CN114414560A - Test paper for measuring total chlorine, preparation method thereof and method for rapidly measuring total chlorine - Google Patents
Test paper for measuring total chlorine, preparation method thereof and method for rapidly measuring total chlorine Download PDFInfo
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- CN114414560A CN114414560A CN202111680139.1A CN202111680139A CN114414560A CN 114414560 A CN114414560 A CN 114414560A CN 202111680139 A CN202111680139 A CN 202111680139A CN 114414560 A CN114414560 A CN 114414560A
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- 238000012360 testing method Methods 0.000 title claims abstract description 100
- 239000000460 chlorine Substances 0.000 title claims abstract description 84
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 238000002791 soaking Methods 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000005470 impregnation Methods 0.000 claims abstract description 16
- 239000000080 wetting agent Substances 0.000 claims abstract description 16
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 10
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 8
- -1 thioglycollic acid alkali metal salt Chemical class 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 5
- 238000011161 development Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000004094 surface-active agent Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 5
- DVMSVWIURPPRBC-UHFFFAOYSA-N 2,3,3-trifluoroprop-2-enoic acid Chemical compound OC(=O)C(F)=C(F)F DVMSVWIURPPRBC-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- HYTYHTSMCRDHIM-UHFFFAOYSA-M potassium;2-sulfanylacetate Chemical compound [K+].[O-]C(=O)CS HYTYHTSMCRDHIM-UHFFFAOYSA-M 0.000 claims description 4
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- GNBVPFITFYNRCN-UHFFFAOYSA-M sodium thioglycolate Chemical compound [Na+].[O-]C(=O)CS GNBVPFITFYNRCN-UHFFFAOYSA-M 0.000 claims description 3
- 229940046307 sodium thioglycolate Drugs 0.000 claims description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 235000005985 organic acids Nutrition 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000003513 alkali Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 claims 1
- CWERGRDVMFNCDR-UHFFFAOYSA-M thioglycolate(1-) Chemical class [O-]C(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-M 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 12
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 238000004587 chromatography analysis Methods 0.000 description 17
- 239000000243 solution Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 8
- 239000012086 standard solution Substances 0.000 description 7
- CWERGRDVMFNCDR-UHFFFAOYSA-N alpha-mercaptoacetic acid Natural products OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000000645 desinfectant Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 230000009182 swimming Effects 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 2
- 229920000084 Gum arabic Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 241000978776 Senegalia senegal Species 0.000 description 2
- 239000000205 acacia gum Substances 0.000 description 2
- 235000010489 acacia gum Nutrition 0.000 description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 2
- 229960002303 citric acid monohydrate Drugs 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000001630 malic acid Substances 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- 125000005007 perfluorooctyl group Chemical group FC(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)* 0.000 description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 2
- UAIUNKRWKOVEES-UHFFFAOYSA-N 3,3',5,5'-tetramethylbenzidine Chemical compound CC1=C(N)C(C)=CC(C=2C=C(C)C(N)=C(C)C=2)=C1 UAIUNKRWKOVEES-UHFFFAOYSA-N 0.000 description 1
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- 239000004155 Chlorine dioxide Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000008277 Immersion Foot Diseases 0.000 description 1
- 206010044584 Trench foot Diseases 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 235000019398 chlorine dioxide Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- JSYGRUBHOCKMGQ-UHFFFAOYSA-N dichloramine Chemical compound ClNCl JSYGRUBHOCKMGQ-UHFFFAOYSA-N 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- QEHKBHWEUPXBCW-UHFFFAOYSA-N nitrogen trichloride Chemical compound ClN(Cl)Cl QEHKBHWEUPXBCW-UHFFFAOYSA-N 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 125000002813 thiocarbonyl group Chemical group *C(*)=S 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides a test paper for measuring total chlorine, a preparation method thereof and a method for rapidly measuring total chlorine, wherein the preparation method of the test paper comprises the following steps: (1) dissolving a color developing agent and a pH regulator in a solvent A to prepare a steeping liquor A; (2) dissolving a wetting agent, a stabilizer and a film forming agent in a solvent B to prepare an impregnation solution B; (3) soaking filter paper in the soaking solution A for the first time, taking out and drying the filter paper, then placing the filter paper in the soaking solution B for the second time, taking out, drying, cutting and pasting the filter paper on a substrate; the color developing agent comprises thiomicone or a compound with an active structure similar to that of the thiomicone; the wetting agent is selected from nonionic fluorosurfactants; the stabilizer is thioglycollic acid alkali metal salt. The test paper for measuring total chlorine prepared by the preparation method has the advantages of high sensitivity, obvious color gradation, wide detection range, simple and convenient operation and long quality guarantee period.
Description
Technical Field
The invention relates to the field of analytical chemistry, in particular to a test paper for measuring total chlorine, a preparation method thereof and a method for rapidly measuring the total chlorine.
Background
The total chlorine refers to free residual chlorine (including Cl) in water after water is disinfected by chlorine-containing disinfectant2、ClO-HClO) and chemical residual chlorine (monochloramine, dichloramine, trichloramine). The chlorine adding amount in the water can be divided into two parts, namely the required chlorine amount and the residual chlorine. The chlorine demand refers to a part consumed for killing bacteria, oxidizing organic matters and reducing substances, and the residual chlorine refers to a part for inhibiting the breeding of bacteria. When the water is mainly polluted by bacteria, organic matters and reducing substances and is free from ammonia nitrogen and nitrogen compounds, adding a chlorine disinfectant (not containing chlorine dioxide), wherein the residual chlorine is mainly free residual chlorine; when ammonia nitrogen or nitrogen-containing organic matters exist in water, after a chlorine disinfectant is added, bacteria and reducing substances firstly consume a part of chlorine, then the bacteria and the reducing substances react with the nitrogen-containing substances such as the ammonia nitrogen and the like to generate chemical residual chlorine, when the adding amount of the chlorine is continuously increased, the chemical residual chlorine is converted into nitrogen, and the free residual chlorine does not appear until the chlorine adding break point. Therefore, when ammonia nitrogen exists in water, the situation that the free residual chlorine value is very low, but the total chlorine value is very high is easy to occur. Therefore, the method has great significance for rapidly detecting the water sample with ammonia nitrogen or nitrogen-containing compounds on site.
The total chlorine test paper product is popular among users due to the advantages of portability, easy operation, rapid test, low detection cost, no need of maintenance, no secondary pollution and the like. The total chlorine test paper on the market at present mainly comprises a thiomico method and a 3,3',5,5' -Tetramethylbenzidine (TMB) method. The sensitivity of the test paper is high, the minimum detection concentration is 0.10mg/L, but the quality guarantee period of the test paper is only half a year generally; the shelf life of the water sample can reach one year, but the sensitivity is not high, the minimum detection concentration is generally not lower than 0.50mg/L, water samples with low total chlorine content such as tap water, medical permeating water and the like cannot be detected, and the application range is limited to a certain extent. In addition, the total chlorine determination test paper on the market generally needs 3-10 minutes for color development, and the determination time is prolonged. In view of this, the current test paper for total chlorine and the rapid detection method need to be further improved.
Disclosure of Invention
In view of the above problems, the present invention provides a method for preparing a test paper for total chlorine, comprising the steps of:
(1) dissolving a color developing agent and a pH regulator in a solvent A to prepare a steeping liquor A;
(2) dissolving a wetting agent, a stabilizer and a film forming agent in a solvent B to prepare an impregnation solution B;
(3) soaking the filter paper in the soaking solution A for the first time, taking out and drying the filter paper, then placing the filter paper in the soaking solution B for the second time, taking out the filter paper, drying, cutting and pasting the filter paper on a substrate;
the color developing agent comprises thiomicone or a compound with an active structure similar to that of the thiomicone; the wetting agent is selected from nonionic fluorosurfactants, and the stabilizer is thioglycolic acid alkali metal salt.
Compared with the prior art, in the preparation method of the test paper for measuring the total chlorine, the color developing agent comprises the thiomicone or a compound with an active structure similar to that of the thiomicone; the wetting agent is selected from nonionic fluorosurfactant and the stabilizer is thioglycolic acid alkali metal salt. The test paper has the advantages that the color developing agent of the thiomicone or the compound with the similar active structure with the thiomicone is difficult to dissolve in water, and the nonionic fluorine surfactant is added, so that the wetting efficiency of the color developing agent in the filter paper matrix is improved, and the test paper has excellent test sensitivity. Meanwhile, through a great deal of experimental research, the inventor finds that: (1) the mercaptoacetic acid alkali metal salt compound is added, so that the active thiocarbonyl in the color developing agent can be effectively protected, and the color of the test paper is stably not changed within half an hour; (2) by means of step-by-step soaking (two-step soaking), the film-forming agent can form a stable and uniform water-soluble polymer film on the surface of the chromatographic filter paper in a short time under the coordination of the nonionic fluorine surfactant, so that the test paper is isolated from direct contact with air, and the purpose of greatly prolonging the quality guarantee period of the test paper on the premise of not influencing the color development sensitivity of the test paper is achieved. On the other hand, the water-soluble polymeric membrane also changes the original surface tension structure of the test paper, increases the contact surface of the color developing agent and the liquid to be tested in the process of soaking the test paper, positively promotes the specific color developing reaction generated by residual chlorine, and greatly shortens the color developing response time of the test paper.
Correspondingly, the invention also provides the test paper for measuring the total chlorine, which is prepared by the preparation method.
Correspondingly, the invention also provides a method for rapidly determining the total chlorine, which comprises the steps of immersing the test paper for determining the total chlorine into a sample to be determined, taking out the test paper after 4-9 seconds, comparing the test paper with a standard color comparison card after complete color development, and determining the total chlorine content in the sample.
The invention has the following beneficial effects:
(1) in the preparation method of the test paper for measuring the total chlorine, the wetting agent is selected from nonionic fluorine surfactants, the film forming agent is selected from water-soluble organic high molecular polymers, and the wetting agent and the film forming agent in the test paper act in a coordinated manner, so that the response time of the test paper for developing color is greatly improved, and the response time of the test paper for developing color is greatly shortened.
(2) In the preparation method of the test paper for measuring total chlorine, the wetting agent is selected from nonionic fluorine surfactants, the stabilizer is thioglycollic acid alkali metal salt, the film forming agent is selected from water-soluble organic high molecular polymers, and the wetting agent, the stabilizer and the film forming agent in the test paper act coordinately, so that the test paper is sealed and stored in a dark place at room temperature, and the shelf life is effectively prolonged.
(3) The test paper for measuring the total chlorine has wide detection range, and is suitable for measuring the total chlorine concentration of medical treatment, food and beverage, scientific research, drinking water, swimming pool water, aquaculture, environmental monitoring wastewater and the like.
(4) The test paper for measuring the total chlorine has the advantages of simple detection and test process, rapid color development, no need of other instruments and accessories and great saving of test cost.
(5) The hand-held bottom plate can prevent hands from being polluted by chlorine-containing water samples in the taking process, and the body of field personnel is prevented from being injured.
(6) The test paper for measuring total chlorine has the advantages of high sensitivity, obvious color gradation, wide detection range, simple and convenient operation and long quality guarantee period.
Detailed Description
The invention provides a preparation method of test paper for measuring total chlorine, which comprises the following steps:
(1) dissolving a color developing agent and a pH regulator in a solvent A to prepare a steeping liquor A;
(2) dissolving a wetting agent, a stabilizer and a film forming agent in a solvent B to prepare an impregnation solution B;
(3) soaking the filter paper in the soaking solution A for the first time, taking out and drying the filter paper, then placing the filter paper in the soaking solution B for the second time, taking out the filter paper, drying, cutting and pasting the filter paper on a substrate;
the color developing agent comprises thiomicone or a compound with an active structure similar to that of the thiomicone; the wetting agent is selected from nonionic fluorosurfactants, and the stabilizer is thioglycolic acid alkali metal salt.
Preferably, the pH adjusting agent is selected from solid organic acids. Further, the pH regulator is at least one selected from citric acid monohydrate, malic acid and oxalic acid. Furthermore, the pH value of the impregnation liquid A can be adjusted to be 2-6 by a pH regulator.
Preferably, the nonionic fluorocarbon surfactant is at least one selected from perfluorooctyl polyoxyethylene ether and perfluoroacrylate.
Preferably, the thioglycolic acid based alkali metal salt is at least one selected from sodium thioglycolate and potassium thioglycolate.
Preferably, the film forming agent is selected from water-soluble organic high molecular polymers. Further, the water-soluble organic high molecular polymer is at least one selected from sodium polyacrylate, gum arabic and polyethylene glycol.
Preferably, the solvent A is selected from one or more of methanol, ethanol, propanol and isopropanol; further preferably, the solvent a is selected from ethanol. The solvent B is selected from pure water.
Preferably, in the impregnation liquid A, the concentration of the color developing agent is 0.5 g/L-10 g/L, and the concentration of the pH regulator is 0.5 g/L-5 g/L; in the impregnation liquid B, the concentration of the wetting agent is 1.5 g/L-5 g/L, the concentration of the stabilizer is 5 g/L-20 g/L, and the concentration of the film forming agent is 1 g-5 g. Wherein, the concentration of the color developing agent can be but is not limited to 0.5g/L, 1g/L, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L and 10 g/L; the concentration of the pH regulator can be, but is not limited to, 0.5g/L, 1g/L, 2g/L, 3g/L, 4g/L, 5 g/L; the concentration of wetting agent can be, but is not limited to, 1.5g/L, 2g/L, 3g/L, 4g/L, 5 g/L; the concentration of the stabilizer can be, but is not limited to, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L, 10g/L, 11g/L, 12g/L, 13g/L, 14g/L, 15g/L, 16g/L, 17g/L, 18g/L, 19g/L, 20 g/L; the concentration of the film forming agent can be, but is not limited to, 1g/L, 2g/L, 3g/L, 4g/L, 5 g/L.
Preferably, the filter paper is selected from any one of chromatography filter paper, qualitative filter paper and quantitative filter paper. Further, the filter paper is chromatography filter paper.
Preferably, the time for the first soaking is 2min to 30min, for example, the time for the first soaking can be, but is not limited to, 2min, 4min, 6min, 8min, 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min, 30 min. Further, the time for the first soaking is 10 min.
Preferably, the time of the second soaking is 5s to 60s, for example, the time of the second soaking can be, but is not limited to, 5s, 10s, 15s, 20s, 25s, 30s, 35s, 40s, 45s, 50s, 55s, 60 s. Further, the time for the second soaking was 10 seconds.
Preferably, drying means vacuum drying at a temperature of not higher than 60 deg.C, oven drying to form, such as 50 deg.C, 40 deg.C, 30 deg.C.
Preferably, the cutting means cutting the filter paper to 25mm2～100mm2Such as, but not limited to, cutting the filter paper into 5mm by 5mm pieces.
Preferably, the substrate is a holdable base plate; the bottom plate is strip-shaped, the width is 5 mm-10 mm, the length is 50 mm-120 mm, and the bottom plate is made of a non-absorbent plastic plate, but is not limited to the above.
The method for rapidly determining total chlorine provided by the invention comprises the following steps: and (3) immersing the test paper for measuring the total chlorine into the sample to be measured, taking out the test paper after 4-9 seconds, comparing the color of the test paper with that of a standard color comparison card after the color is completely developed, and measuring the total chlorine content in the sample.
Preferably, the preparation method of the standard colorimetric card is as follows:
1) preparing total chlorine standard solutions with the concentrations of 0.10mg/L, 0.50mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 10.0mg/L and 20.0mg/L respectively by using pure water;
2) immersing the total chlorine test paper into each total chlorine standard solution, taking out after 4-9 seconds, and finding out a corresponding standard color on a pantone color card when the color is completely developed;
3) and preparing a standard colorimetric card according to the color value of each standard color.
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples. It should be noted that the following implementation of the method is a further explanation of the present invention, and should not be taken as a limitation of the present invention. The starting materials used in the examples are, unless otherwise specified, commercially available from conventional sources.
Example 1
A method for preparing a test paper for measuring total chlorine, comprising the steps of:
(1) preparing an impregnation liquid A containing 0.95g/L of thiomicrobile ketone and 1.8g/L of citric acid monohydrate by using absolute ethyl alcohol;
(2) preparing a steeping liquor B containing 12.5ml/L of perfluorooctyl polyoxyethylene ether fluorine surfactant (calculated by effective content of 20%), 3g/L of sodium thioglycolate and 4g/L of sodium polyacrylate by using pure water;
(3) completely soaking chromatographic filter paper in the impregnation liquid A for 10 minutes, taking out and drying at 55 ℃ under a vacuum condition; drying the chromatography filter paper, completely soaking the chromatography filter paper in the impregnation liquid B for 10 seconds, taking out the chromatography filter paper, and drying the chromatography filter paper at 55 ℃ under a vacuum condition. After drying the chromatography filter paper, cutting the filter paper into small pieces of 5 multiplied by 5mm, and adhering one end of a strip-shaped bottom plate of 5 multiplied by 75mm to prepare the test paper for measuring the total chlorine, which is called 1# test paper for short.
Example 2
A method for preparing a test paper for measuring total chlorine, comprising the steps of:
(1) preparing an impregnating solution A containing 2.5g/L of thiomizone and 2.0g/L of malic acid by using absolute ethyl alcohol;
(2) preparing a steeping liquor B containing 14ml/L of perfluoroacrylate fluorosurfactant (calculated by the effective content of 20 percent), 3.4g/L of potassium thioglycolate and 7.0g/L of gum arabic by using pure water;
(3) completely soaking chromatographic filter paper in the impregnation liquid A for 10 minutes, taking out and drying at 55 ℃ under a vacuum condition; drying the chromatography filter paper, completely soaking the chromatography filter paper in the impregnation liquid B for 10 seconds, taking out the chromatography filter paper, and drying the chromatography filter paper at 55 ℃ under a vacuum condition. After drying the chromatography filter paper, cutting the filter paper into small pieces of 5 multiplied by 5mm, and adhering one end of a strip-shaped bottom plate of 5 multiplied by 75mm to prepare the test paper for measuring the total chlorine, which is called 2# test paper for short.
Example 3
A method for preparing a test paper for measuring total chlorine, comprising the steps of:
(1) preparing a steeping liquor A containing 4.0g/L of thiomicrobile ketone and 0.8g/L of sulfamic acid by using absolute ethyl alcohol;
(2) preparing a steeping fluid B containing 18ml/L of perfluoroacrylate fluorosurfactant (calculated by the effective content of 20 percent), 3.4g/L of potassium thioglycolate and 10g/L of polyethylene glycol by using pure water;
(3) completely soaking chromatographic filter paper in the impregnation liquid A for 10 minutes, taking out and drying at 55 ℃ under a vacuum condition; drying the chromatography filter paper, completely soaking the chromatography filter paper in the impregnation liquid B for 10 seconds, taking out the chromatography filter paper, and drying the chromatography filter paper at 55 ℃ under a vacuum condition. After drying the chromatography filter paper, cutting the filter paper into small pieces of 5 multiplied by 5mm, and adhering one end of a strip-shaped bottom plate of 5 multiplied by 75mm to prepare the test paper for measuring the total chlorine, which is called 3# test paper for short.
Examples of Standard color cards
A standard colorimetric card 1# was prepared for use in combination with test paper for total chlorine (test paper No. 1).
1) Preparing a total hydrochloric acid standard solution with the concentration of 0.10mg/L by using pure water, immersing the test paper No. 1 prepared in the example 1 into the solution, taking out the test paper after 5 seconds, throwing off redundant solution, and finding out a standard color with consistent hue on a pantone color card according to the color presented by the test paper;
2) adopting the method in the step 1) to respectively obtain standard colors presented by the test paper when detecting total chlorine standard solutions with the concentrations of 0.50mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 10.0mg/L and 20.0 mg/L;
3) and (3) performing color mixing and printing by using a computer according to the color values listed in the obtained pantone standard colors to obtain a standard color comparison card 1#, wherein the color values are shown in a table 1.
TABLE 1 Standard color card 1#
Referring to Table 1, the pantone color numbers of the total chlorine standard solutions with concentrations of 0.10mg/L, 0.50mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 10.0mg/L and 20.0mg/L in the standard colorimetric card 1# are 617CP, 7766CP, 384CP, 5757CP, 370C, 348CP, 342CP and 7708CP, respectively.
The standard colorimetric cards 2# to 3# which are matched with the test paper 2# to 3# can be prepared respectively by the same method.
Test example 1
And (3) placing the No. 1-3 test paper in a compact bag, placing the compact bag in a 37 ℃ oven, observing the appearance of the test paper every 30 days, and carrying out test on the stability and the color development effect of the test paper.
The color development effect test method comprises the following steps: 0.10mg/L, 0.50mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 7.0mg/L, 10.0mg/L and 20.0mg/L of total chlorine standard solution are prepared respectively. And (3) respectively inserting the No. 1 test paper, the No. 2 test paper and the No. 3 test paper into the standard solution, taking out after 5 seconds, throwing off redundant solution on the test paper, observing the color development effect after complete color development, and respectively contrasting with a matched standard colorimetric card to obtain total chlorine data. As the total chlorine content increased, the color developed by the test paper changed from yellow to light green and then to green. The detection results are shown in tables 2 to 4.
Table 21 # stability test paper
| Test index | Standing for 30 days | Standing for 60 days | Standing for 120 days |
| Appearance of the product | Yellow colour | Yellow colour | Yellow colour |
| Color scale | Is obvious | Is obvious | Is obvious |
| Color development response time | Color development is completed within 5 seconds | Color development is completed within 5 seconds | Color development is completed within 6 seconds |
Table 32 # stability test paper
| Test index | Standing for 30 days | Standing for 60 days | Standing for 120 days |
| Appearance of the product | Yellow colour | Yellow colour | Yellow colour |
| Color scale | Is obvious | Is obvious | Is obvious |
| Color development response time | Color development is completed within 5 seconds | Color development is completed within 5 seconds | Color development is completed within 6 seconds |
Table 43 # stability test paper
| Test index | Standing for 30 days | Standing for 60 days | Standing for 120 days |
| Appearance of the product | Yellow colour | Yellow colour | Yellow colour |
| Color scale | Is obvious | Is obvious | Is obvious |
| Color development response time | Color development is completed within 5 seconds | Color development is completed within 5 seconds | Color development is completed within 5 seconds |
From the test results in tables 2 to 4, it is clear that the response time of the test paper # 1, the test paper # 2 and the test paper # 3 is within 6 seconds, and the color can be stabilized for 30 minutes after the color development is completed.
As shown in tables 2 to 4, after the test paper No. 1, the test paper No. 2 and the test paper No. 3 are placed in an oven at 37 ℃ for 120 days, the color development response time speed is slightly slowed, the influence on the other test paper is avoided, and the shelf life at normal temperature is greatly prolonged.
Test example 2
A total chlorine-containing water sample was tested using the test paper # 1 prepared in example 1 and compared with the results of the colorimeter. And when the color tone of the developed sample is consistent with the standard color gradation, directly taking the color gradation indicating concentration as a measured value, and if the color depth is between the two color gradations, taking the middle concentration of the two color gradation indicating concentrations as the measured value. The colorimeter method is to use the color development principle of the national standard DPD method, measure specific numerical values on the colorimeter after color development, and finally carry out standard addition verification.
The actual sample test results are shown in table 5. In table 5: sample 1 is the terminal water of a guest room of a hotel in Guangzhou; sample 2 is swimming pool water in a hotel in Guangzhou; sample 3 is the pool water of the immersion foot of a swimming pool in a certain community; sample 4 is a sterilized water sample for a food processing plant.
TABLE 5 actual sample testing and comparative experiments with other methods
The test results in table 5 show that the test paper prepared by the invention is used for measuring the total chlorine concentration, and the detection method does not need other instruments and accessories, is simple and convenient to operate, has high detection sensitivity, wide detection range and reliable results, has higher practical value, and is suitable for detecting the total chlorine concentration in the disinfection process of various scenes.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it is not limited to the embodiments, and those skilled in the art should understand that the technical solutions of the present invention can be modified or substituted with equivalents without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method for preparing test paper for measuring total chlorine is characterized by comprising the following steps:
(1) dissolving a color developing agent and a pH regulator in a solvent A to prepare a steeping liquor A;
(2) dissolving a wetting agent, a stabilizer and a film forming agent in a solvent B to prepare an impregnation solution B;
(3) soaking filter paper in the soaking solution A for the first time, taking out and drying the filter paper, then placing the filter paper in the soaking solution B for the second time, taking out, drying, cutting and pasting the filter paper on a substrate;
the color developing agent comprises thiomicone or a compound with an active structure similar to that of the thiomicone; the wetting agent is selected from nonionic fluorosurfactants; the stabilizer is thioglycollic acid alkali metal salt.
2. The method of preparing test paper for total chlorine according to claim 1, wherein the pH adjusting agent is selected from solid organic acids.
3. The method of preparing test paper for total chlorine according to claim 1, wherein the non-ionic fluorocarbon surfactant is at least one selected from perfluorooctylpolyoxyethylene ether and perfluoroacrylate.
4. The method of producing test paper for total chlorine according to claim 1, wherein the alkali thioglycolate salt is at least one selected from the group consisting of sodium thioglycolate and potassium thioglycolate.
5. The method of producing test paper for total chlorine according to claim 1, wherein the film-forming agent is selected from water-soluble organic high molecular polymers.
6. The method for preparing test paper for the determination of total chlorine according to claim 1, wherein the solvent A is selected from one or more of methanol, ethanol, propanol and isopropanol; the solvent B is selected from pure water.
7. The method of manufacturing test paper for total chlorine according to claim 1, wherein the concentration of the color-developing agent in the impregnation liquid a is 0.5 to 10g/L, and the concentration of the pH adjuster is 0.5 to 5 g/L; in the impregnation liquid B, the concentration of the wetting agent is 1.5 g/L-5 g/L, the concentration of the stabilizer is 5 g/L-20 g/L, and the concentration of the film forming agent is 1 g-5 g.
8. The method for preparing test paper for the determination of total chlorine according to claim 1, wherein the time for the first soaking is 2min to 30 min; the time of the second soaking is 5-60 s.
9. A test paper for total chlorine measurement, which is produced by the production method according to any one of claims 1 to 8.
10. A method for rapidly determining total chlorine, characterized in that the test paper for total chlorine according to claim 9 is immersed in a sample to be determined, taken out after 4 to 9 seconds, and after the color development is completed, the test paper is compared with a standard color chart in color to determine the total chlorine content in the sample.
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| CN117538318A (en) * | 2024-01-10 | 2024-02-09 | 山东利尔康医疗科技股份有限公司 | Residual peracetic acid test card and preparation method thereof |
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