CN104142310B - A kind of method for quick of aniline - Google Patents
A kind of method for quick of aniline Download PDFInfo
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- CN104142310B CN104142310B CN201410346473.7A CN201410346473A CN104142310B CN 104142310 B CN104142310 B CN 104142310B CN 201410346473 A CN201410346473 A CN 201410346473A CN 104142310 B CN104142310 B CN 104142310B
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- aniline
- pyrans
- spiro
- color
- dipstick
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- PAYRUJLWNCNPSJ-UHFFFAOYSA-N aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000001514 detection method Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 14
- CYGKLLHTPPFPHH-UHFFFAOYSA-N aniline;hydrate Chemical compound O.NC1=CC=CC=C1 CYGKLLHTPPFPHH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012086 standard solution Substances 0.000 claims abstract 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 230000003252 repetitive Effects 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 7
- 231100000719 pollutant Toxicity 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000002371 ultraviolet--visible spectrum Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 4
- 150000001448 anilines Chemical class 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N propionic acid Chemical compound CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Carbodicyclohexylimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 231100000601 Intoxication Toxicity 0.000 description 1
- YFJAIURZMRJPDB-UHFFFAOYSA-N N,N-dimethylpiperidin-4-amine Chemical compound CN(C)C1CCNCC1 YFJAIURZMRJPDB-UHFFFAOYSA-N 0.000 description 1
- 206010034912 Phobia Diseases 0.000 description 1
- 208000005374 Poisoning Diseases 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 206010041247 Social fear Diseases 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 235000012970 cakes Nutrition 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000005039 chemical industry Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000566 intoxication Toxicity 0.000 description 1
- 230000035987 intoxication Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 201000001552 phobic disease Diseases 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention discloses the detection method of aniline pollutant in a kind of water body, belong to chemical sensor detection field of material technology.The method utilizes the color distortion produced because " selectivity " of spiro-pyrans uv-vis spectra absorbs in aniline-water solution to come fast qualitative, detection by quantitative aniline pollutant.This technology contents comprises: (1) changes, according to the color of the spiro-pyrans dipstick in the aniline water quality standard solution of series concentration, the color standard card that acquisition is relevant to concentration of aniline.(2) according to the color of spiro-pyrans dipstick in solution to be measured, contrast color standard card quickly judges the concentration of aniline.The preparation of this detection method material is simple, simple operation, and is not limited by large test equipment and professional and technical personnel, particularly suitable to the most quickly the detecting of aniline pollutant in environment.
Description
Technical field
The present invention relates to the method for quick of aniline pollutant in a kind of water body.The color distortion that this detection method absorbs based on " selectivity " of spiro-pyrans uv-vis spectra in aniline-water solution and produces carrys out fast qualitative detection by quantitative aniline, belongs to chemical sensor detection field of material technology.
Background technology
Aniline is simplest aromatic amine, is also a kind of chemical intermediate particularly important in pharmacy and the building-up process such as dyestuff, rubber.But, aniline has the strongest toxicity and carcinogenesis, therefore during production, accumulating and use, once occurs aniline to reveal and will result in serious environmental pollution, directly threaten the living environment of people, even causes serious social fear.On December 31st, 1, the safe drinking water of the aniline leakage accident serious threat turbid Zhanghe River downstream area that Shanxi Province Changzhi City Tian Ji Coal Chemical Industry company occurs, directly result in Handan in Hebei province and close Rail West water factory, Handan citizen lest flurried and rush to purchase pure water.Eliminate this type of society's fear and depend on the timely issue about polluted information, and in existing many aniline detection meanss, such as electrochemical process, chemical titration, spectrographic method, gas phase and liquid chromatograph etc., all rely on greatly large test instrument and professional test personnel, thus be difficult to the aniline pollution condition in very first time real-time on-site, rapidly and efficiently detection water body or soil.
Summary of the invention
It is an object of the invention to provide the method for quick of a kind of aniline, it utilizes " selectivity " of spiro-pyrans ultravioletvisible absorption in aniline solution, with spiro-pyrans dipstick for detection medium, uses color standard block-regulations quickly to detect the aniline in polluted-water.
The detection foundation of the present invention:
Being dissolved in different organic solvents by spiro-pyrans 3-(3 ', 3 '-dimethyl-6-nitro spiral shell [pyrans-2,2 '-indoline]-1 '-yl) propanoic acid, aniline is shown " selectivity " by the ultraviolet-visible absorption spectroscopy of corresponding spiro-pyrans.In addition to aniline, the spiro-pyrans main absworption peak in other organic solvent all falls and spiro-pyrans can be suppressed in the absorption of visible region visible absorbance district (400nm to 700nm shows color), i.e. aniline.In like manner, under different concentration of anilines, the color of spiro-pyrans dipstick there is also difference." selectivity " of this spiro-pyrans dipstick UV, visible light absorbs the aniline that can be used in qualitative and quantitative detection environment.
Therefore, firstly the need of preparing spiro-pyrans dipstick in the method for quick of the present invention, its step is as follows:
10g cellulosic filter paper bits are dipped in 300mL oxolane, serosity is fully blended into high speed agitator, it is subsequently adding 1.90g 3-(3 ', 3 '-dimethyl-6-nitro spiral shell [pyrans-2,2 '-indoline]-1 '-yl) propanoic acid, 0.1527g 4-dimethylamino piperidine；Said mixture stirring is cooled to 0 DEG C.Under nitrogen protection, 1.135g dicyclohexylcarbodiimide is dissolved in 25mL oxolane, is then slowly added dropwise in said mixture, after keeping about 0 DEG C stirring 2h, then continue stirring reaction 24h under room temperature and terminate.Filter, according to this with oxolane, ethanol, water washing, dry acquisition spiro-pyrans cellulose cake.Second step, is re-dispersed into above-mentioned filter cake in about 500mL deionized water, is broken into paper pulp, can obtain spiro-pyrans dipstick with conventional papermaking processes.
The detection method of the present invention comprises the following steps:
(1) color standard card is prepared
Compound concentration is 10-7The series standard aniline-water solution that mol/L to 1mol/L does not waits, spiro-pyrans dipstick is dipped in above-mentioned solution 3～5min, obtains the spiro-pyrans reagent paper color standard card under different concentration of aniline according to the color of spiro-pyrans dipstick under different concentration of anilines.
(2) detection of pollution water sample
Spiro-pyrans dipstick is soaked in aniline pollution water sample to be measured 3～5min；According to the color of spiro-pyrans dipstick, contrast above-mentioned color standard card and quickly estimate the concentration of aniline in aqueous solution, take multiple measurements and take assembly average.
It is an advantage of the invention that simple, simple operation prepared by material, detection mode is similar to pH reagent paper test solution pH value, do not limited by Large-scale professional test equipment and technical staff, be suitable for the concentration of aniline pollutant in real-time on-site, quickly and efficiently detection environment and report decision-making section in time.This is for eliminating the Psychological phobia of people, being avoided intoxication accident generation etc. to suffer from important meaning.
Accompanying drawing explanation
Fig. 1: spiro-pyrans ultraviolet-visible absorption spectroscopy in different organic solvents.
Fig. 2: aniline pollutant monitoring flow process.
Fig. 3: 10-7The spiro-pyrans dipstick color standard card obtained in the aniline-water solution of mol/L to 1mol/L series concentration.
Fig. 4: utilize the contrast of color standard block-regulations gained concentration of aniline test value and actual value.
Detailed description of the invention
Describe the present invention in detail below in conjunction with the accompanying drawings and by specific embodiment.
Embodiment 1-6:
Choosing the many groups of aniline-water solutions with variable concentrations as test sample, test according to following step respectively, the concentration of aniline measured value obtained is listed the most in detail:
(1) color standard card is prepared
Compound concentration is 10-7The series standard aniline-water solution that mol/L to 1mol/L does not waits, spiro-pyrans dipstick is dipped in above-mentioned solution 3～5min, obtains the spiro-pyrans reagent paper color standard card under different concentration of aniline according to the color of spiro-pyrans dipstick under different concentration of anilines.
(2) detection of pollution water sample
Spiro-pyrans dipstick is soaked in aniline pollution water sample to be measured 3～5min；According to the color of spiro-pyrans dipstick, contrast above-mentioned color standard card and quickly estimate the concentration of aniline in aqueous solution, take multiple measurements and take assembly average.
Reliability demonstration:
In each embodiment, equal repetitive measurement takes assembly average.By standard error analysis (referring to table 1), as shown in Figure of description 4, the method relative error in the aniline solution of higher concentration less (> 10-3mol/L).Owing to being affected resolution capability and the subjective judgment of color by human eye, under higher concentration of aniline, color becomes apparent from, thus relative error is less.After being concentrated according to a certain percentage by aniline-water solution to be measured, can further improve the precision of test.The method is similar to pH reagent paper, simple to operate, is not limited by Large-scale professional test equipment and technical staff, is extremely suitable for carrying out the aniline pollutant in environment the fast qualitative detection of real-time on-site, for concentration of aniline 10-7Detection by quantitative in the range of mol/L～1mol/L has important references equally and is worth.
The range estimation concentration value of table 1 color standard card aniline and actual value
Note: concentration unit mol/L；Av. it is meansigma methods；σ is standard deviation
Claims (2)
1. the method for quick of an aniline, it is characterized in that, it is with spiro-pyrans dipstick for detection medium, comprise the steps: the first step, the standard aniline-water solution of preparation series variable concentrations, spiro-pyrans dipstick is dipped in above-mentioned solution, changes the spiro-pyrans reagent paper color standard card obtained under different concentration of aniline according to the color of reagent paper；Second step, is dipped into spiro-pyrans dipstick in aniline pollution water sample to be measured, and soak time is identical with previous step, and according to the color of spiro-pyrans dipstick, contrast color standard card quickly detects the concentration of aniline in aqueous solution, and repetitive measurement takes assembly average.
The method for quick of aniline the most according to claim 1, it is characterised in that the concentration range of aniline water quality standard solution is 10-7Mol/L～1mol/L, uses front sonicated 5min；Soak time is 3～5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410346473.7A CN104142310B (en) | 2014-07-18 | A kind of method for quick of aniline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410346473.7A CN104142310B (en) | 2014-07-18 | A kind of method for quick of aniline |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104142310A CN104142310A (en) | 2014-11-12 |
| CN104142310B true CN104142310B (en) | 2017-01-04 |
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