CN103018241B - Method for rapidly detecting hydrazine content in water in semi-quantitative mode - Google Patents
Method for rapidly detecting hydrazine content in water in semi-quantitative mode Download PDFInfo
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- CN103018241B CN103018241B CN201210548189.9A CN201210548189A CN103018241B CN 103018241 B CN103018241 B CN 103018241B CN 201210548189 A CN201210548189 A CN 201210548189A CN 103018241 B CN103018241 B CN 103018241B
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Abstract
The invention provides a method for rapidly detecting the hydrazine content in water in a semi-quantitative mode. The method comprises the following steps: using an ethanol solution of a rare earth-beta-diketone complex as a reagent A, and using an ethanol solution of 1,10-phenanthroline-5,6-diketone as a reagent B; uniformly mixing the reagent A and the reagent B in equal volume; subsequently sucking a certain-volume mixed liquor to be added into a certain-volume water sample; shaking for half a minute, and comparing the color of the water sample with a standard color spectrum so as to judge the content of the hydrazine in the water sample. By utilizing the method, the hydrazine within a range of 0.2-50mg/L in the water can be detected with good repeatability; very few reagents are needed, so that the secondary pollution to the environment is reduced, and the method belongs to semi-quantitative detection; detection results can be given within 2-5 minutes by using ordinary glass instruments, the detection method is simple and rapid, and articles used are convenient to carry over, so that the method is particularly applicable to the use in situations that the content of the hydrazine in water is rapidly detected outdoors or on site, however the result accuracy is not highly required.
Description
Technical field
The invention belongs to water pollutant monitoring field, be specifically related to a kind of method that sxemiquantitative detects hydrazine content in water fast.
Background technology
Hydration hydrazine and its derivative is the important fine chemical material of a class, is widely used in the fields such as chemical products, medical product, agrochemical product, water treatment, photograph and photographic product, as reductive agent, antioxidant.The toxicity of hydrazine hydrate belongs to hypertoxic type, if the hydrazine hydrate in industrial waste water is discharged in rivers, brings huge destruction by environment, the not only safety of the local potable water of serious harm, and nitrogenous effluent can also cause the eutrophication of water quality, consume the dissolved oxygen DO in water, worsen water ecological setting.Therefore the content detecting hydrazine in industrial discharge waste water is significant.
At present, the method detecting hydrazine mainly contains paradime thylaminobenzaldehyde spectrophotometric method (national standard detects the method for hydrazine), iodimetric titration (Guo Xiushuan, rare metal and wimet, phase nineteen ninety-five 02), electrochemical method (Xu Qin, Li Lihua, Hu Xiaoya, assay laboratory, 2008, 72(5), 20-25), although these method accuracy are higher, but the deficiency of said method all must possess laboratory condition and corresponding analytical instrument just can detect, which increase the cost of detection, require also higher to the professional skill of checker, detect required time longer.During outdoor or detection that scene is to hydrazine content in water, do not have room to test the requirement of room accuracy in detection to the requirement of testing result accuracy high, mainly can rapid semi-quantitative obtain out result, and said method cannot meet the requirement of open air or Site Detection.
Summary of the invention
The object of the invention is to solve existing detection method Shortcomings, providing a kind of and being suitable for the method that open air or on-the-spot sxemiquantitative detect hydrazine content in water fast.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
Sxemiquantitative detects a method for hydrazine content in water fast, and the method is with the ethanolic solution of rare earth-beta-diketon class complex for A reagent, and the ethanolic solution of 1,10-Phendione is B reagent; A reagent and B reagent equal-volume are mixed, then draws the mixed liquor determining volume and join and determine in the water sample of volume, after jolting half a minute, water sample and standard colour chart are carried out color comparison, the content of hydrazine in water sample can be judged.
The volume ratio preferred (1-10) of described mixed liquor and water sample: 100.
Further, described standard colour chart is after first A reagent and B reagent equal-volume being mixed, then drawing the mixed liquor determining volume, to join the hydrazine concentration of determining volume be in the series standard solution of 0.2 ~ 50 mg/L, after jolting half a minute, the solution colour corresponding to gained series standard solution is standard colour chart.
The volume ratio preferred (1-10) of described mixed liquor and standard solution: 100.
Further, printing technology standard colour chart is adopted to make standard colour chart plate.
Further, the mass concentration of described A reagent is 1.5 ~ 2.5%.
Further, the mass concentration of described A reagent is 1.8%.
Further, described rare earth-beta-diketon class complex is Rare Earth with Acetylacetone complex, rare earth trifluoroacetylacetone (TFA) complex, rare earth benzoyl acetone complex or rare earth dibenzoyl-acetone complex.
Further, the mass concentration of described B reagent is 0.5 ~ 1.5%.
Further, the mass concentration of described B reagent is 0.84%.
Self-evident, the present invention, as colourimetry, when detecting the content of hydrazine in water sample, replaces hydrazine standard solution with isopyknic water sample, and the consumption of A reagent and B reagent and usage identical with during preparation standard chromatogram.
Beneficial effect of the present invention:
(1) method of the present invention can detect the hydrazine of content within the scope of 0.2 ~ 50mg/L in water, reproducible, and required amount of reagent is few, decreases the secondary pollution to environment, belongs to half-quantitative detection.
(2) this method uses conventional glass apparatus can provide testing result within 2 ~ 5 minutes, without the need to special detection instrument, as spectrophotometer, simple, quick, the used article of detection method are easy to carry, the method is particularly suitable for the content of hydrazine in open air or field quick detection water, but requires that not too high place uses to result precision.
Accompanying drawing explanation
Fig. 1 is standard colour chart of the present invention.
In figure solution colour from deep to shallow respectively corresponding hydrazine concentration be 50.0,25.0,10.0,5.0,1.0 and 0.2mg/L.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
The employing prior art synthesis of rare earth-beta-diketon class complex obtains, the selection of rare earth element is not particularly limited, can be any one in europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, cerium, lanthanum, praseodymium, scandium, yttrium, samarium, neodymium and lutetium, beta-diketonate ligand adopts diacetone, trifluoroacetylacetone (TFA), benzoyl acetone or dibenzoyl-acetone, building-up process specifically can list of references 1, " syntheses and properties of Rare Earth with Acetylacetone complex " Li Mengjie, Chu Xin
mining science technology2nd phase in 2006; 2, " synthesis of trifluoroacetylacetone (TFA) (HTTA) and rare earth ion Y (III), Er (III) and Nd (III) complex and character " Zhong Sanzi, Li is newborn, Chen Yilang, Liu Juanjuan
university Of Nanchang's journal (natural sciences version)03 phase in 2003; 3, " synthesis and study on property of the complex of four kinds of novel beta-diketons and yttrium " Chen Yilang, Li is newborn, Zhang Hua, Ou Yangmeng
rare earth06 phase in 2004.
Embodiment 1
Detection reagent is A: mass concentration is the ethanolic solution of rare-earth europium (III) acetyl acetone complex of 1.8%; And B: the ethanolic solution of 1,10-Phendione of mass concentration 0.84%, use before by A, B two solution equal-volume mix, obtain C reagent.
Hydrazine concentration is become by the hydrazine hydrate solution thin up of concentration known to be respectively the series standard solution of 0.2,1.0,5.0,10.0,25.0 and 50.0mg/L.
Pipette the above-mentioned standard solution of 10ml respectively, then add the C reagent of 0.1ml, after jolting half a minute, obtain the standard colour chart that color changes from shallow to deep, thus obtain the corresponding relation of color and concentration.Carry for convenience and use, adopting conventional printing technology standard colour chart to be made standard colour chart plate made of paper.
Measuring 10ml water sample to be measured pours in glass sample bottle, the C reagent of 0.1ml is pipetted with transfer pipet, after hand half a minute, water sample and standard colour chart or standard colour chart plate made of paper are carried out color contrast, observe which two adjacent color is water sample color be between, the content of hydrazine water sample can be judged from the concentration corresponding to two adjacent colors.
For making to obtain content more accurately, first can prepare the standard colour chart plate of many cover variable concentrations gradients, then comparing with water sample.
Claims (7)
1. sxemiquantitative detects a method for hydrazine content in water fast, it is characterized in that: described method is with the ethanolic solution of rare earth-beta-diketon class complex for A reagent, and the ethanolic solution of 1,10-Phendione is B reagent; A reagent and B reagent equal-volume are mixed, the mixed liquor then drawing a certain amount of volume joins in the water sample of a certain amount of volume, after jolting half a minute, water sample and standard colour chart is carried out color comparison, can judge the content of hydrazine in water sample;
Described standard colour chart is after first A reagent and B reagent equal-volume being mixed, then the hydrazine concentration that the mixed liquor drawing a certain amount of volume joins a certain amount of volume is in the series standard solution of 0.2 ~ 50mg/L, after jolting half a minute, the solution colour corresponding to gained series standard solution is standard colour chart.
2. sxemiquantitative detects the method for hydrazine content in water fast according to claim 1, it is characterized in that: described rare earth-beta-diketon class complex is Rare Earth with Acetylacetone complex, rare earth trifluoroacetylacetone (TFA) complex, rare earth benzoyl acetone complex or rare earth dibenzoyl-acetone complex.
3. sxemiquantitative detects the method for hydrazine content in water fast according to claim 1, it is characterized in that: standard colour chart adopted printing technology to make standard colour chart plate.
4. sxemiquantitative detects the method for hydrazine content in water fast according to claim 1, it is characterized in that: the mass concentration of described A reagent is 1.5 ~ 2.5%.
5. sxemiquantitative detects the method for hydrazine content in water fast according to claim 4, it is characterized in that: the mass concentration of described A reagent is 1.8%.
6. sxemiquantitative detects the method for hydrazine content in water fast according to claim 1, it is characterized in that: the mass concentration of described B reagent is 0.5 ~ 1.5%.
7. sxemiquantitative detects the method for hydrazine content in water fast according to claim 6, it is characterized in that: the mass concentration of described B reagent is 0.84%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210548189.9A CN103018241B (en) | 2012-12-17 | 2012-12-17 | Method for rapidly detecting hydrazine content in water in semi-quantitative mode |
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| CN201210548189.9A CN103018241B (en) | 2012-12-17 | 2012-12-17 | Method for rapidly detecting hydrazine content in water in semi-quantitative mode |
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| CN103018241B true CN103018241B (en) | 2015-06-10 |
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| CN104155292A (en) * | 2014-06-19 | 2014-11-19 | 东力（南通）化工有限公司 | Method for detecting content of mildronate intermediate 3-(2,2,2-trimethylhydrazine) methyl propionate methylsulfate |
| CN112304932A (en) * | 2020-11-02 | 2021-02-02 | 三门核电有限公司 | Device and method for rapidly detecting loop hydrazine in nuclear power plant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4395494A (en) * | 1979-10-24 | 1983-07-26 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Reagent and method for the determination of hydrazine |
| CN1687079A (en) * | 2005-04-07 | 2005-10-26 | 黑龙江大学 | Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method |
| CN101885675A (en) * | 2009-05-13 | 2010-11-17 | 吉林师范大学 | Preparation method of beta-diketone tine (IV) compound |
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2012
- 2012-12-17 CN CN201210548189.9A patent/CN103018241B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4395494A (en) * | 1979-10-24 | 1983-07-26 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Reagent and method for the determination of hydrazine |
| CN1687079A (en) * | 2005-04-07 | 2005-10-26 | 黑龙江大学 | Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method |
| CN101885675A (en) * | 2009-05-13 | 2010-11-17 | 吉林师范大学 | Preparation method of beta-diketone tine (IV) compound |
Non-Patent Citations (2)
| Title |
|---|
| "1,10-邻菲罗啉-5,6二酮的合成工艺研究";胡晓洁等;《浙江化工》;20071231;第38卷(第3期);第4，5和11页 * |
| "A senstive colorimetric determination of microquantities of isonicotinic acid hydrazide(isoniazid)";Prodromos B. Issopoulos et al.;《International Journal of Pharmaceutics》;19891231;第57卷;第235-239页 * |
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