CN1425917A - Method for producing chlorine residue test paper - Google Patents

Method for producing chlorine residue test paper Download PDF

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Publication number
CN1425917A
CN1425917A CN 03101338 CN03101338A CN1425917A CN 1425917 A CN1425917 A CN 1425917A CN 03101338 CN03101338 CN 03101338 CN 03101338 A CN03101338 A CN 03101338A CN 1425917 A CN1425917 A CN 1425917A
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China
Prior art keywords
test paper
chlorine residue
manufacture method
residue test
acid
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CN 03101338
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Chinese (zh)
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CN1177222C (en
Inventor
吴雄德
陈华清
黄清之
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MINGDA PLASTIC (XIAMEN) CO Ltd
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MINGDA PLASTIC (XIAMEN) CO Ltd
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Priority to CNB031013384A priority Critical patent/CN1177222C/en
Publication of CN1425917A publication Critical patent/CN1425917A/en
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Publication of CN1177222C publication Critical patent/CN1177222C/en
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Abstract

The present invention relates to the production process of chlorine residue test paper with tetraalkyl benzidine, especially 3,3',5,5'-tetramethyl benzidine as color-developing agent. THe production process includes the steps of: compounding the soaking solution with tetraalkyl benzidine, volatile solvent and weak acid regualting agent; soaking test paper in the solution; air drying at 60 deg.c; stoving and cutting the test paper into small sheets; and adhering the sheets to base. The test can resist the pH developing effect in wide range, may be grade into 0,1,2,3,5,10 ppm grades. Being fast and stable in development, the test paper is used in the detection of disinfectant content in swimming pool.

Description

A kind of manufacture method of chlorine residue test paper
(1) technical field
What the present invention relates to is a kind of tetraalkyl diphenyl amine of using, and especially using 3,3 ', 5,5 ' one tetramethyl benzidine (TMB) is the manufacture method of the chlorine residue test paper of developer.
(2) background technology
At present, have multiple chlorine residue test paper both at home and abroad.As the CN4055240A public announcement of a patent application be a kind of chelate (colourless) that utilizes tygon pyrrolinone and potassium iodide with the effective chlorine effect of variable concentrations after, can produce the chelate of tygon pyrrolinone and iodine, the color of its chelate is directly proportional with the concentration of effective chlorine, color range is excessive to brown by yellow, its test specification is 10~50000ppm, and the color range grade is 50,100,150,200,300,500,1000,2000ppm.The CN1286402A public announcement of a patent application be a kind of with N, N-diethyl p-phenylenediamine (DPD) is the chlorine residue test paper of developer, to pink, the color range scope is 0~100ppm to color range by pale red.The CN2375965Y public announcement of a patent application be the test paper that a kind of dissolving power of utilizing siliver chromate is far longer than the principle preparation of silver chloride, it is known as is to be used for measuring effectively cl concn of water, but is actually the mensuration chlorine ion concentration.The CN87102722A public announcement of a patent application be that a kind of potassium iodide that utilizes can be had an effect with effective chlorine in sour environment, use the test paper of starch coloration again, can measure the color range scope is 31.25~8000ppm.The ubiquitous problem of obvious above-mentioned technology is that the scope that detects is too big, insensitive.What the US5976823 patent was set forth is that a kind of employing aniline category matter is a developer, with peroxidase is catalyzer, add the test paper that materials such as buffer solution and surfactant are made, it is used to measure total cl concn, it is said the total cl concn that can measure 0~2ppm.The US5491094 patent is set forth be a kind of be the test paper of developer with tetraalkyl biphenylamine, it has added polyethoxy fatty alcohol (polyethoxylatedfatty alcohol) improves developer and carrier regenerated fiber as non-ionic surfactant absorption property in prescription, and adopting low alkyl vinyl ether and 1, the multipolymer of the low alkyl monoester of 2-ethylene carboxylic acid is as stabilizing agent.The patented product can be measured the effective chlorine of 0~25ppm.
Swimming pool generally adopts chlorine-containing disinfectant to carry out disinfection now, by U.S. public health bureau and international swimming union's regulation, the contents of residual chlorine of swimming-pool water must be higher than 0.2ppm, and (China requires the swimming pool contents of residual chlorine to be controlled at 0.4~0.6ppm), to the swimming-pool water that adopts TCCA (TCCA), DCCNa (SDIC) to carry out disinfection, require its available chlorine content on be limited to 3ppm, surpassing 5ppm will stimulate eyes.Therefore be used for the contents of residual chlorine that test paper that the swimming-pool water contents of residual chlorine measures must be able to be tested 0~10ppm.
(3) summary of the invention
The present invention aims to provide a kind of manufacture method that is mainly used in the test paper of the semiquantitative determination of contents of residual chlorine in the swimming-pool water.
The present invention adopts the tetraalkyl diphenyl amine as developer, adds acid regulator and realizes test paper color development.
Procedure of processing of the present invention is as follows:
1, by the formulated soaking solution, said prescription is (press mass ratio and calculate, down together): with tetraalkyl biphenylamine is 1, and volatile solvent is 40~100, and the weak acid correctives is 1~2;
2, the test paper body paper is dipped in the above-mentioned solution, takes out after 30~60 seconds;
3, under normal temperature~60 ℃, dry;
4, the good test paper of oven dry is cut into fritter, pastes again on the substrate, make test paper, to the test paper of making can test 0,1,2,3,5 respectively, the effective chlorine standard solution of 10ppm, compare color discrimination.
The alkyl of tetraalkyl biphenylamine can be groups such as methyl, ethyl, can be with a kind of group, also can be group not of the same race, but the effect of group of the same race can be quite a lot of, 4 methyl-3 particularly, 3 ', 5,5 '-tetramethyl benzidine (TMB).Solvent requires to select volatile solvent for use, can be ethanol, propyl alcohol, isopropyl alcohol, acetone, butanone or cyclohexanone etc., or their potpourri.The potpourri of ethanol and acetone particularly.
Acid regulator requires to select the weak acid material for use, can be lactic acid, acetic acid, sodium dihydrogen phosphate or citric acid etc., or their potpourri.Particularly lactic acid, citric acid.
Said substrate can be the hard substrate, for example rigid plastic substrate etc.
The test paper of gained of the present invention can be resisted the influence of pH value (pH=4~10) to the colour developing of test paper in the larger context, can be by 0,1,2,3,5, the 10ppm classification, quick colour-developing, color stability, color range is distinguished obviously, can be used for daily swimming sterilizing agent content and detect and instruct an amount of sanitizer of interpolation.
(4) embodiment
Embodiment 1~8: soak solution prescription and color developing effect are as shown in the table:
Raw material Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7 Embodiment 8
??TMB ??1 ????1 ????1 ????1 ????1 ????1 ????1 ????1
Ethanol ????20 ????35 ????35 ????35 ????100 ????100
Acetone ??40 ????40 ????20 ????7 ????7 ????7
Citric acid ??2 ????1 ????1.5 ????1 ????1 ????2
Lactic acid ????1 ????2 ????1 ????2
Soak time (S) ??30 ????35 ????40 ????50 ????40 ????60 ????30 ????35
Dry temperature (℃) Normal temperature Normal temperature ????50 ????45 ????40 ????60 ????55 ????30
Color developing effect Generally Generally Better Best Better Better Relatively poor Relatively poor
In processing test paper process, the good test paper of oven dry is cut fritter into about 5mm * 5mm, paste again on the white hard plastic sheet of about 70mm * 5mm * 0.2mm and get final product.
Embodiment 9~13: its manufacturing technology steps is identical, and the prescription of process conditions and soaking solution sees for details shown in the following table, and the color developing effect of gained test paper is difference slightly.
Raw material Embodiment 9 Embodiment 10 Embodiment 11 Embodiment 12 Embodiment 13
The A group ????1
The B group ????1
The A+B group ????0.5+0.5 ????0.3+0.7 ????0.6+0.4
Ethanol ????25 ????40 ????30
Propyl alcohol ????20 ????35 ????30
Isopropyl alcohol ????20 ????20 ????10
Acetone ????30 ????30 ????10
Butanone ????10 ????20
Cyclohexanone ????20
Lactic acid ????1 ????0.5 ????1
Acetic acid ????1 ????0.5 ????0.5 ????1
Sodium dihydrogen phosphate ????1 ????1
Citric acid ????0.5 ????0.5 ????0.5
Soak time (S) ????60 ????30 ????45 ????50 ????40
Dry temperature (0 ℃) ????40 ????50 ????60 Normal temperature ????30
In last table, A represents tetramethyl benzidine, and B represents tetraethyl biphenylamine.

Claims (10)

1, a kind of manufacture method of chlorine residue test paper is characterized in that its procedure of processing is as follows:
1), by the formulated soaking solution, said prescription is calculated as by mass ratio: with tetraalkyl biphenylamine is 1, volatile solvent is 40~100, the weak acid correctives is 1~2;
2), the test paper body paper is dipped in the above-mentioned solution taking-up after 30~60 seconds;
3), under normal temperature~60 ℃, dry;
4), the good test paper of oven dry is cut into fritter, paste again on the substrate, make test paper.
2, the manufacture method of a kind of chlorine residue test paper as claimed in claim 1, the alkyl that it is characterized in that tetraalkyl biphenylamine is a methyl, or ethyl, or methyl and ethyl group.
3, the manufacture method of a kind of chlorine residue test paper as claimed in claim 1 is characterized in that said group is 4 methyl-3,3 ', 5, and 5 '-tetramethyl benzidine.
4, the manufacture method of a kind of chlorine residue test paper as claimed in claim 1 is characterized in that said solvent is an ethanol, propyl alcohol, isopropyl alcohol, acetone, butanone or cyclohexanone.
5, the manufacture method of a kind of chlorine residue test paper as claimed in claim 4 is characterized in that said solvent is an ethanol, propyl alcohol, isopropyl alcohol, acetone, at least two kinds potpourri in butanone or the cyclohexanone.
6, the manufacture method of a kind of chlorine residue test paper as claimed in claim 4 is characterized in that said solvent is the potpourri of ethanol and acetone.
7, the manufacture method of a kind of chlorine residue test paper as claimed in claim 1 is characterized in that acid regulator is a lactic acid, acetic acid, sodium dihydrogen phosphate or citric acid.
8, the manufacture method of a kind of chlorine residue test paper as claimed in claim 7 is characterized in that acid regulator is a lactic acid, acetic acid, at least two kinds potpourri in sodium dihydrogen phosphate or the citric acid.
9, the manufacture method of a kind of chlorine residue test paper as claimed in claim 7 is characterized in that acid regulator is the potpourri of lactic acid and citric acid.
10, the manufacture method of a kind of chlorine residue test paper as claimed in claim 1 is characterized in that said substrate is the hard substrate.
CNB031013384A 2003-01-03 2003-01-03 Method for producing chlorine residue test paper Expired - Fee Related CN1177222C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB031013384A CN1177222C (en) 2003-01-03 2003-01-03 Method for producing chlorine residue test paper

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Application Number Priority Date Filing Date Title
CNB031013384A CN1177222C (en) 2003-01-03 2003-01-03 Method for producing chlorine residue test paper

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CN1177222C CN1177222C (en) 2004-11-24

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101042353B (en) * 2006-03-23 2010-05-26 三浦工业株式会社 Composition for measuring concentration of residual chlorine
CN104458719A (en) * 2014-11-25 2015-03-25 成都威尔诺生物科技有限公司 Preparation method for sing-component TMB color development solution
CN108132248A (en) * 2016-12-01 2018-06-08 中国科学院大连化学物理研究所 A kind of free chlorine Test paper and its preparation method and application
CN110095457A (en) * 2019-04-17 2019-08-06 广东环凯微生物科技有限公司 A kind of the measurement test paper and rapid assay methods of chlorine residue
CN114414560A (en) * 2021-12-30 2022-04-29 广东环凯生物技术有限公司 Test paper for measuring total chlorine, preparation method thereof and method for rapidly measuring total chlorine

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101042353B (en) * 2006-03-23 2010-05-26 三浦工业株式会社 Composition for measuring concentration of residual chlorine
CN104458719A (en) * 2014-11-25 2015-03-25 成都威尔诺生物科技有限公司 Preparation method for sing-component TMB color development solution
CN104458719B (en) * 2014-11-25 2017-04-05 成都威尔诺生物科技有限公司 A kind of preparation method of one-component TMB nitrite ions
CN108132248A (en) * 2016-12-01 2018-06-08 中国科学院大连化学物理研究所 A kind of free chlorine Test paper and its preparation method and application
CN110095457A (en) * 2019-04-17 2019-08-06 广东环凯微生物科技有限公司 A kind of the measurement test paper and rapid assay methods of chlorine residue
CN114414560A (en) * 2021-12-30 2022-04-29 广东环凯生物技术有限公司 Test paper for measuring total chlorine, preparation method thereof and method for rapidly measuring total chlorine

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