CN105548430A - Method for detecting aniline in soil - Google Patents
Method for detecting aniline in soil Download PDFInfo
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- CN105548430A CN105548430A CN201510905883.5A CN201510905883A CN105548430A CN 105548430 A CN105548430 A CN 105548430A CN 201510905883 A CN201510905883 A CN 201510905883A CN 105548430 A CN105548430 A CN 105548430A
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- aniline
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- pedotheque
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for detecting aniline in soil. The method is characterized by comprising S01: preparation of a to-be-detected solution. In the S01, a proper amount of an air-dried soil sample is weighed and is put into a measuring flask; an acid solution 15-20 times as much as the soil sample is added; the measuring flask is subjected to ultrasonic treatment under an ice-bath condition and is taken out; a proper amount of an alkaline solution is added, and the volume of the solution is allowed to reach a constant volume at the scale; and after standing, a proper amount of supernatant is taken out, filtered, and put into a sample introduction bottle. According to the method, aniline in the soil sample is extracted through acid dissolution and alkaline reduction. The method is simple in operation and steps, free of organic solvents, and friendly to environment. Aniline can be completely extracted, and the detection result is accurate, real, and reliable. Gas chromatography is adopted for aniline detection, is high in sensitivity and accuracy and good in specificity, and is a scientific method for aniline detection.
Description
Technical field
The present invention relates to the detection method of aniline in a kind of soil, belong to method of environmental monitoring technical field.
Background technology
Aniline, as a kind of important Organic Chemicals, is widely used in the art production process such as rubber, printing and dyeing, pharmacy, plastics, delft.Be a kind of material of carcinogenicity, belong to high toxicity organic contaminant.Aniline can cause human body acute poisoning or slow poisoning, produces headache, dizzy, tired, decrease of memory, unsmooth breath, even the symptom such as death by suffocation, and long-term contact with aniline also can cause cancer.Various countries' environmental protection, hygiene department using aniline as one of important Testing index, China is also listed in the pollutant of priority monitoring already.Therefore, to its sensitive detect fast most important.
The method of current mensuration aniline mainly contains chemical analysis, there is detection means and fall behind in chemiluminometry, testing result poor accuracy, a series of compounds with aniline group just can luminous or colour developing, therefore this method specificity is poor, and be difficult to concrete content aniline accurately being detected, testing result needs to be verified further.
Summary of the invention
Technical matters to be solved by this invention is, provides a kind of specificity strong, can accurately detect the detection method of aniline in soil by qualitative, quantitative.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
In soil, a detection method for aniline, is characterized in that, comprises the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque in right amount in measuring bottle, add the acid solution being equivalent to pedotheque 15 ~ 20 times amount, ultrasonic rear taking-up under condition of ice bath, add appropriate bases solution again, be settled to scale, leave standstill after get supernatant filter in right amount after in sample injection bottle;
S02, the preparation of standard solution: compound concentration is 0.1,0.5,1,5, the aniline standard serial solution of 10mg/L, constant volume solution is ethanol, is filtered to sample injection bottle after shaking up;
S03, detects: successively aniline standard serial solution and need testing solution being injected GC, GC testing conditions is: the 7890A type gas chromatograph of Agilent; HP-INNOWAX capillary column (0.25 μm, 0.25mm*60m); Flame ionization ditector; Detector temperature 240 ~ 280 DEG C; Injector temperature 230 ~ 250 DEG C; Temperature programme, initial temperature 90 ~ 120 DEG C, 10 DEG C/min rises to 230 ~ 250 DEG C, keeps 10min; Input mode is split sampling, split ratio 20:1.
Described acid solution comprises one or more in hydrochloric acid, nitric acid, sulfuric acid; The concentration of described acid solution is 0.2 ~ 0.3mol/L.
Described aqueous slkali comprise in NaOH, potassium hydroxide one or both; The concentration of described aqueous slkali is 0.2 ~ 0.3mol/L.
The order number of described pedotheque is 120 ~ 200 orders.
Described pedotheque also comprises pre-treatment step, adopts grid to arrange method sampling, at least gets 16 points, the section of each point samples respectively to veneer of soil, underearth.
Described ultrasonic time is 2 ~ 5min.
The detection method of aniline in a kind of soil provided by the invention, the method adopting acid-soluble alkali to reduce extracts the aniline in pedotheque, and this method is easy and simple to handle, step is simple, and organic solvent-free is environmentally friendly, and this method aniline extracts completely, and testing result is accurate, true and reliable.The present invention uses vapor-phase chromatography to detect aniline, and this method detection sensitivity is high, and accuracy is high, and precision is high, and specificity is good, is a kind of detection method of aniline of science.
Embodiment
Below the present invention is further described.
Embodiment 1:
1# sample and 2# sample: to pick up near chemical plant soil near soil and pharmaceutical factory respectively.
In soil, a detection method for aniline, is characterized in that, comprises the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque 2g in 100ml measuring bottle, add the hydrochloric acid solution of 30ml0.2mol/L, ultrasonic rear taking-up under condition of ice bath, add the sodium hydroxide solution of 35ml0.2mol/L again, ethanol is settled to scale, leave standstill after get supernatant filter in right amount after in sample injection bottle;
S02, the preparation of standard solution: compound concentration is 0.1,0.5,1,5, the aniline standard serial solution of 10mg/L, constant volume solution is ethanol, is filtered to sample injection bottle after shaking up;
S03, detects: successively aniline standard serial solution and need testing solution being injected GC, GC testing conditions is: the 7890A type gas chromatograph of Agilent; HP-INNOWAX capillary column (0.25 μm, 0.25mm*60m); Flame ionization ditector; Detector temperature 240 DEG C; Injector temperature 230 DEG C; Temperature programme, initial temperature 90 DEG C, 10 DEG C/min rises to 230 DEG C, keeps 10min; Input mode is split sampling, split ratio 20:1.
The order number of described pedotheque is 120 orders.
Described pedotheque also comprises pre-treatment step, adopts grid to arrange method sampling, at least gets 16 points, the section of each point samples respectively to veneer of soil, underearth.
Described ultrasonic time is 2min.
Testing result:
Typical curve is Y=690.09X+4.9889(r=0.9999), illustrate that aniline is good in the scope internal linear relation of 0.1 ~ 10mg/L, after Precision Experiment, stability test, replica test and average recovery test, find that each experimental result of this detection method is all good, can be used to detect the aniline content in pedotheque, average recovery test findings well illustrates that the aniline in pedotheque of the present invention extracts completely, and testing result is true and reliable.
After testing, the aniline content near chemical plant near soil and pharmaceutical factory in soil is all greater than national standard, illustrates that these two local soil are not suitable for planting farming.
Embodiment 2:
In soil, a detection method for aniline, is characterized in that, comprises the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque 2g in 100ml measuring bottle, add the sulfuric acid solution of 40ml0.3mol/L, ultrasonic rear taking-up under condition of ice bath, add the potassium hydroxide solution of 30ml0.3mol/L again, ethanol is settled to scale, leave standstill after get supernatant filter in right amount after in sample injection bottle;
S02, the preparation of standard solution: compound concentration is 0.1,0.5,1,5, the aniline standard serial solution of 10mg/L, constant volume solution is ethanol, is filtered to sample injection bottle after shaking up;
S03, detects: successively aniline standard serial solution and need testing solution being injected GC, GC testing conditions is: the 7890A type gas chromatograph of Agilent; HP-INNOWAX capillary column (0.25 μm, 0.25mm*60m); Flame ionization ditector; Detector temperature 280 DEG C; Injector temperature 250 DEG C; Temperature programme, initial temperature 120 DEG C, 10 DEG C/min rises to 250 DEG C, keeps 10min; Input mode is split sampling, split ratio 20:1.
The order number of described pedotheque is 200 orders.
Described pedotheque also comprises pre-treatment step, adopts grid to arrange method sampling, at least gets 16 points, the section of each point samples respectively to veneer of soil, underearth.
Described ultrasonic time is 5min.
After testing, the aniline content near chemical plant near soil and pharmaceutical factory in soil is all greater than national standard, illustrates that these two local soil are not suitable for planting farming.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. the detection method of aniline in soil, is characterized in that, comprise the following steps:
S01, the preparation of need testing solution: accurately take air-dry after pedotheque in right amount in measuring bottle, add the acid solution being equivalent to pedotheque 15 ~ 20 times amount, ultrasonic rear taking-up under condition of ice bath, add appropriate bases solution again, be settled to scale, leave standstill after get supernatant filter in right amount after in sample injection bottle;
S02, the preparation of standard solution: compound concentration is 0.1,0.5,1,5, the aniline standard serial solution of 10mg/L, constant volume solution is ethanol, is filtered to sample injection bottle after shaking up;
S03, detects: successively aniline standard serial solution and need testing solution being injected GC, GC testing conditions is: the 7890A type gas chromatograph of Agilent; HP-INNOWAX capillary column (0.25 μm, 0.25mm*60m); Flame ionization ditector; Detector temperature 240 ~ 280 DEG C; Injector temperature 230 ~ 250 DEG C; Temperature programme, initial temperature 90 ~ 120 DEG C, 10 DEG C/min rises to 230 ~ 250 DEG C, keeps 10min; Input mode is split sampling, split ratio 20:1.
2. the detection method of aniline in a kind of soil according to claim 1, is characterized in that: described acid solution comprises one or more in hydrochloric acid, nitric acid, sulfuric acid; The concentration of described acid solution is 0.2 ~ 0.3mol/L.
3. the detection method of aniline in a kind of soil according to claim 1, is characterized in that: described aqueous slkali comprise in NaOH, potassium hydroxide one or both; The concentration of described aqueous slkali is 0.2 ~ 0.3mol/L.
4. the detection method of aniline in a kind of soil according to claim 1, is characterized in that: the order number of described pedotheque is 120 ~ 200 orders.
5. the detection method of aniline in a kind of soil according to claim 1, it is characterized in that: described pedotheque also comprises pre-treatment step, adopt grid to arrange method sampling, at least get 16 points, the section of each point samples respectively to veneer of soil, underearth.
6. the detection method of aniline in a kind of soil according to claim 1, is characterized in that: described ultrasonic time is 2 ~ 5min.
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| CN201510905883.5A CN105548430A (en) | 2015-12-10 | 2015-12-10 | Method for detecting aniline in soil |
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| CN201510905883.5A CN105548430A (en) | 2015-12-10 | 2015-12-10 | Method for detecting aniline in soil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106323687A (en) * | 2016-08-04 | 2017-01-11 | 福建中烟工业有限责任公司 | Method for extracting aromatic amine, detection method, kit and application |
| CN110441436A (en) * | 2019-09-03 | 2019-11-12 | 江苏环科检测有限公司 | The analysis method of aniline in a kind of measurement 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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| CN104155375A (en) * | 2014-07-22 | 2014-11-19 | 浙江大学 | Method for detecting phenylamine compounds in environmental water samples by using synchronous derivation ultrasonic emulsification micro-extraction gas chromatography |
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| CN104655779A (en) * | 2015-03-03 | 2015-05-27 | 浙江中一检测研究院股份有限公司 | Simple and convenient testing method for phenylamine in soil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106323687A (en) * | 2016-08-04 | 2017-01-11 | 福建中烟工业有限责任公司 | Method for extracting aromatic amine, detection method, kit and application |
| CN110441436A (en) * | 2019-09-03 | 2019-11-12 | 江苏环科检测有限公司 | The analysis method of aniline in a kind of measurement 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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Application publication date: 20160504 |