CN105300973A - Rapid detection reagent and method for concentration of quaternary ammonium salt - Google Patents
Rapid detection reagent and method for concentration of quaternary ammonium salt Download PDFInfo
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Abstract
The invention discloses a rapid detection reagent and method for the concentration of quaternary ammonium salt. The detection reagent is composed of a color developing agent and a color fixing agent, and the mass ratio of the color developing agent to the color fixing agent is (1-3):(10-40). The detection method includes the following steps that 1, the rapid detection reagent for the concentration of quaternary ammonium salt, solvent and diluent are mixed to be prepared into a solution, filter paper is immersed into the solution to be soaked for 5-30 min and is then taken out to be dried, and rapid detection test paper for the concentration of quaternary ammonium salt is obtained; 2, the rapid detection test paper for the concentration of quaternary ammonium salt is immersed into a test solution prepared from a sample to be tested and is taken out 5 s later, the redundant solution on the test paper is thrown away, the test paper is compared with a standard color chart after 15 s of color development, and the concentration data of quaternary ammonium salt are obtained. The method is short in response time, wide in detection range and high in detection sensitivity, the reagent dosage needed in a single time of testing is only hundredths of that of a common laboratory method, the test process is simple, other instruments and accessories are not needed, and the test cost is low.
Description
Technical field
The present invention relates to a kind of quaternary ammonium salt concentration quick detection reagent and detection method, belong to analytical chemistry field.
Background technology
Quaternary ammonium salt is the important cationic surfactant of a class, and it and other classes of surfactant compatibility are good, and there is good wetting, solubilising, washing, sterilization, softness, help dye, fixation, the premium properties such as antistatic, range of application is more and more wider.Quaternary ammonium disinfectant has the advantages such as bacteriocidal concentration is low, spinoff is little, colourless, odorless, pungency are little, safety low-poison, more and more payes attention to by people.But a large amount of uses of quaternary surfactant can to environmental danger.Therefore, to the accurate Fast Measurement of quaternary ammonium salt concentration, just reasonable employment quaternary ammonium salt can be instructed, harm reduction to greatest extent under in order to be effective prerequisite if can realize.Therefore, a kind of simple and quick quaternary ammonium salt method for measurement of concentration of exploitation is needed badly.
At present, method for quaternary ammonium salt concentration determination mainly comprises following several: volumetric analysis, spectrophotometric method, fluorometry, oscilloscopic polarography, chromatography, capillary electrophoresis and mass spectroscopy etc., the operation that these methods have is very loaded down with trivial details, large-scale analytical instrument used by some need, is all unfavorable for the on-the-spot fast monitored of quaternary ammonium salt concentration.
Test paper method is because of non-secondary pollution, easy to use, the advantage such as to be easy to carry about with one and becoming at present by a kind of in-situ check and test method of consumers.In disinfection technology standard, by under NaOH existent condition, carry out the mensuration of quaternary ammonium salt concentration as a kind of indicator of diphasic titration using bromophenol blue.Experimental study shows, under mildly acidic conditions, bromophenol blue class pH indicator directly can develop the color with quaternary ammonium salt surface active agent in aqueous phase, and has higher sensitivity.The present invention's a kind of quaternary ammonium salt concentration quick detection reagent that utilized this colour developing principle to prepare, only need by this reagent load on test paper, be made into the Test paper of detectable concentration wide ranges, highly sensitive, good stability, just can be used for fast-field evaluation quaternary ammonium salt concentration.
Summary of the invention
The object of the present invention is to provide a kind of quaternary ammonium salt concentration quick detection reagent and detection method.
The technical solution used in the present invention is:
A kind of quaternary ammonium salt concentration quick detection reagent, its component comprises developer and colouring stabilizer, and the mass ratio of described developer and colouring stabilizer is (1 ~ 3): (10 ~ 40).
Further, the component of described detection reagent also comprises pH stabilizing agent.
The pH value of sample solution can be stabilized between 2.5 ~ 4.6 by described pH stabilizing agent.
Described pH stabilizing agent is the one in citrate-phosphate disodium hydrogen buffer system, citric acid-hydrogen citrate potassium buffer system, citric acid-sodium citrate buffer system, tartrate-sodium tartrate buffer system, lactic acid-sodium lactate buffer system.
Described developer is at least one in tetra-chloro-phenol sulfonephthalein, tetrabromophenolsulfonphthalein, tetraiodo phenolsulfonphthalein, tetrabromophenol blue, the green phenol basket of bromine.
Described colouring stabilizer is at least one in polyglycol, soluble starch, polyvinylpyrrolidone.
Further, a kind of quaternary ammonium salt concentration quick detection reagent, its component comprises tetra-chloro-phenol sulfonephthalein, polyglycol, citric acid and sodium hydrogen phosphate, and the mass ratio of described tetra-chloro-phenol sulfonephthalein, polyglycol, citric acid and sodium hydrogen phosphate is (5 ~ 15): (50 ~ 200): (28 ~ 39): (49 ~ 71).
A kind of quaternary ammonium salt concentration detection method, comprises the following steps:
1) by quaternary ammonium salt concentration quick detection reagent, solvent and mixing diluents, wiring solution-forming, immerses in this solution by filter paper, takes out after soaking 5 ~ 30min, dry, obtains quaternary ammonium salt concentration quick detection test paper;
2), in test solution quaternary ammonium salt concentration quick detection test paper immersion testing sample made, take out after 5 seconds, get rid of solution unnecessary on test paper, develop the color after 15 seconds, contrast with standard color comparison card, obtain the concentration data of quaternary ammonium salt.
Solvent described in step 1) is absolute ethyl alcohol, and the mass percentage of described absolute ethyl alcohol is 15% ~ 25%.
Thinning agent described in step 1) is at least one in deionized water, distilled water, ultrapure water.
The invention has the beneficial effects as follows:
1) the method response time of the present invention is fast, measures the fastest an of sample and needs 15 seconds, can carry out fast-field evaluation;
2) method sensing range of the present invention is wide, and detectable quaternary ammonium salt concentration range is 0 ~ 1000mg/L;
3) method single test agent consumption of the present invention only has more than one percent of usual laboratory methods, and test process is simple, and without the need to Other Instruments and accessory, testing cost is low;
4) The inventive process provides a kind of test paper that can carry out field quick detection quaternary ammonium salt concentration, this test paper be highly sensitive, sensing range is wide, good stability, easy and simple to handle, be easy to carry, economical and practical;
5) a large amount of in test paper of the present invention pH stabilizing agents can ensure that the pH value of sample solution does not change in test process, ensure that the accuracy of test result, and the polyglycol in test paper ensure that homogeneity and the stability of test paper color development;
6) detection method of the present invention can be used for the quick detection of quaternary ammonium salt working concentration and residual concentration in quaternary ammonium salt cleaning and sterilization industry.
Accompanying drawing explanation
Fig. 1 is the view of the standard color comparison card 1# of embodiment 1.
Embodiment
The technical solution used in the present invention is:
A kind of quaternary ammonium salt concentration quick detection reagent, its component comprises developer and colouring stabilizer, and the mass ratio of described developer and colouring stabilizer is (1 ~ 3): (10 ~ 40).
Preferably, the component of described detection reagent also comprises pH stabilizing agent.
Preferably, the pH value of sample solution can be stabilized between 2.5 ~ 4.6 by described pH stabilizing agent.
Preferably, described pH stabilizing agent is the one in citrate-phosphate disodium hydrogen buffer system, citric acid-hydrogen citrate potassium buffer system, citric acid-sodium citrate buffer system, tartrate-sodium tartrate buffer system, lactic acid-sodium lactate buffer system.
Preferred further, described pH stabilizing agent is citrate-phosphate disodium hydrogen buffer system.
Preferably, described developer is at least one in tetra-chloro-phenol sulfonephthalein, tetrabromophenolsulfonphthalein, tetraiodo phenolsulfonphthalein, tetrabromophenol blue, the green phenol basket of bromine.
Preferred further, described developer is tetra-chloro-phenol sulfonephthalein.
Preferably, described colouring stabilizer is at least one in polyglycol, soluble starch, polyvinylpyrrolidone.
Preferred further, described colouring stabilizer is polyglycol.
Preferably, a kind of quaternary ammonium salt concentration quick detection reagent, its component comprises tetra-chloro-phenol sulfonephthalein, polyglycol, citric acid and sodium hydrogen phosphate, and the mass ratio of described tetra-chloro-phenol sulfonephthalein, polyglycol, citric acid and sodium hydrogen phosphate is (5 ~ 15): (50 ~ 200): (28 ~ 39): (49 ~ 71).
A kind of quaternary ammonium salt concentration detection method, comprises the following steps:
1) by quaternary ammonium salt concentration quick detection reagent, solvent and mixing diluents, wiring solution-forming, immerses in this solution by filter paper, takes out after soaking 5 ~ 30min, dry, obtains quaternary ammonium salt concentration quick detection test paper;
2), in test solution quaternary ammonium salt concentration quick detection test paper immersion testing sample made, take out after 5 seconds, get rid of solution unnecessary on test paper, develop the color after 15 seconds, contrast with standard color comparison card, obtain the concentration data of quaternary ammonium salt.
Preferably, the solvent described in step 1) is absolute ethyl alcohol, and the mass percentage of described absolute ethyl alcohol is 15% ~ 25%.
Preferably, the thinning agent described in step 1) is at least one in deionized water, distilled water, ultrapure water.
Preferably, the filter paper described in step 1) is the one in chromatography filter paper, qualitative filter paper, quantitative filter paper.
Preferred further, the filter paper described in step 1) is chromatography filter paper.
Preferably, the preparation method of described standard color comparison card comprises the following steps:
1) with pure water compound concentration be the cetyl trimethyl ammonium bromide standard solution of 10mg/L, quaternary ammonium salt concentration quick detection test paper is immersed in solution, take out after 5 seconds, get rid of unnecessary solution, the color presented according to test paper after 15 seconds finds out the consistent standard colors of tone on PMS;
2) with method described in step 1), the standard colors that cetyl trimethyl ammonium bromide concentration of standard solution presents for test paper when 0mg/L, 25mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L, 1000mg/L is measured respectively;
3) contrast the colour that PMS obtains each standard colors, by computer color-mixed and printing, obtain standard color comparison card.
Preferably, by turning the concentration interval of cetyl trimethyl ammonium bromide standard solution down, the standard colors of more concentration can be obtained, and then obtain the standard color comparison card with more standard colorss, the accuracy of semi-quantitative detection method of the present invention can be made to improve further.
Below in conjunction with specific embodiment, the present invention is made further explanation and description.
embodiment 1:
the preparation of quaternary ammonium salt concentration quick detection test paper:
Take absolute ethyl alcohol as solvent, deionized water is thinning agent, and preparation is containing the mixing nitrite ion (wherein the mass percentage of absolute ethyl alcohol is 15%) of 1.0g/L tetra-chloro-phenol sulfonephthalein, 3.9g/L citric acid, 7.1g/L sodium hydrogen phosphate, 12.0g/L polyglycol.Chromatography filter paper to be dipped to completely in above-mentioned mixed liquor about 10 minutes, to take out filter paper, dry in 50 DEG C of baking ovens, then filter paper is cut into the fritter of 5 × 6mm, stick with glue the base plate one end at 5 × 80mm strip, obtain quaternary ammonium salt concentration quick detection test paper 1#.
the preparation of standard color comparison card:
1) with pure water compound concentration be the cetyl trimethyl ammonium bromide standard solution of 10mg/L, test paper embodiment 1 prepared immerses in solution, take out after 5 seconds, get rid of unnecessary solution, the color presented according to test paper after 15 seconds finds out the consistent standard colors of tone on PMS;
2) with method described in step 1), the standard colors that cetyl trimethyl ammonium bromide concentration of standard solution presents for test paper when 0mg/L, 25mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L, 1000mg/L is measured respectively;
3) contrast PMS, obtain the colour of each standard colors, adopt computer color-mixed and print, obtaining standard color comparison card 1#, as shown in Figure 1.
embodiment 2:
the preparation of quaternary ammonium salt concentration quick detection test paper:
Take absolute ethyl alcohol as solvent, deionized water is thinning agent, and preparation is containing the mixing nitrite ion (wherein the mass percentage of absolute ethyl alcohol is 18%) of 0.5g/L tetrabromophenolsulfonphthalein, 2.8g/L citric acid, 4.9g/L sodium hydrogen phosphate, 5.0g/L polyglycol.Chromatography filter paper to be dipped to completely in above-mentioned mixed liquor about 5 minutes, to take out filter paper, dry in 50 DEG C of baking ovens, then filter paper is cut into the fritter of 5 × 5mm, stick with glue the base plate one end at 5 × 80mm strip, obtain quaternary ammonium salt concentration quick detection test paper 2#.
the preparation of standard color comparison card:
1) with pure water compound concentration be the cetyl trimethyl ammonium bromide standard solution of 10mg/L, test paper embodiment 1 prepared immerses in solution, take out after 5 seconds, get rid of unnecessary solution, the color presented according to test paper after 15 seconds finds out the consistent standard colors of tone on PMS;
2) with method described in step 1), the standard colors that cetyl trimethyl ammonium bromide concentration of standard solution presents for test paper when 0mg/L, 25mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L, 1000mg/L is measured respectively;
3) contrast PMS, obtain the colour of each standard colors, adopt computer color-mixed and print, obtaining standard color comparison card 2#.
embodiment 3:
the preparation of quaternary ammonium salt concentration quick detection test paper:
Take absolute ethyl alcohol as solvent, deionized water is thinning agent, and preparation is containing the mixing nitrite ion (wherein the mass percentage of absolute ethyl alcohol is 20%) of 1.5g/L tetraiodo phenolsulfonphthalein, 3.0g/L citric acid, 6.0g/L sodium hydrogen phosphate, 8.0g/L polyglycol.Chromatography filter paper to be dipped to completely in above-mentioned mixed liquor about 15 minutes, to take out filter paper, dry in 50 DEG C of baking ovens, then filter paper is cut into the fritter of 6 × 6mm, stick with glue the base plate one end at 6 × 100mm strip, obtain quaternary ammonium salt concentration quick detection test paper 3#.
the preparation of standard color comparison card:
1) with pure water compound concentration be the cetyl trimethyl ammonium bromide standard solution of 10mg/L, test paper embodiment 1 prepared immerses in solution, take out after 5 seconds, get rid of unnecessary solution, the color presented according to test paper after 15 seconds finds out the consistent standard colors of tone on PMS;
2) with method described in step 1), the standard colors that cetyl trimethyl ammonium bromide concentration of standard solution presents for test paper when 0mg/L, 25mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L, 1000mg/L is measured respectively;
3) contrast PMS, obtain the colour of each standard colors, adopt computer color-mixed and print, obtaining standard color comparison card 3#.
embodiment 4:
the preparation of quaternary ammonium salt concentration quick detection test paper:
Take absolute ethyl alcohol as solvent, deionized water is thinning agent, and preparation is containing the mixing nitrite ion (wherein the mass percentage of absolute ethyl alcohol is 22%) of 0.8g/L tetrabromophenol blue, 3.5g/L citric acid, 6.5g/L sodium hydrogen phosphate, 15.0g/L polyglycol.Chromatography filter paper to be dipped to completely in above-mentioned mixed liquor about 20 minutes, to take out filter paper, dry in 50 DEG C of baking ovens, then this filter paper is cut into the fritter of 8 × 8mm, stick with glue the base plate one end at 8 × 100mm strip, obtain quaternary ammonium salt concentration quick detection test paper 4#.
the preparation of standard color comparison card:
1) with pure water compound concentration be the cetyl trimethyl ammonium bromide standard solution of 10mg/L, test paper embodiment 1 prepared immerses in solution, take out after 5 seconds, get rid of unnecessary solution, the color presented according to test paper after 15 seconds finds out the consistent standard colors of tone on PMS;
2) with method described in step 1), the standard colors that cetyl trimethyl ammonium bromide concentration of standard solution presents for test paper when 0mg/L, 25mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L, 1000mg/L is measured respectively;
3) contrast PMS, obtain the colour of each standard colors, adopt computer color-mixed and print, obtaining standard color comparison card 4#.
embodiment 5:
the preparation of quaternary ammonium salt concentration quick detection test paper:
Take absolute ethyl alcohol as solvent, deionized water is thinning agent, and preparation is containing the mixing nitrite ion (wherein the mass percentage of absolute ethyl alcohol is 25%) of the green phenol indigo plant of 1.2g/L bromine, 3.0g/L citric acid, 6.0g/L sodium hydrogen phosphate, 20.0g/L polyglycol.Chromatography filter paper to be dipped to completely in above-mentioned mixed liquor about 30 minutes, to take out filter paper, dry in 50 DEG C of baking ovens, then filter paper is cut into the fritter of 10 × 10mm, stick with glue the base plate one end at 10 × 120mm strip, obtain quaternary ammonium salt concentration quick detection test paper 5#.
the preparation of standard color comparison card:
1) with pure water compound concentration be the cetyl trimethyl ammonium bromide standard solution of 10mg/L, test paper embodiment 1 prepared immerses in solution, take out after 5 seconds, get rid of unnecessary solution, the color presented according to test paper after 15 seconds finds out the consistent standard colors of tone on PMS;
2) with method described in step 1), the standard colors that cetyl trimethyl ammonium bromide concentration of standard solution presents for test paper when 0mg/L, 5mg/L, 25mg/L, 50mg/L, 75mg/L, 100mg/L, 125mg/L, 250mg/L, 375mg/L, 500mg/L, 625mg/L, 750mg/L, 875mg/L, 1000mg/L is measured respectively;
3) contrast PMS, obtain the colour of each standard colors, adopt computer color-mixed and print, obtaining standard color comparison card 5#.
test case 1:
quaternary ammonium salt concentration determination Contrast on effect is tested:
Choose the quaternary ammonium salt concentration quick detection test paper 1# of the embodiment of the present invention 1, carry out the experiment of quaternary ammonium salt concentration determination Contrast on effect.Method of testing: the cetyl trimethyl ammonium bromide sample solution preparing a series of variable concentrations, adopts the titrimetry in disinfection technology standard and this test paper method to carry out the mensuration of concentration respectively.During test paper method test, when the tone of sample nitrite ion is consistent with standard color range, directly getting color range instruction concentration is measured value, if color is inconsistent, the tone with regard to nitrite ion per sample chooses two adjacent standard color ranges, obtains sample concentration scope.Test result is as shown in table 1.
Effect control experiment result tested by table 1:
test case 2:
quaternary ammonium salt concentration determination Contrast on effect is tested:
Choose the quaternary ammonium salt concentration quick detection test paper 5# of the embodiment of the present invention 5, carry out the experiment of quaternary ammonium salt concentration determination Contrast on effect.Method of testing: the cetyl trimethyl ammonium bromide sample solution preparing a series of variable concentrations, adopts the titrimetry in disinfection technology standard and this test paper method to carry out the mensuration of concentration respectively.During test paper method test, when the tone of sample nitrite ion is consistent with standard color range, directly getting color range instruction concentration is measured value, if color is inconsistent, the tone with regard to nitrite ion per sample chooses two adjacent standard color ranges, obtains sample concentration scope.Test result is as shown in table 2.
Effect control experiment result tested by table 2:
From table 1 and table 2: by quaternary ammonium salt concentration quick detection reagent of the present invention load is obtained quaternary ammonium salt concentration quick detection test paper on filter paper, the Fast Measurement of quaternary ammonium salt concentration can be carried out, without the need to any other instrument and accessory, easy and simple to handle, sensing range is wide, reliable results, has higher using value.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a quaternary ammonium salt concentration quick detection reagent, its component comprises developer and colouring stabilizer, and the mass ratio of described developer and colouring stabilizer is (1 ~ 3): (10 ~ 40).
2. detection reagent according to claim 1, is characterized in that: the component of described detection reagent also comprises pH stabilizing agent.
3. detection reagent according to claim 2, is characterized in that: the pH value of sample solution can be stabilized between 2.5 ~ 4.6 by described pH stabilizing agent.
4. detection reagent according to claim 3, is characterized in that: described pH stabilizing agent is the one in citrate-phosphate disodium hydrogen buffer system, citric acid-hydrogen citrate potassium buffer system, citric acid-sodium citrate buffer system, tartrate-sodium tartrate buffer system, lactic acid-sodium lactate buffer system.
5. detection reagent according to claim 1, is characterized in that: described developer is at least one in tetra-chloro-phenol sulfonephthalein, tetrabromophenolsulfonphthalein, tetraiodo phenolsulfonphthalein, tetrabromophenol blue, the green phenol basket of bromine.
6. detection reagent according to claim 1, is characterized in that: described colouring stabilizer is at least one in polyglycol, soluble starch, polyvinylpyrrolidone.
7. detection reagent according to claim 1, it is characterized in that: its component comprises tetra-chloro-phenol sulfonephthalein, polyglycol, citric acid and sodium hydrogen phosphate, the mass ratio of described tetra-chloro-phenol sulfonephthalein, polyglycol, citric acid and sodium hydrogen phosphate is (5 ~ 15): (50 ~ 200): (28 ~ 39): (49 ~ 71).
8. a quaternary ammonium salt concentration detection method, is characterized in that: comprise the following steps:
1) by quaternary ammonium salt concentration quick detection reagent, solvent and mixing diluents, wiring solution-forming, immerses in this solution by filter paper, takes out after soaking 5 ~ 30min, dry, obtains quaternary ammonium salt concentration quick detection test paper;
2), in test solution quaternary ammonium salt concentration quick detection test paper immersion testing sample made, take out after 5 seconds, get rid of solution unnecessary on test paper, develop the color after 15 seconds, contrast with standard color comparison card, obtain the concentration data of quaternary ammonium salt.
9. detection method according to claim 8, is characterized in that: the solvent described in step 1) is absolute ethyl alcohol, and the mass percentage of described absolute ethyl alcohol is 15% ~ 25%.
10. detection method according to claim 8, is characterized in that: the thinning agent described in step 1) is at least one in deionized water, distilled water, ultrapure water.
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| CN106596530A (en) * | 2016-11-17 | 2017-04-26 | 广东环凯微生物科技有限公司 | Quick detection method for residual concentration of quaternary ammonium salt |
| CN107991292A (en) * | 2016-10-26 | 2018-05-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | The method for detecting quaternary ammonium compound in raw material milk |
| CN109991218A (en) * | 2019-03-29 | 2019-07-09 | 迪瑞医疗科技股份有限公司 | A kind of preparation method of coagulase Test paper |
| CN109991221A (en) * | 2019-03-29 | 2019-07-09 | 迪瑞医疗科技股份有限公司 | A kind of preparation method of Prolyl iminopeptidase Test paper |
| CN111157645A (en) * | 2020-01-03 | 2020-05-15 | 浙江方圆检测集团股份有限公司 | High performance liquid chromatography-tandem mass spectrometry method for determining quaternary ammonium salt in paper for food packaging based on dispersed solid phase extraction |
| CN111693521A (en) * | 2020-05-15 | 2020-09-22 | 杭州临安咔咔玛科技有限公司 | Visual color development method of non-woven fabric with antimicrobial function |
| CN111751189A (en) * | 2020-07-27 | 2020-10-09 | 广东石油化工学院 | Method for determining quaternary ammonium salt disinfectant residue of dairy product based on QuEChERS purification technology |
| CN111948197A (en) * | 2020-07-29 | 2020-11-17 | 福建警察学院 | Colorimetric card for color development test of novel psychoactive substance and design method thereof |
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| CN106596530A (en) * | 2016-11-17 | 2017-04-26 | 广东环凯微生物科技有限公司 | Quick detection method for residual concentration of quaternary ammonium salt |
| CN106596530B (en) * | 2016-11-17 | 2019-04-02 | 广东环凯微生物科技有限公司 | A kind of quaternary ammonium salt residual concentration rapid detection method |
| CN109991218A (en) * | 2019-03-29 | 2019-07-09 | 迪瑞医疗科技股份有限公司 | A kind of preparation method of coagulase Test paper |
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