizer in explosive, the anti-knock agent in gasoline and be used as solvent;It is other to be also used as manufacture to benzene two
Phenol, 2-phenylindone etc..
Aniline be produce pesticide important source material, by aniline can derive N- alkyl benzene amine, alkyl benzene amine, ortho-nitraniline,
Cyclohexylamine etc., can be used as fungicide sulfonat, Seedvax, insecticide Hostathion, pyridaphethione, quinalphos, herbicide alachlor,
The intermediate of hexazinone, imazaquin etc..
And had some limitations for aniline detection method in existing soil, sensitivity is inadequate, anti-interference ability
Difference, stability not can guarantee, it is difficult to meet the testing requirements of aniline in soil.
Summary of the invention
The purpose of the present invention is to provide a kind of analysis methods of aniline in measurement soil, to solve in above-mentioned background technique
Aniline detection method has some limitations in the existing soil proposed, and sensitivity is inadequate, poor anti jamming capability, stability
It not can guarantee, it is difficult to the problem of meeting the testing requirements of aniline in soil.
To achieve the above object, the invention provides the following technical scheme: a kind of analysis method for measuring aniline in soil, packet
Include following steps:
S1: sample acquisition: pedotheque is acquired in sampled point, impurity elimination after freeze-drying, is placed in grinding save set and carries out
It grinds and saves to be measured, grinding condition was 50~60 meshes, and storage temperature is -15 DEG C~-20 DEG C;
S2: sample pre-treatments: 20.0 ± 0.01 above-mentioned ground sediment samples are accurately weighed, with 10 ± 0.05g silicon
Diatomaceous earth mixing is fitted into 66mL abstraction pool, is extracted using silent winged your the ASE350 Accelerate solvent extraction system of generation of match, is used dichloro
Methane/acetone (50/50, V/V) circulation obtains extracting solution after extracting 1 time~2 times;Extracting solution rotary evaporation is concentrated into the left side 2mL
The right side is added about 5mL ethyl acetate/hexamethylene (50/50) and carries out solvent switch, is further concentrated to about 0.5mL~1mL, uses magnesium sulfate
Column purification is settled to 1.0mL with methylene chloride after purification, is transferred in the sample bottle of 1mL~2mL, to be measured;
S3: it preparing standard solution: a: prepares standard reserving solution (100mg/L): it is dense that aniline standard solution being configured to quality
Degree is the standard reserving solution of 100mg/L, is stored in spare under 2 DEG C~4 DEG C environment;B: using methylene chloride as solvent, will be above-mentioned
Stock solution (100mg/L) be made into after proportionally diluting mass concentration be respectively 0.00,1.00,2.00,3.00,4.00,
The standard solution of 5.00mg/L saves at 2 DEG C~4 DEG C;
S4: draw standard curve: with methylene chloride prepare mass concentration be respectively 0.00,1.00,2.00,3.00,4.00,
The standard solution of 5.00mg/L draws standard curve with mass concentration (x) of the peak area (y) to object;
S5: scan pattern analysis: gas chromatograph mass spectrograph combined instrument selects ion scan pattern analysis;
S6: after analyzing by step S5, the peak face of sample solution quantified by external standard method: is calculated according to the chromatogram of drafting
Product, and the concentration in sample solution is calculated by standard curve described in step S3, standard of the object in 1~5mg/L is molten
It is in good linear relationship within the scope of liquid METHOD FOR CONTINUOUS DETERMINATION, with signal-to-noise ratio S/N=3 computing equipment method detection limit, S/N=10 conduct
Instrumental method quantitative limit, while to 1.5mg/L, the standard solution of 4.0mg/L measures 4 times~6 times, calculates precision.
Preferably, the substance is aniline.
Preferably, in the S2 extraction conditions be 1200~2000psi of pressure, 80 DEG C~100 DEG C of temperature, keep 5min~
10min, 60% flush volume rinse 40s~60s.
Preferably, the gas chromatograph mass spectrograph selects ion scan pattern analysis.
Preferably, the GC conditions of the ion scan pattern analysis are as follows: injector temperature: 240 DEG C~280 DEG C,
It does not shunt;Sample volume: 1.0ul, column flow: 1.0ml/min constant current;Column temperature: 35 DEG C start to keep 2min;With 15 DEG C/min heating
To 150 DEG C, 5min is kept;250 DEG C~290 DEG C are warming up to 3 DEG C/min, keeps 2min.
Preferably, the Mass Spectrometry Conditions of the ion scan pattern analysis are as follows: electron bombardment ionization source (EI);Ion source temperature: 200
DEG C~230 DEG C;Ionizability: 70eV;Interface temperature: 280 DEG C;Level four bars temperature: 150 DEG C;Choice ion pattern is swept
It retouches, chooses corresponding parent ion peak, second mass analysis is carried out to its ion, obtains fragment ion information.
Preferably, temperature when being extracted in the step S2 using silent winged your the ASE350 Accelerate solvent extraction system of generation of match
It is 80 DEG C~100 DEG C.
Preferably, ethyl acetate/hexamethylene (50/50) carries out needing to cooperate stirring when solvent switch in the step S2.
Compared with prior art, the beneficial effects of the present invention are: this kind measures the analysis method of aniline in soil, gas is utilized
The measuring method of phase chromatograph-mass spectrometer coupling technology combination Accelerate solvent extraction and rotary evaporation concentration, pedotheque is by quick
Solvent extraction and rotary evaporation concentration select ion scan mode, quantified by external standard method, the present invention with gas chromatography-mass spectrography
Method detection limit it is low, stability is good, and the rate of recovery is high, and detection sensitivity is high, for the rapid screening of aniline in soil, Neng Gou great
Amplitude shortens extraction time, improves the content of extract component, and then improve the accuracy of detection, and detection sensitivity is high, resists dry
It disturbs that ability is strong, the testing goal of aniline in soil can be reached.
Detailed description of the invention
Fig. 1 is aniline standard colour chart schematic diagram of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution: a kind of analysis method measuring aniline in soil, comprising the following steps:
S1: sample acquisition: pedotheque is acquired in sampled point, impurity elimination after freeze-drying, is placed in grinding save set and carries out
It grinds and saves to be measured, grinding condition was 50~60 meshes, and storage temperature is -15 DEG C~-20 DEG C;
S2: sample pre-treatments: 20.0 ± 0.01 above-mentioned ground sediment samples are accurately weighed, with 10 ± 0.05g silicon
Diatomaceous earth mixing is fitted into 66mL abstraction pool, is extracted using silent winged your the ASE350 Accelerate solvent extraction system of generation of match, is used dichloro
Methane/acetone (50/50, V/V) circulation obtains extracting solution after extracting 1 time~2 times;Extracting solution rotary evaporation is concentrated into the left side 2mL
The right side is added about 5mL ethyl acetate/hexamethylene (50/50) and carries out solvent switch, is further concentrated to about 0.5mL~1mL, uses magnesium sulfate
Column purification is settled to 1.0mL with methylene chloride after purification, is transferred in the sample bottle of 1mL~2mL, to be measured;
S3: it preparing standard solution: a: prepares standard reserving solution (100mg/L): it is dense that aniline standard solution being configured to quality
Degree is the standard reserving solution of 100mg/L, is stored in spare under 2 DEG C~4 DEG C environment;B: using methylene chloride as solvent, will be above-mentioned
Stock solution (100mg/L) be made into after proportionally diluting mass concentration be respectively 0.00,1.00,2.00,3.00,4.00,
The standard solution of 5.00mg/L saves at 2 DEG C~4 DEG C;
S4: draw standard curve: with methylene chloride prepare mass concentration be respectively 0.00,1.00,2.00,3.00,4.00,
The standard solution of 5.00mg/L draws standard curve with mass concentration (x) of the peak area (y) to object;
S5: scan pattern analysis: gas chromatograph mass spectrograph combined instrument selects ion scan pattern analysis;
S6: after analyzing by step S5, the peak face of sample solution quantified by external standard method: is calculated according to the chromatogram of drafting
Product, and the concentration in sample solution is calculated by the standard curve of step S3, standard solution of the object in 1~5mg/L connects
It is in good linear relationship in continuous measurement range, with signal-to-noise ratio S/N=3 computing equipment method detection limit, S/N=10 is as instrument
Method quantitative limit, while to 1.5mg/L, the standard solution of 4.0mg/L measures 4 times~6 times, calculates precision.
Wherein, substance is aniline, and extraction conditions are 1200~2000psi of pressure in S2,80 DEG C~100 DEG C of temperature, protects
5min~10min is held, 60% flush volume rinses 40s~60s, and gas chromatograph mass spectrograph selects ion scan mode point
Analysis, the GC conditions of ion scan pattern analysis are as follows: injector temperature: 240 DEG C~280 DEG C, does not shunt;Sample volume:
1.0ul, column flow: 1.0ml/min constant current;Column temperature: 35 DEG C start to keep 2min;150 DEG C are warming up to 15 DEG C/min, is kept
5min;250 DEG C~290 DEG C are warming up to 3 DEG C/min, keeps 2min, the Mass Spectrometry Conditions of ion scan pattern analysis are as follows: electronics bangs
Hit source (EI);Ion source temperature: 200 DEG C~230 DEG C;Ionizability: 70eV;Interface temperature: 280 DEG C;Level four bars temperature:
150℃;Choice ion pattern is scanned, and chooses corresponding parent ion peak, is carried out second mass analysis to its ion, is obtained broken
Piece ion information, when being extracted using silent winged your the ASE350 Accelerate solvent extraction system of generation of match in step S2 temperature be 80 DEG C~
100 DEG C, ethyl acetate/hexamethylene (50/50) carries out needing to cooperate stirring when solvent switch in step S2.
Embodiment
The analysis method of aniline in a kind of measurement soil, comprising the following steps:
S1: sample acquisition: pedotheque is acquired in sampled point, impurity elimination after freeze-drying, is placed in grinding save set and carries out
It grinds and saves to be measured, grinding condition was 60 meshes, and storage temperature is -20 DEG C;
S2: sample pre-treatments: 20.0 ± 0.01 above-mentioned ground sediment samples are accurately weighed, with 10 ± 0.05g silicon
Diatomaceous earth mixing is fitted into 66mL abstraction pool, is extracted using silent winged your the ASE350 Accelerate solvent extraction system of generation of match, is used dichloro
Methane/acetone (50/50, V/V) circulation obtains extracting solution after extracting 2 times;Extracting solution rotary evaporation is concentrated into 2mL or so, is added
Enter about 5mL ethyl acetate/hexamethylene (50/50) and carry out solvent switch, be further concentrated to about 1mL, with magnesium sulfate column purification, after purification
It is settled to 1.0mL with methylene chloride, is transferred in the sample bottle of 2mL, it is to be measured;
S3: it preparing standard solution: a: prepares standard reserving solution (100mg/L): it is dense that aniline standard solution being configured to quality
Degree is the standard reserving solution of 100mg/L, is stored in spare under 4 DEG C of environment;B: use methylene chloride as solvent, by above-mentioned stock solution
It is respectively 0.00,1.00,2.00,3.00,4.00,5.00mg/L that (100mg/L), which is made into mass concentration after proportionally diluting,
Standard solution saves at 4 DEG C;
S4: draw standard curve: with methylene chloride prepare mass concentration be respectively 0.00,1.00,2.00,3.00,4.00,
The standard solution of 5.00mg/L draws standard curve with mass concentration (x) of the peak area (y) to object;
S5: scan pattern analysis: gas chromatograph mass spectrograph combined instrument selects ion scan pattern analysis;
S6: after analyzing by step S5, the peak face of sample solution quantified by external standard method: is calculated according to the chromatogram of drafting
Product, and the concentration in sample solution is calculated by the standard curve of step S3, standard solution of the object in 1~5mg/L connects
It is in good linear relationship in continuous measurement range, with signal-to-noise ratio S/N=3 computing equipment method detection limit, S/N=10 is as instrument
Method quantitative limit, while to 1.5mg/L, the standard solution of 4.0mg/L measures 6 times, calculates precision.
Wherein, substance is aniline, in S2 extraction conditions be pressure 2000psi, 100 DEG C of temperature, keep 10min, 60%
Flush volume, rinse 60s, gas chromatograph mass spectrograph select ion scan pattern analysis, the gas of ion scan pattern analysis
Phase chromatographic condition are as follows: injector temperature: it 280 DEG C, does not shunt;Sample volume: 1.0ul, column flow: 1.0ml/min constant current;Column temperature:
35 DEG C start to keep 2min;150 DEG C are warming up to 15 DEG C/min, keeps 5min;290 DEG C are warming up to 3 DEG C/min, is kept
2min, the Mass Spectrometry Conditions of ion scan pattern analysis are as follows: electron bombardment ionization source (EI);Ion source temperature: 230 DEG C;Ionizability:
70eV;Interface temperature: 280 DEG C;Level four bars temperature: 150 DEG C;Choice ion pattern is scanned, and chooses corresponding parent ion peak,
Second mass analysis is carried out to its ion, obtains fragment ion information, uses silent winged your ASE350 of generation of match instant fastly in step S2
Temperature is 100 DEG C when agent extracting system extracts, when ethyl acetate/hexamethylene (50/50) carries out solvent switch in step S2
It needs to cooperate stirring.
Table 1 is the calibration curve of aniline;
Table 2 is precision;
Table 3 is accuracy.
In summary, being concentrated using Gas chromatographyMass spectrometry combination Accelerate solvent extraction and rotary evaporation
Measuring method, pedotheque is concentrated by Accelerate solvent extraction and rotary evaporation, selects ion with gas chromatography-mass spectrography
Scan pattern, quantified by external standard method, method detection limit of the invention is low, and stability is good, and the rate of recovery is high, and detection sensitivity is high, is used for
The rapid screening of aniline in soil, can be greatly shortened extraction time, improve the content of extract component, and then improve detection
Accuracy, detection sensitivity is high, and strong antijamming capability can reach the testing goal of aniline in soil.
Although hereinbefore invention has been described by reference to embodiment, the scope of the present invention is not being departed from
In the case where, various improvement can be carried out to it and can replace component therein with equivalent.Especially, as long as being not present
Structural conflict, the various features in presently disclosed embodiment can be combined with each other use by any way, In
The description for not carrying out exhaustive to the case where these combinations in this specification is examined merely for the sake of omission length with what is economized on resources
Consider.Therefore, the invention is not limited to specific embodiments disclosed herein, but the institute including falling within the scope of the appended claims
There is technical solution.
Claims (8)
1. the analysis method of aniline in a kind of measurement soil, it is characterised in that: the following steps are included:
S1: sample acquisition: pedotheque is acquired in sampled point, impurity elimination after freeze-drying, is placed in grinding save set and is ground
And saving to be measured, grinding condition was 50~60 meshes, and storage temperature is -15 DEG C~-20 DEG C;
S2: sample pre-treatments: 20.0 ± 0.01 above-mentioned ground sediment samples are accurately weighed, with 10 ± 0.05g diatomite
Mixing is fitted into 66mL abstraction pool, is extracted using the silent winged generation that ASE350 Accelerate solvent extraction system of match, with methylene chloride/
Acetone (50/50, V/V) circulation obtains extracting solution after extracting 1 time~2 times;Extracting solution rotary evaporation is concentrated into 2mL or so, is added
Enter about 5mL ethyl acetate/hexamethylene (50/50) and carry out solvent switch, is further concentrated to about 0.5mL~1mL, it is net with magnesium sulfate column
Change, is settled to 1.0mL with methylene chloride after purification, is transferred in the sample bottle of 1mL~2mL, it is to be measured;
S3: preparing standard solution: a: prepare standard reserving solution (100mg/L): aniline standard solution, which is configured to mass concentration, is
The standard reserving solution of 100mg/L is stored in spare under 2 DEG C~4 DEG C environment;B: use methylene chloride as solvent, by above-mentioned deposit
Liquid (100mg/L) is made into mass concentration after proportionally diluting be respectively 0.00,1.00,2.00,3.00,4.00,5.00mg/L
Standard solution, saved at 2 DEG C~4 DEG C;
S4: draw standard curve: with methylene chloride prepare mass concentration be respectively 0.00,1.00,2.00,3.00,4.00,
The standard solution of 5.00mg/L draws standard curve with mass concentration (x) of the peak area (y) to object;
S5: scan pattern analysis: gas chromatograph mass spectrograph combined instrument selects ion scan pattern analysis;
S6: quantified by external standard method: after analyzing by step S5, the peak area of sample solution is calculated according to the chromatogram of drafting, and
The concentration in sample solution is calculated by standard curve described in step S3, standard solution of the object in 1~5mg/L is continuous
It is in good linear relationship in measurement range, with signal-to-noise ratio S/N=3 computing equipment method detection limit, S/N=10 is as instrument side
Standard measure limit, while to 1.5mg/L, the standard solution of 4.0mg/L measures 4 times~6 times, calculates precision.
2. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: the substance is
Aniline.
3. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: extracted in the S2
Condition is 1200~2000psi of pressure, 80 DEG C~100 DEG C of temperature, keeps 5min~10min, 60% flush volume is rinsed
40s~60s.
4. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: the gas-chromatography
Instrument mass spectrograph selects ion scan pattern analysis.
5. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: the ion scan
The GC conditions of pattern analysis are as follows: injector temperature: it 240 DEG C~280 DEG C, does not shunt;Sample volume: 1.0ul, column flow:
1.0ml/min constant current;Column temperature: 35 DEG C start to keep 2min;150 DEG C are warming up to 15 DEG C/min, keeps 5min;With 3 DEG C/min
250 DEG C~290 DEG C are warming up to, 2min is kept.
6. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: the ion scan
The Mass Spectrometry Conditions of pattern analysis are as follows: electron bombardment ionization source (EI);Ion source temperature: 200 DEG C~230 DEG C;Ionizability: 70eV;
Interface temperature: 280 DEG C;Level four bars temperature: 150 DEG C;Choice ion pattern is scanned, and corresponding parent ion peak is chosen, to it
Ion carries out second mass analysis, obtains fragment ion information.
7. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: in the step S2
Temperature is 80 DEG C~100 DEG C when being extracted using silent winged your the ASE350 Accelerate solvent extraction system of generation of match.
8. the analysis method of aniline in a kind of measurement soil according to claim 1, it is characterised in that: in the step S2
Ethyl acetate/hexamethylene (50/50) carries out needing to cooperate stirring when solvent switch.
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CN110907558A (en) * | 2019-12-12 | 2020-03-24 | 江苏尚美环保科技有限公司 | Method for detecting aniline in soil |
CN111257031A (en) * | 2020-02-24 | 2020-06-09 | 重庆中科检测技术服务有限公司 | Method for detecting aniline in soil |
CN111458441A (en) * | 2020-05-28 | 2020-07-28 | 河北省地质实验测试中心 | Method for detecting aniline in soil |
CN111474261A (en) * | 2020-04-24 | 2020-07-31 | 山东省济南生态环境监测中心 | Method for measuring aniline in soil and sediment |
CN113219093A (en) * | 2021-05-06 | 2021-08-06 | 河北百润环境检测技术有限公司 | Method for detecting pyridaphenthion, pyridaben, cypermethrin and lambda-cyhalothrin in soil or sediment |
CN113390979A (en) * | 2021-05-07 | 2021-09-14 | 江苏泰斯特专业检测有限公司 | Method for measuring aniline in soil and sediment |
CN113984910A (en) * | 2020-07-27 | 2022-01-28 | 苏州华能检测技术有限公司 | Detection and analysis method for determining aniline in soil |
CN114324660A (en) * | 2021-12-29 | 2022-04-12 | 广电计量检测(湖南)有限公司 | Method for detecting methomyl oxime in soil and/or sediment by gas chromatography-mass spectrometry |
CN114487220A (en) * | 2020-10-27 | 2022-05-13 | 天津市职业大学 | Method for measuring semi-volatile organic compounds in soil based on temperature programming sample introduction-gas chromatography-mass spectrometry |
CN115508459A (en) * | 2021-06-22 | 2022-12-23 | 无锡中证检测技术(集团)有限公司 | Method for detecting aniline pollutants in soil |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE202009007714U1 (en) * | 2009-05-27 | 2009-08-27 | Helmholtz-Zentrum Für Umweltforschung Gmbh - Ufz | Detection system for interfacing with membranes Interphase Probe (MIP) techniques based on ion mobility spectrometry |
CN105548430A (en) * | 2015-12-10 | 2016-05-04 | 苏州国环环境检测有限公司 | Method for detecting aniline in soil |
-
2019
- 2019-09-03 CN CN201910826853.3A patent/CN110441436A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE202009007714U1 (en) * | 2009-05-27 | 2009-08-27 | Helmholtz-Zentrum Für Umweltforschung Gmbh - Ufz | Detection system for interfacing with membranes Interphase Probe (MIP) techniques based on ion mobility spectrometry |
CN105548430A (en) * | 2015-12-10 | 2016-05-04 | 苏州国环环境检测有限公司 | Method for detecting aniline in soil |
Non-Patent Citations (3)
Title |
---|
环境保护部: "《中华人民共和国国家环境保护标准HJ 783-2016》", 1 February 2016 * |
环境保护部: "《中华人民共和国国家环境保护标准HJ 834-2017》", 18 July 2017 * |
陶云锋等: "ASE-GPC-GC/MS同时测定土壤中16种苯胺类物质", 《环境科学与技术》 * |
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CN110907558A (en) * | 2019-12-12 | 2020-03-24 | 江苏尚美环保科技有限公司 | Method for detecting aniline in soil |
CN111257031A (en) * | 2020-02-24 | 2020-06-09 | 重庆中科检测技术服务有限公司 | Method for detecting aniline in soil |
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CN111474261B (en) * | 2020-04-24 | 2023-02-24 | 山东省济南生态环境监测中心 | Method for measuring aniline in soil and sediment |
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CN113390979A (en) * | 2021-05-07 | 2021-09-14 | 江苏泰斯特专业检测有限公司 | Method for measuring aniline in soil and sediment |
CN115508459A (en) * | 2021-06-22 | 2022-12-23 | 无锡中证检测技术(集团)有限公司 | Method for detecting aniline pollutants in soil |
CN114324660A (en) * | 2021-12-29 | 2022-04-12 | 广电计量检测(湖南)有限公司 | Method for detecting methomyl oxime in soil and/or sediment by gas chromatography-mass spectrometry |
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