CN105445265B - The preparation method of permanent chlorine residue standard colorimetric serial solution - Google Patents
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Abstract
A kind of preparation method of permanent chlorine residue standard colorimetric serial solution, it includes selection chlorine residual measurement instrument, it prepares and compares solution, it prepares chlorine residue standard colorimetric serial solution mother liquor and prepares chlorine residue standard colorimetric serial solution, the present invention provides a kind of preparation method of permanent chlorine residue standard colorimetric serial solution, the permanent chlorine residue standard colorimetric serial solution prepared, for N, the calibration of instrument or direct visual colorimetric determination measure when N diethyl Isosorbide-5-Nitrae phenylenediamines spectrophotometry measures free chlorine and total chlorine.The tedious steps that repetition prepares chlorine residue standard solution are eliminated, which prepares once, can be used for a long time.
Description
Technical field
The invention belongs to elemental analysis auxiliary material technical fields, are exactly specifically to be related to a kind of permanent chlorine residue mark
The preparation method of quasi- colorimetric serial solution, available for N, N- diethyl-Isosorbide-5-Nitraes-phenylenediamine spectrophotometry measures free chlorine and total
The calibration of instrument or direct visual colorimetric determination measure during chlorine.
Background technology
Chlorine residue is also known as free chlorine residual or active free chlorine or potential free chlorine, with hypochlorous acid, hypochlorite ion and list
The form of matter chlorine is present in water body, total chlorine is also known as total residual chlorine, i.e. the combined chlorines such as free chlorine residual and chloramines, organochlorine amine
General name.After chlorine is added to the water with simple substance or chloric acid salt form, through hydrolysis generate free chlorine, including aqueous mol-chloric, hypochlorous acid and
The forms such as hypochlorite ion, relative scale is decided by the pH and temperature of water, under the pH of general water body, mainly secondary chlorine
Acid and hypochlorite ion.Free chlorine residual reacts with ammonium and certain nitrogenous compounds, generates combined chlorine.Chlorine reacts generation with ammonium
Chloramines：Monochloro amine, dichlormaine and tri-chlorination amine.Both free chlorine residual and combined chlorine can be existed simultaneously in water.Through chlorination
The water outlet of sewage and certain industrial wastewaters, usually containing only combined chlorine.
The source of chlorine is mainly that chlorination is to kill or inhibit microorganism in drinking water or sewage in water, chlorination in electroplating wastewater
Decompose toxic cyanide.The adverse effect that chlorination generates is that the water containing phenol can be made to generate chlorophenol, can also generate organochlorine
Compound, it is extremely harmful to human body, and can be because there are generate illeffects to certain aquatic organisms during combined chlorine.
Therefore, it is necessary to monitor the content of chlorine residue and total chlorine in water-outlet body, the detection method of chlorine residue and total chlorine has at present：Iodine number
Method, N, N- diethyl -1,4- phenylenediamines ferrous ammonium sulfate titration and N, N- diethyl -1,4- phenylenediamine spectrophotometry.Its
In, the principle that N, N- diethyl-Isosorbide-5-Nitrae-phenylenediamine spectrophotometry measure chlorine residue is：Under the conditions of pH is 6.2~6.5, with trip
It directly reacts from chlorine standard solution with N, N- diethyl-Isosorbide-5-Nitrae-phenylenediamine, generates red compound, under 515nm wavelength,
Its absorbance is measured using spectrophotometry, measures chlorine residue.N, N- diethyl -1,4- phenylenediamines spectrophotometry measure total chlorine
Principle is：In pH under the conditions of 6.2~6.5, there are during excessive potassium iodide, simple substance chlorine, hypochlorous acid, hypochlorite and chloramines with
N, N- diethyl-Isosorbide-5-Nitrae-phenylenediamine react, and generate red compound, under 515nm wavelength, are measured using spectrophotometry
Its absorbance measures total chlorine.
But free chlorine standard solution is unstable and is not easy to obtain, and free chlorine and total chlorine and N, N- diethyl-Isosorbide-5-Nitrae-
Phenylenediamine react generation red compound it is unstable, it is impossible to persistence, every time measure when be both needed to prepare standard again
Solution draws standard curve or calibration instrument.
Invention content
During the purpose of the present invention is being directed to the content of chlorine residue and total chlorine in existing monitoring water body, free chlorine standard solution is not
Stablize and be not easy the technological deficiency obtained, a kind of preparation method of permanent chlorine residue standard colorimetric serial solution is provided, prepare
Permanent chlorine residue standard colorimetric serial solution, for N, N- diethyl-Isosorbide-5-Nitraes-phenylenediamine spectrophotometry measure free chlorine and
The calibration of instrument or direct visual colorimetric determination measure during total chlorine.The tedious steps that repetition prepares chlorine residue standard solution are eliminated, this is molten
Liquid is prepared once, can be used for a long time.
Technical solution
In order to realize above-mentioned technical purpose, the preparation of a kind of permanent chlorine residue standard colorimetric serial solution that the present invention designs
Method, it is characterised in that, it includes following steps：
First, a chlorine residual measurement instrument is selected；
Then, it prepares and compares solution：It prepares chlorine residual measurement instrument and measures the corresponding chlorine residue standard solution of the upper limit, and by specification
It is required that being measured after addition chlorine residue chromogenic reagent, its millivolt of value is recorded, duplicate measurements three times, calculates average valueIn this, as
Compare the standard value of solution；
Then, chlorine residue standard colorimetric serial solution mother liquor is prepared：Appropriate rose element is taken to be dissolved in pure water, treats pigment
Millivolt value all is measured after dissolving and mixing, if more than average valuePigment is then added, if less than average valueIt then adds pure
Water is so adjusted repeatedly, and the millivolt value of pigment solution is made to existmV.It is molten using this solution as chlorine residue standard colorimetric series
Liquid mother liquor；
Finally, chlorine residue standard colorimetric serial solution is prepared：As needed, by chlorine residue standard colorimetric serial solution mother liquor press than
Example dilution prepares each concentration chlorine residue standard colorimetric serial solution, is kept in dark place in 4 DEG C of refrigerators.
Further, chlorine residual measurement instrument can directly read mV values in the first step.
Advantageous effect
The present invention provides a kind of preparation method of permanent chlorine residue standard colorimetric serial solution, the permanent chlorine residue prepared
Standard colorimetric serial solution, for N, instrument when N- diethyl-Isosorbide-5-Nitraes-phenylenediamine spectrophotometry measures free chlorine and total chlorine
Calibration or directly visual colorimetric determination measurement.The tedious steps that repetition prepares chlorine residue standard solution are eliminated, which prepares once, can
It is used for a long time.
Specific embodiment
With reference to embodiment, the present invention will be further described.
Embodiment
The first step, selection can directly read the portable chlorine residual measurement instrument of mV values.
Second step, prepares and compares solution, and detailed process is：
(1) 1.006g/L potassium iodate solutions are prepared
Top pure grade Potassiumiodate (drying 2h at 120 DEG C~140 DEG C in advance) 1.006g accurately is weighed, it is soluble in water, it moves into
In 1000mL volumetric flasks, graticule, mixing are added water to.
(2) 100.00mg/L Cl are prepared2Stoichiometric standard solution
The accurate 1.006g/L potassium iodate solutions for drawing 100.0mL add water to graticule in 1000mL brown volumetric flasks, mix
It is even.Face with now matching.
(3) 5.00mg/L Cl are prepared2Stoichiometric standard solution
The accurate 100.00mg/L Cl for drawing 50.0mL2Stoichiometric standard solution adds in about in 1000mL brown volumetric flasks
1g potassium iodide adds in 1.0mL 1.0mol/L sulfuric acid solutions, and after 1min, the 1.0mol/L NaOH that 1mL is added in into volumetric flask are molten
Liquid, adds water to graticule, mixing, faces with now matching.
(4) prepare color developing agent
The matching used chlorine residue color developing agent of chlorine residual measurement instrument measures one parcel of addition every time.
(5) it prepares and compares solution
Draw 10mL 5.00mg/L Cl2In stoichiometric standard solution to colorimetric cylinder, a packet color developing agent is added in, screws colorimetric cylinder
Lid, rocks colorimetric cylinder, and after color developing agent dissolving, turn upside down colorimetric cylinder, eliminates the bubble adhered on colour developing tube wall, is put into colorimetric
Chi Zhong covers shading cover, records millivolt value, and repeated measurement three times, calculates average value, is denoted as
Third walks, and prepares chlorine residue standard colorimetric serial solution mother liquor
Rose element is gradually dissolved in about 60mL pure water, pigment all dissolves and millivolt value is measured after mixing, if
It is more thanPigment is then added, if being less thanThen add pure water.It so adjusts, the millivolt value of pigment solution is made to existIn the least
Volt.
4th step prepares permanent chlorine residue standard colorimetric serial solution
According to the form below accurately pipettes 5.00mg/L Cl2Equivalent pigment solution and pure water screw colorimetric cylinder lid in colorimetric cylinder,
It is kept in dark place after mixing in 4 DEG C of refrigerators.
If need the Cl of other concentration (being set as C mg/L)2Equivalent pigment solution then accurately pipettes 5.00mg/L Cl2Equivalent color
Plain solution 2C mL and pure water (10-2C) mL are prepared in colorimetric cylinder.
It needs, in use, by pigment serial solution after refrigerator taking-up, to restore to room temperature, shake up before measurement, and dry ratio
The steam of colour tube surface attachment.With the chlorine residue standard colorimetric solution of respective concentration, without adding other reagents such as color developing agent, directly
It is demarcated or visual colorimetric determination measures.
The present invention provides a kind of preparation method of permanent chlorine residue standard colorimetric serial solution, the permanent chlorine residue prepared
Standard colorimetric serial solution, for N, instrument when N- diethyl-Isosorbide-5-Nitraes-phenylenediamine spectrophotometry measures free chlorine and total chlorine
Calibration or directly visual colorimetric determination measurement.The tedious steps that repetition prepares chlorine residue standard solution are eliminated, which prepares once, can
It is used for a long time.
Claims (2)
1. a kind of preparation method of permanent chlorine residue standard colorimetric serial solution, it is characterised in that, it includes following steps：
(a) chlorine residual measurement instrument is selected；
(b) it prepares and compares solution：It prepares chlorine residual measurement instrument and measures the corresponding chlorine residue standard solution of the upper limit, and by specification requires to add
It is measured after adding chlorine residue chromogenic reagent, records its millivolt of value, duplicate measurements three times, calculates average valueIt is molten in this, as comparing
The standard value of liquid；
(c) chlorine residue standard colorimetric serial solution mother liquor is prepared：Appropriate rose element is taken to be dissolved in pure water, treats that pigment is all molten
It solves and millivolt value is measured after mixing, if more than average valuePigment is then added, if less than average valuePure water is then added, so
It adjusts repeatedly, the millivolt value of pigment solution is made to existMillivolt, it is female using this solution as chlorine residue standard colorimetric serial solution
Liquid；
(d) chlorine residue standard colorimetric serial solution is prepared：As needed, it is diluted in proportion by chlorine residue standard colorimetric serial solution mother liquor
Each concentration chlorine residue standard colorimetric serial solution is prepared, is kept in dark place in 4 DEG C of refrigerators.
2. a kind of preparation method of permanent chlorine residue standard colorimetric serial solution as described in claim 1, it is characterised in that：Institute
Millivolt value can be directly read by stating chlorine residual measurement instrument in step (a).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067739A (en) * | 1992-04-07 | 1993-01-06 | 山东省卫生防疫站 | Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water |
| CN101592612A (en) * | 2008-05-26 | 2009-12-02 | 刘侠 | Test paper for rapidly checking residual content of sterilizing agent |
| CN103293121A (en) * | 2013-05-29 | 2013-09-11 | 上海市计量测试技术研究院 | Residual chlorine standard substance, application of residual chlorine standard substance and residual chlorine tester correction or calibration method |
-
2015
- 2015-12-03 CN CN201510884896.9A patent/CN105445265B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067739A (en) * | 1992-04-07 | 1993-01-06 | 山东省卫生防疫站 | Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water |
| CN101592612A (en) * | 2008-05-26 | 2009-12-02 | 刘侠 | Test paper for rapidly checking residual content of sterilizing agent |
| CN103293121A (en) * | 2013-05-29 | 2013-09-11 | 上海市计量测试技术研究院 | Residual chlorine standard substance, application of residual chlorine standard substance and residual chlorine tester correction or calibration method |
Non-Patent Citations (5)
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| 37 余氯;中华人民共和国卫生部;《中华人民共和国国家标准GB5750-85》;19861001;第96-100页 * |
| DPD余氯比色器的研制;王少松等;《环境科学》;19860302;第7卷(第1期);一、DPD永久比色的研制与稳定性观察 * |
| TMB法测定水源水及饮用水中余氯;冯海涛等;《中国卫生工程学》;20030228;第2卷(第1期);全文 * |
| 医院污水余氯量简易测定方法探讨;胡玉芬等;《浙江预防医学》;20040108;第14卷(第5期);全文 * |
| 水中余氯现场快速测定方法研究;王静斌等;《环境污染与防治》;20020830;第24卷(第4期);全文 * |
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