CN104931436A - Rapid detection agent for determination of water quality aniline concentration - Google Patents
Rapid detection agent for determination of water quality aniline concentration Download PDFInfo
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- CN104931436A CN104931436A CN201410107412.5A CN201410107412A CN104931436A CN 104931436 A CN104931436 A CN 104931436A CN 201410107412 A CN201410107412 A CN 201410107412A CN 104931436 A CN104931436 A CN 104931436A
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Abstract
The invention relates to a preparation and use method of a rapid detection agent for determination of water quality aniline concentration, the a rapid detection agent comprises two kinds of powder, and is prepared by mainly mixing sodium nitrite, N-(1-naphthyl) ethylenediamine hydrochloride, ammonium sulfamate, amino sulfonic acid and the like, the two kinds of powder are successively added into a to-be-tested sample, and a spectrophotometer or a colorimeter is used for direct measurement of a chromophoric solution. The rapid aniline detection agent is easy to store, easy to carry, stable in performance, accurate and reliable in result, and simple in operation, can be used by non-professional personnel, and is suitable for on-site rapid detection of aniline in water surface water, industrial waste water and other water bodies.
Description
Technical field
The present invention relates to a kind of preparation and application measuring the quick detection agent of water quality concentration of aniline, belong to environmental monitoring technology field.
Background technology
Along with the fast development of industrial technology, Sudden Pollution Accident constantly increases, and threatens human health, destroys ecologic environment, seriously governs the ecologic equilibrium and society, expanding economy.Take precautions against abrupt polluting accident problem demanding prompt solution a lot, top priority sets up monitoring method for emergency, once contamination accident occurs, can drop into monitoring rapidly, contamination data is accurately provided, for antipollution diffusion and take counter-measure to provide scientific basis within the shortest time.Therefore, extremely strong for Time and place characteristic, the significant Sudden Pollution Accident of random variation, Site Detection obtain in time and the accurate perfect answer of answer comparatively accurately comes too late than one test in laboratory is valuable many.In-situ check and test method normally detects in real time in workplace, namely records in sample whether there is test substance and concentration thereof at short notice.It is few that method for Site Detection needs sampling quantity, and possess higher accuracy and sensitivity, the feature such as the instrument fast, to use easy and simple to handle is easy to carry.In-situ check and test method comparatively ripe at present has test paper method, detects tube method, miniature LHD units, Bioexperiment method, portable instrument method etc.
Measurement of Aniline many employings naphthodiamide photometry, amino benzenes compounds is (pH1.5 ~ 2.0) and nitrite diazotising in acid condition, again with N-(1-naphthyl) ethylenediamine-hydrochloride coupling, generate aubergine dyestuff, carry out spectrophotometry (Yang Xiaofen, Zhao Meiping, Li Yuanzong etc. the spectrophotometry of amino benzenes compounds in water. analytical chemistry, 2002,30 (5): 540-543).Zhang Lijun etc. have studied the electrochemical method measuring aniline, the electrochemical oxidation product of aniline can be enriched on the pretreated glass-carbon electrode of electrochemical activation, in dilution heat of sulfuric acid, enriched substance is in+0.4 ~+0.5V(vs.SCE) in produce the good redox peak of a pair peak shape, this redox peak is utilized to establish the method (Zhang Lijun of voltammetric determination aniline, Zhang Zhanen. electrochemical activation pre-service glass-carbon electrode voltammetric determination aniline. physical and chemical inspection-chemical fascicle, 2008,44 (5): 460-463).Under optimum test condition, the range of linearity of method is 1 × 10
-7-1 × 10
-5mol/ L is+1.2V(vs.SCE when enrichment time is 5 min and accumulating potential) time, the detection limit of method reaches 5 × 10
-8mol/ L.Huang Jin etc. establish a kind of new method utilizing flow injection spec-trophotometry directly to measure trace aniline in water sample, and (Huang enters, Zhang Xinshen, Yuan Dong etc. flow Injection Spectrophotometry for Determination determines the aniline in water sample. spectroscopy and spectral analysis, 2008,28 (2): 415-417), the method in strong acid media, diazo-reaction occurs based on aniline and nitrite, diazo-reaction product in the basic conditions with methyl naphthol generation oxidation-coupled reaction, and quantitatively detect in 495 nm places, the mensuration of aniline in leather waste water, the recovery is 98.0 ~ 103.0%.Zhang Aimei etc. establish Inhibitory Kinetic synchronous fluorimetry measure aniline method (Zhang Aimei, Jia Liping. Inhibitory Kinetic-Synchronous Fluorimetric Determination of Trace Aniline. spectroscopy and spectral analysis, 2004,24 (6): 723-725).Under Dilute Sulphuric Acid Medium and CTMAB exist, the reaction of trace aniline to Meat with Potassium Bromate Oxygenation for Fluorescein has sensitive resistance inhibitor action, the oxidation product of fluorescein has hyperfluorescenceZeng Yongminggaoyingguang, but its excitation spectrum and emission spectrum overlapping, Synchronous fluorimetric method is adopted to reduce bands of a spectrum overlap, the range of linearity of method is 0 ~ 10ug/L, detects and is limited to 0.3ug/L.
Although above-mentioned traditional experiment room method can carry out accurate quantitative analysis to pollutant, and there is higher accuracy and sensitivity, but the instrument and equipment need to gather a large amount of sample, being equipped with professional and costliness, complicated operation is consuming time, is not suitable for the on-the-spot water quality detection to remote districts, rural area and Sudden Pollution Accident.At present, the report to the agent of aniline field quick detection is not yet found.
Summary of the invention
The object of this invention is to provide a kind of detection agent of Fast Measurement concentration of aniline, significant for the Site Detection of aniline in the day water, industrial sewage.
In order to achieve the above object, the present invention adopts N-(1-naphthyl) ethylenediamine coloration method (GB 11889-89) to prepare and detects pulvis, primarily of compositions such as sodium nitrite, N-(1-naphthyl) ethylenediamine-hydrochloride, Amcide Ammate, sulfaminic acids, concrete preparation method is as follows:
The first step: 1:25:25 takes sodium nitrite in mass ratio, citric acid, polyvinylpyrrolidone are each some, mixing, obtains aniline and detects powder I;
Second step: 1:1:8:10:20 takes N-(1-naphthyl)-ethylenediamine-hydrochloride in mass ratio, polyvinyl alcohol (PVA), potassium acid sulfate, sulfaminic acid, Amcide Ammate are each some, first N-(1-naphthyl)-ethylenediamine-hydrochloride is mixed with polyvinyl alcohol (PVA), add a small amount of hot water and grind to form pasty state, grind evenly again together with potassium acid sulfate, 50 degree of baking oven inner dryings 2 hours, mix with sulfaminic acid, Amcide Ammate after pulverizing, obtain aniline and detect powder II;
Above-mentioned N-(1-naphthyl) ethylenediamine-hydrochloride, sodium nitrite, citric acid, polyvinyl alcohol (PVA), sulfaminic acid, Amcide Ammate, polyvinylpyrrolidone are commercially available analysis pure chemicals.
The using method of aniline detection agent: first 0.2 ~ 0.4g aniline is detected powder I and join in 5ml water sample to be measured, abundant mixing, dissolving, after 5min, add 0.1 ~ 0.3g aniline again and detect powder II, after 1min, vibration is to dissolving, place 20min, utilize spectrophotometer or colorimetric measurements water sample chromophoric solution;
Above-mentioned water sample to be measured is the day water, industrial waste water etc.
Aniline detection agent system of the present invention pulvis, have that preparation technology is simple, easy to carry, stable performance, lower-price characteristic, aniline sensing range: 0.02 ~ 1mg/L, be suitable for the Site Detection of the water body such as surface water, industrial waste water aniline content, layman can operate.
Embodiment
embodiment 1,the preparation of aniline detection agent
Weigh 1g sodium nitrite, 25g citric acid, 25g polyvinylpyrrolidone respectively, mix aniline detects powder I; Weigh 0.1gN-(1-naphthyl)-ethylenediamine-hydrochloride, 0.1g polyvinyl alcohol (PVA), 0.8g potassium acid sulfate, 1g sulfaminic acid, 2g Amcide Ammate respectively, first N-(1-naphthyl)-ethylenediamine-hydrochloride is mixed with polyvinyl alcohol (PVA), add a small amount of hot water and grind to form pasty state, grind evenly again together with potassium acid sulfate, 50 degree of baking oven inner dryings 2 hours, mix with sulfaminic acid, Amcide Ammate after pulverizing, obtain aniline and detect powder II.
embodiment 2,in the day water, concentration of aniline measures
Get certain day water 5ml in color comparison tube, add aniline detection powder I 0.2g that embodiment 1 prepares, shaking test tube, to dissolving, after 5min, adds 0.1g aniline and detects powder II, after 1min, shaking test tube extremely dissolves again, place 20min, utilize spectrophotometer (the portable spectrometer Beijing Pu Xi company of PORS-15V) to measure absorbance at 545nm, calculating concentration of aniline in the day water is 0.041mg/L, recovery of standard addition is 98.6%, shows that this detection agent accurately, reliably.
embodiment 3,in industrial waste water, concentration of aniline measures
Get certain industrial waste water 5ml in color comparison tube, add aniline detection powder I 0.2g that embodiment 1 prepares, shaking test tube, to dissolving, after 5min, adds 0.1g aniline and detects powder II, after 1min, vibration is to dissolving, place 20min, utilize spectrophotometer (the portable spectrometer Beijing Pu Xi company of PORS-15V) to measure absorbance at 545nm, calculating concentration of aniline in this industrial waste water is 0.387mg/L, recovery of standard addition is 104.6%, shows that this detection agent accurately, reliably.
Claims (3)
1. one kind measures the quick detection agent of water quality concentration of aniline, it is characterized in that: this detection agent comprises two kinds of pulvis, mix primarily of sodium nitrite, N-(1-naphthyl) ethylenediamine-hydrochloride, Amcide Ammate, sulfaminic acid etc., as long as successively join in water sample by two kinds of pulvis during use, spectrophotometer or tintmeter is utilized directly to measure.
2. a kind of preparation method measuring the quick detection agent of water quality concentration of aniline as claimed in claim 1, is characterized in that:
1:25:25 takes sodium nitrite in mass ratio, citric acid, polyvinylpyrrolidone are each some, mixing, obtains aniline and detects powder I;
1:1:8:10:20 takes N-(1-naphthyl)-ethylenediamine-hydrochloride in mass ratio, polyvinyl alcohol (PVA), potassium acid sulfate, sulfaminic acid, Amcide Ammate are each some, first N-(1-naphthyl)-ethylenediamine-hydrochloride is mixed with polyvinyl alcohol (PVA), add a small amount of hot water and grind to form pasty state, grind evenly again together with potassium acid sulfate, 50 degree of baking oven inner dryings 2 hours, mix with sulfaminic acid, Amcide Ammate after pulverizing, obtain aniline and detect powder II;
Above-mentioned N-(1-naphthyl) ethylenediamine-hydrochloride, sodium nitrite, citric acid, polyvinyl alcohol (PVA), sulfaminic acid, Amcide Ammate, polyvinylpyrrolidone are commercially available analysis pure chemicals.
3. a kind of using method measuring the quick detection agent of water quality concentration of aniline as claimed in claim 1, it is characterized in that: first 0.2 ~ 0.4g aniline is detected powder I and join in 5ml water sample to be measured, abundant mixing, dissolving, after 5min, add 0.1 ~ 0.3g aniline again and detect powder II, after 1min, vibration is to dissolving, and places 20min, utilizes spectrophotometer or colorimetric measurements;
Above-mentioned water sample to be measured is the day water, industrial waste water etc.
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| CN201410107412.5A CN104931436A (en) | 2014-03-21 | 2014-03-21 | Rapid detection agent for determination of water quality aniline concentration |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106918564A (en) * | 2017-01-22 | 2017-07-04 | 北京华腾新材料股份有限公司 | A kind of detection method for determining primary aromatic diamine migration amount in composite plastic packaging |
| CN108152230A (en) * | 2017-12-19 | 2018-06-12 | 江苏康达检测技术股份有限公司 | A kind of method for measuring Nitrobenzene in Wastewater class compound concentration |
| GB2581883A (en) * | 2019-02-12 | 2020-09-02 | Innospec Performance Chemicals Europe Ltd | Treatment of subterranean formations |
| US11753583B2 (en) | 2019-02-12 | 2023-09-12 | Innospec Limited | Treatment of subterranean formations |
| US11987751B2 (en) | 2019-02-12 | 2024-05-21 | Innospec Limited | Treatment of subterranean formations |
-
2014
- 2014-03-21 CN CN201410107412.5A patent/CN104931436A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106918564A (en) * | 2017-01-22 | 2017-07-04 | 北京华腾新材料股份有限公司 | A kind of detection method for determining primary aromatic diamine migration amount in composite plastic packaging |
| CN108152230A (en) * | 2017-12-19 | 2018-06-12 | 江苏康达检测技术股份有限公司 | A kind of method for measuring Nitrobenzene in Wastewater class compound concentration |
| GB2581883A (en) * | 2019-02-12 | 2020-09-02 | Innospec Performance Chemicals Europe Ltd | Treatment of subterranean formations |
| US11739256B2 (en) | 2019-02-12 | 2023-08-29 | Innospec Limited | Treatment of subterranean formations |
| US11753583B2 (en) | 2019-02-12 | 2023-09-12 | Innospec Limited | Treatment of subterranean formations |
| GB2581883B (en) * | 2019-02-12 | 2023-11-15 | Innospec Ltd | Treatment of subterranean formations |
| US11987751B2 (en) | 2019-02-12 | 2024-05-21 | Innospec Limited | Treatment of subterranean formations |
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