CN102692386A - Detection method and colorimetric detection device for high-concentration chlorine dioxide - Google Patents
Detection method and colorimetric detection device for high-concentration chlorine dioxide Download PDFInfo
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- CN102692386A CN102692386A CN2012101576118A CN201210157611A CN102692386A CN 102692386 A CN102692386 A CN 102692386A CN 2012101576118 A CN2012101576118 A CN 2012101576118A CN 201210157611 A CN201210157611 A CN 201210157611A CN 102692386 A CN102692386 A CN 102692386A
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Abstract
The invention discloses a detection method and a colorimetric detection device for high-concentration chlorine dioxide. The detection method includes: placing a sample to be tested in a colorimetric bottle, sealing the colorimetric bottle, using an LED with 440-450nm center wavelength as a single-color light source to emit light passing through the sample to be tested, which contains chlorine dioxide; and detecting energy of the light passing through the sample to be tested, and calculating to obtain concentration value of ClO2. By the detection method and the colorimetric detection device, the technical problem that measurement of chlorine dioxide concentration has great errors as existing measuring methods need dilution when the concentration of the chlorine dioxide is higher than 250mg/L is solved. The detection method consumes no extra reagents and allows for quick, accurate and dilution-free measurement of high-concentration chlorine dioxide content on the site.
Description
Technical field
The present invention relates to a kind of high concentration of chlorine dioxide detection method and colour comparison detection apparatus thereof.
Background technology
Chlorine dioxide (ClO
2) be the new disinfectant of generally acknowledging at present efficient, wide spectrum in the world and belonging to the A1 level security, be widely used in fields such as drinking water disinfection, food safety control, medical apparatus sterilizing.Because the ClO of high concentration
2Solution is very unstable, and commercially available stable ClO 2 solution is not ClO truly
2, but itself does not possess the chlorite of sterilizing function, need add active agent during use and just can discharge the ClO with high-effective disinfecting bactericidal action
2Stipulated ClO among the new standard GB 26366-2010 " disinfection agent of chlorine dioxide hygienic standard "
2Sanitizer is applied in the activity in each field: be low to moderate 1mg/L～2mg/L, and high to 400mg/L～600mg/L.In order better to guarantee ClO
2Disinfection effect, ClO
2The research of concentration detection method receives people's attention day by day.
Owing to be dissolved in the volatile decomposition of chlorine dioxide in the water, if fail in time to detect its concentration, along with the prolongation of time, the accuracy of testing result must be difficult to guarantee that this just requires ClO
2Detection method not only to possess accurately, sensitive characteristics, also must be quick as much as possible, shorten analytical cycle, realize monitoring in real time, in time feed intake, reach best Disinfection Effect.
Low concentration ClO
2The test laboratory method mainly contains the DPD AAS, and existing in the market various low concentration chlorine dioxide tintmeter based on DPD development process principles can be tested 5.0mg/L with interior ClO
2Concentration, this series products has obtained promotion and application in numerous enterprises and superintendent office.
High concentration ClO
2That adopts among the laboratory method GB 26366-2010 of test mainly contains five step iodimetric titration and ultraviolet-visible spectrophotometries.Wherein five step iodimetric titration need be gathered sample three times, and substep determines ClO in the solution
2, Cl
2, ClO
2 -, ClO
3 -The concentration of each material, operating process is very loaded down with trivial details, and measuring accuracy and repeatability are difficult to guarantee, are inappropriate for high concentration ClO
2Real-time monitoring.
Ultraviolet-visible spectrophotometry utilizes ClO
2The yellow green of itself has to absorb at visible region directly measures ClO
2Concentration, ClO
2Peak absorbtivity wavelength at 359nm, but this place can compatible Cl
2, ClO
2 -, ClO
3 -Deng material absorption is arranged all, adopt wavelength 430nm can eliminate interference basically, testing range is 10mg/L～250mg/L.This method of testing is relatively simple, but need use large-scale spectrophotometer, also is not suitable for grass-roots unit and enterprise and monitors ClO in real time
2Concentration.
High concentration ClO
2Solution can see generally that in dilution tangible aerosol produces, and loss is fairly obvious, and chlorine dioxide concentration is high more, and dilution error is big more.The ClO that adopts 10 times of iodimetric titration and ultraviolet-visible spectrophotometry dilutions to measure concentration near 1000mg/L
2Sample, dilution error reaches 20%.And dilution need be used a series of devices and article such as transfer pipet, Liquid absorption ball, volumetric flask, pure water, wash bottle, needs the tester of specialty could accurately dilute operation, and is very unfavorable to on-site measurement.So high concentration ClO
2The direct determination method that need not to dilute is preferably adopted in on-site measurement.Also there is not this series products in the market; What the disclosed portable instanteanous tester for concentration of chlorine dioxide solution of CN101806721A adopted is GB 26366-2010 spectrophotometric principles; Wavelength is all consistent with GB 26366-2010 with testing range; So measure again after being higher than 250mg/L and need diluting, be unfavorable for high concentration ClO in theory
2Mensuration.
Summary of the invention
The object of the present invention is to provide a kind of additional agents that need not to consume, can be at the scene accurately, fast, the high concentration of chlorine dioxide detection method that need not to dilute and the colorimetric device of realizing this method.
The technical scheme that the present invention taked is:
A kind of high concentration of chlorine dioxide detection method may further comprise the steps:
1) testing sample placed in the colorimetric bottle seal, use centre wavelength as the LED of 440nm～450nm as monochromatic source, through testing sample solution;
2) detection light source calculates the concentration of chlorine dioxide in the sample through the luminous energy behind the testing sample solution.
Preferably, the centre wavelength of monochromatic source is the LED of 445nm, and the emission half-angle of LED is 4 °～15 °.
A kind of high concentration of chlorine dioxide colorimetric device; Comprise monochromatic source, cell, colorimetric bottle, monochromatic source adopts the LED of centre wavelength 440nm～450nm, and the emission half-angle of LED is 4 °～15 °; Place the colorimetric bottle of cell to have gland bonnet, the diameter of colorimetric bottle is 16mm～28mm.
Further, the inwall of cell is provided with positioning mark, the colorimetric bottle wall be provided with the cell inwall on the telltale mark that is complementary of positioning mark.
Further, the bottom of gland bonnet is provided with sealing rubber ring, and sealing rubber ring and sample surface of contact are provided with anticorrosive coat.
Further, cell inwall both sides are provided with the screens that is used for fixing colorimetric bottle.
Further, screens is the wire projection.
The invention has the beneficial effects as follows:
The inventive method has overcome that chlorine dioxide concentration is higher than 250mg/L in the existing assay method; Need dilute that to cause measuring the result inaccurate; Error is bigger than normal and be not suitable for the technical matters of on-site measurement, and the mensuration concentration range 10mg/L～250mg/L of prior art is widened to 10mg/L～1000mg/L, does not need additive decrementation reagent; Can be on-the-spot accurately and fast, measure the concentration of chlorine dioxide, need not to dilute the concentration that can accurately measure high concentration of chlorine dioxide.
Based on the inventive method, through the LED and the colorimetric bottle of existing tintmeter are simply adjusted, colorimetric device that can accomplished this method.
Through positioning mark is set, can conveniently confirm sample size, also help avoiding colorimetric bottle is misplaced simultaneously, reduced operate miss effectively.
Through sealing rubber ring and anticorrosive coat are set, can improve the leakproofness of colorimetric bottle greatly, and prolong its serviceable life, help to measure more exactly high concentration of chlorine dioxide, be higher than the concentration of 250mg/L like content.
Through screens is set, can guarantee that the position of colorimetric bottle is accurate, guarantee the accuracy of testing result.
Description of drawings
Fig. 1: the casing surface structure synoptic diagram of high concentration of chlorine dioxide colorimetric device of the present invention.
Fig. 2: the structural representation that the detachable shading cover among Fig. 1 is taken apart.
Fig. 3: the interior structural representation of high concentration of chlorine dioxide colorimetric device of the present invention.
Fig. 4: the colorimetric bottle structural representation of high concentration of chlorine dioxide colorimetric device of the present invention.
Embodiment
Common ClO
2Use in the liquid except ClO
2Can not exist visible region that the material of absorption is arranged outward, the inventor improves on the basis of National Standard Method, and the test peak wavelength is extended to the less 440nm～450nm of absorption intensity by 430nm, so not only can eliminate Cl fully
2, ClO
2 -, ClO
3 -Deng the interference of material, also widen testing range greatly to 10mg/L～1000mg/L.Can need not dilution, the actual concentration accurate at the scene, that the fast measuring chlorine dioxide uses solution, the assurance disinfection agent of chlorine dioxide is realized adding through concentration monitor when constantly consuming in good time, with the dynamic stability of maintenance concentration.
A kind of high concentration of chlorine dioxide detection method may further comprise the steps:
1) testing sample placed in the colorimetric bottle seal, use centre wavelength as the LED of 440nm～450nm as monochromatic source, through testing sample solution;
2) detection light source calculates the concentration of chlorine dioxide in the sample through the luminous energy behind the testing sample solution.
Preferably, the centre wavelength of monochromatic source is the LED of 445nm, and the emission half-angle of LED is 4 °～15 °.
Below in conjunction with accompanying drawing and embodiment the present invention is described further:
With reference to Fig. 1～4, a kind of high concentration of chlorine dioxide colorimetric device comprises the casing 1 of sealing, and the casing surface is provided with zeroing button 3, reading button 4, power switch 5, data cutout screen 2 and dismountable shading cover 6; Corresponding position at detachable shading cover 6 is fixed with a cell 7; Cell 7 between monochromatic source 8 and photoelectric sensor 9, cell 7 built-in colorimetric bottles 12 that have gland bonnet 13 wherein, and photoelectric sensor 9, microprocessor 10 and data cutout screen 2 interconnect successively; In addition; Also be provided with respectively at power switch 5 photoelectric sensor 9, microprocessor 10 and data cutout screen 2 interconnective batteries 11 in the casing; Monochromatic source 8 adopts the LED of centre wavelength 440nm～450nm, and the emission half-angle of LED is 4 °～15 °.
Monochromatic source 8 preferred employing centre wavelengths are the LED of 445nm; Spectrum width is preferably ± 5nm, and the emission half-angle of LED is preferably 4 °～15 °, and the LED emission angle is more little in theory; Energy is concentrated more; Help widening of testing range more, but absolute linear light source is difficult to realize that the minimum emission half-angle of the LED that can find on the market at present is 4 °.Angle is too big, will cause the energy of light beam too to disperse, even the light that sees through of part is dispersed to and can not be received by photoelectric sensor, causes the loss of luminous energy, possibly shorten testing range.
The bottom that gland bonnet 13 is preferably lid is bonded with caulking gum, is bonded with one deck anticorrosive on the sample surface of contact of preferred caulking gum, like anti-corrosion materials such as teflon.
Colorimetric bottle 12 is preferably optical glass bottle or the round thread mouth bottle that other printing opacity resistant material is processed of the screw thread mouth of diameter 16mm～28mm.The height of colorimetric bottle 12 should be complementary with the height of cell 7 with detachable shading cover 6.
The size of colorimetric bottle 12 diameters is represented the size of light beam average light path when the sample, and testing sample causes the light absorption degree varies of different wave length, for fixing testing range, selects the LED of different centre wavelengths should mate the colorimetric bottle of suitable diameter.
Photoelectric sensor 9 is the sensitive components that can light signal converted into electric signal and have certain range and resolution, and the resolution of this photoelectric sensor is preferably ClO in the testing sample
2Concentration is 1mg/L.
Microprocessor 10 is the data processors on the single-chip microcomputer, is used for the detection signal of photoelectric sensor is carried out data processing.According to detection signal and ClO
2The correlativity matched curve of concentration of standard solution adopts integrated digital filtering, curve fitting algorithm to carry out the calculating of sample concentration.Said data processor is provided with reasonable calibration point, preferred zero point or certain concentration point.ClO
2Standard solution adopts freshly prepd pure ClO
2Solution adopts conventional iodimetric titration to demarcate ClO
2Concentration.
Embodiment one:
Method according to the pure ClO 2 solution of preparation among the GB 26366-2010 prepares the pure solution of high concentration of chlorine dioxide, demarcates with conventional iodimetric titration; Adopt high concentration of chlorine dioxide colorimetric device of the present invention to carry out high concentration of chlorine dioxide simultaneously and directly detect, detection method is following:
1) opens colorimetric device power switch 5, take away shading cover 6;
2) distilled water being added internal diameter is colorimetric bottle 12 to the scale mark sign of 16mm more than 17, and screwing hermetic lid 13 is made as blank bottle;
3) the blank bottle is placed in the cell 7, the telltale mark 14 of blank bottle outer wall is corresponding with the positioning mark 15 of colorimetric notch, and making centre wavelength is 440nm, and the emission half-angle is that the light beam that 5 ° LED 8 launches passes through colorimetric bottle 12;
4) cover shading cover 6,, open shading cover 6, take out blank bottle by 3 zeroings of " zeroing " key;
5) testing sample is added in the colorimetric bottle 12 of another same size to scale mark sign more than 17, screwing hermetic lid 13 is sample bottle;
6) sample bottle is placed in the cell 7, the telltale mark 14 of blank bottle outer wall is corresponding with the positioning mark 15 of colorimetric notch, and making centre wavelength is 440nm, and the emission half-angle is that the light beam that 5 ° LED 8 launches passes through colorimetric bottle 12;
7) cover shading cover 6, by " reading " key 4 readings.
Determination data is as shown in the table:
Table 1: the high concentration of chlorine dioxide colorimetric device is measured chlorine dioxide concentration
Embodiment two:
Method according to the pure ClO 2 solution of preparation among the GB 26366-2010 prepares the pure solution of high concentration of chlorine dioxide, demarcates with conventional iodimetric titration; Adopt one of high concentration of chlorine dioxide tintmeter of the present invention to carry out high concentration of chlorine dioxide simultaneously and directly detect, detection method is with embodiment 1, and difference is that the centre wavelength of LED is 445nm, and the emission half-angle is 8 °.
Determination data is as shown in the table:
Table 2: the high concentration of chlorine dioxide colorimetric device is measured chlorine dioxide concentration
Embodiment three:
According to the pure solution of method preparation standard high concentration of chlorine dioxide of the pure ClO 2 solution of preparation among the GB 26366-2010, demarcate with conventional iodimetric titration; Adopt one of high concentration of chlorine dioxide tintmeter of the present invention to carry out high concentration of chlorine dioxide simultaneously and directly detect, detection method is with embodiment 1, and difference is that the centre wavelength of LED is 450nm, and the emission half-angle is 15 °.
Determination data is as shown in the table:
Table 3: the high concentration of chlorine dioxide colorimetric device is measured chlorine dioxide concentration
Table 1～table 3 data show, the chlorine dioxide that three kinds of high concentration of chlorine dioxide detection methods described in the embodiment and colorimetric device thereof can directly carry out high concentration detects, and the testing range of colorimetric device is 10-1000mg/L.Each method all has tests collimation and test accuracy preferably, and the test error basic controlling is in ± 5%.Wherein, less with the detection method and the device mensuration chlorine dioxide concentration relative error that provide among the embodiment two especially, be fit to the chlorine dioxide mensuration that concentration is higher than 250mg/L more.
Comparative Examples 1:
It is following to adopt ultraviolet spectrophotometry to detect the high concentration of chlorine dioxide step:
1) concentration is higher than the ClO of 250mg/L
2Pure solution adopts conventional iodimetric titration to demarcate concentration, dilutes 2 times, 5 times, 10 times more respectively.
2) adopt UV/1800 (day island proper Tianjin) ultraviolet-visible pectrophotometer, under wavelength 430nm, adopt the 1cm cuvette to measure the absorbance of dilution.
3) absorbance and the typical curve of concentration relationship: the A=0.0022C (A is an absorbance, and C is chlorine dioxide concentration (mg/L)) that obtain according to experiment
4) calculate diluent concentration, it is following to measure the result:
Table 4 ultraviolet spectrophotometry chlorine dioxide concentration
Comparative Examples 2:
With the ClO of concentration greater than 250mg/L
2Pure solution dilutes 2 times, 5 times, 10 times respectively, and stoste and dilution all adopt conventional iodometric determination ClO
2Concentration, it is following to measure the result:
Table 5: iodometric determination chlorine dioxide concentration
Table 4 and table 5 test figure show no matter take which kind of method, as long as carry out dilution metering, dilution all has considerable influence to the mensuration result of high concentration of chlorine dioxide, and ClO
2The working sample ClO that concentration is high more or extension rate causes more greatly
2Concentration error is big more.Compare, it is little to use detection method provided by the invention to record data error, and the result is more accurate, and can realize fast-field evaluation, easy and simple to handle.
Claims (7)
1. high concentration of chlorine dioxide detection method is characterized in that may further comprise the steps:
1) testing sample placed in the colorimetric bottle seal, use centre wavelength as the LED of 440nm～450nm as monochromatic source, through testing sample solution;
2) detection light source calculates the concentration of chlorine dioxide in the sample through the luminous energy behind the testing sample solution.
2. a kind of high concentration of chlorine dioxide detection method according to claim 1 is characterized in that: the centre wavelength of monochromatic source is the LED of 445nm, and the emission half-angle of LED is 4 °～15 °.
3. high concentration of chlorine dioxide colorimetric device; Comprise monochromatic source (8), cell (7), colorimetric bottle (12); It is characterized in that: monochromatic source (8) adopts the LED of centre wavelength 440nm～450nm, and the emission half-angle of LED is 4 °～15 °, and spectrum width is ± 5nm; Place the colorimetric bottle (12) of cell (7) to have gland bonnet (13), the diameter of colorimetric bottle (12) is 16mm～28mm.
4. a kind of high concentration of chlorine dioxide colorimetric device according to claim 3; It is characterized in that: the inwall of cell (7) is provided with positioning mark (15), colorimetric bottle (12) wall be provided with cell (7) inwall on the telltale mark (14) that is complementary of positioning mark (15).
5. a kind of high concentration of chlorine dioxide colorimetric device according to claim 3 is characterized in that: the bottom of gland bonnet (13) is provided with sealing rubber ring, and sealing rubber ring and sample surface of contact are provided with anticorrosive coat.
6. a kind of high concentration of chlorine dioxide colorimetric device according to claim 3 is characterized in that: cell (7) inwall both sides are provided with the screens (16) that is used for fixing colorimetric bottle.
7. a kind of high concentration of chlorine dioxide colorimetric device according to claim 6 is characterized in that: said screens is the wire projection.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101576118A CN102692386A (en) | 2012-05-18 | 2012-05-18 | Detection method and colorimetric detection device for high-concentration chlorine dioxide |
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| CN2012101576118A CN102692386A (en) | 2012-05-18 | 2012-05-18 | Detection method and colorimetric detection device for high-concentration chlorine dioxide |
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Cited By (3)
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| CN103645146A (en) * | 2013-11-16 | 2014-03-19 | 中山欧麦克仪器设备有限公司 | Chlorine dioxide detection device |
| CN106092941A (en) * | 2016-08-29 | 2016-11-09 | 华南理工大学 | A kind of device of in-situ evaluation metal catalyst reduction performance |
| CN109328356A (en) * | 2016-08-31 | 2019-02-12 | 雅培制药有限公司 | For assessing the system, equipment and correlation technique of biological sample integrality |
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| CN103645146A (en) * | 2013-11-16 | 2014-03-19 | 中山欧麦克仪器设备有限公司 | Chlorine dioxide detection device |
| CN106092941A (en) * | 2016-08-29 | 2016-11-09 | 华南理工大学 | A kind of device of in-situ evaluation metal catalyst reduction performance |
| CN109328356A (en) * | 2016-08-31 | 2019-02-12 | 雅培制药有限公司 | For assessing the system, equipment and correlation technique of biological sample integrality |
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Application publication date: 20120926 |