CN102495058A - Constant-temperature fiber optic colorimetric titration device and detection method thereof - Google Patents
Constant-temperature fiber optic colorimetric titration device and detection method thereof Download PDFInfo
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- CN102495058A CN102495058A CN2011103987933A CN201110398793A CN102495058A CN 102495058 A CN102495058 A CN 102495058A CN 2011103987933 A CN2011103987933 A CN 2011103987933A CN 201110398793 A CN201110398793 A CN 201110398793A CN 102495058 A CN102495058 A CN 102495058A
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Abstract
The invention relates to a constant-temperature fiber optic colorimetric titration device and a detection method thereof. The constant-temperature fiber optic colorimetric titration device comprises a magnetic stirring device, a light-emitting diode, an incident optical fiber, heat-conducting silicone grease, a cuvette, a glass cap, a vent, an aluminum block, an outgoing optical fiber, a selenium photocell, a lens, a heating plate, a liquid inlet/outlet and a temperature sensor. The magnetic stirring device is arranged on the lower part of the cuvette, and the glass cap with the vent is arranged on the cuvette in a covering way; the bottom end of the cuvette is provided with the liquid inlet/outlet and the heating plate; the two sides of the cuvette are respectively provided with the light-emitting diode and the selenium photocell, the incident optical fiber is connected between the cuvette and the light-emitting diode, and the lens and the outgoing optical fiber are connected sequentially between the selenium photocell and the cuvette; and the outer wall of the cuvette is coated with the aluminum block, the heat-conducting silicone grease is filled between the outer wall of the cuvette and the aluminum block, the outer side of the aluminum block is provided with a groove for arrangement of the heating plate, and the aluminum block is internally provided with a round hole for accommodating the temperature sensor. The constant-temperature fiber optic colorimetric titration device has high heating speed and is suitable for online monitoring, and uniform heating can be realized.
Description
Technical field
The present invention relates to the colorimetric titration device of field of environment protection water quality online automatic monitor, relate in particular to a kind of thermostatical color comparison titration apparatus.
Background technology
Environmental pollution has become the significant problem of whole world common concern, particularly along with the development of industrial economy, in the environment pollution of water body more serious, the task of on-line monitoring is very arduous.Therefore water quality monitoring needs more accurate, the stable survey instrument that faces, to satisfy the needs of modern environment monitoring development.Various titrators are arranged at present both at home and abroad: conductance titration, radio frequency titration, coulometric titration, photometric titration etc., wherein be not subject to the interference and the pollution of complex sample component with photometric titration, range of application is the wideest, in international and domestic standard by extensively employing; Colorimetric analysis also is one of important method in the analytical chemistry, for constant, trace, trace analysis very high sensitivity, accuracy is arranged all; Photometric titration and colorimetric analysis; Must in a reaction tank, carry out titration or chromogenic reaction, and, just analyze, calculate to provide the detection data according to different programs by the light activated element output voltage signal; Therefore with the reaction tank universalization of this two alanysis; Dual-use, existing objective possibility possesses skills again, economic implications.In addition, because monitored water body adopts electrically heated rod or oil bath type of heating,, exist defectives such as thermal field is inhomogeneous, thermometric is inaccurate although it is very fast to heat up.
Application number is 01131529.6; Name is called the Chinese invention patent of titration, the general reaction unit of colorimetric; The reaction tank that is respectively equipped with incident monochromatic source and light activated element by relative both sides constitutes; Be provided with magnetic stirrer, inlet and leakage fluid dram in its underpart, described incident monochromatic source is to conduct to reaction pool wall one side through incident optical, and described light activated element is to come the light signal in the acceptable response pond through the outgoing optical fiber that is located at the relative side of pool wall; Said reaction tank top is provided with the loam cake that has steam (vapor) outlet; Its middle and lower part also is provided with temperature sensor, automatically controlled well heater, and described inlet is connected with automatically controlled impregnator, and described leakage fluid dram is connected with automatically controlled peristaltic pump.This patent only is designed with automatically controlled well heater in both sides, reaction tank lower end, and it is slow not only to heat up, and heats inhomogeneously, causes thermometric inaccurate, and chromogenic reaction waits defective slowly.
The patent No. is ZL200820240834.X; Name is called a kind of Chinese utility model patent of clearing up titration apparatus, comprises the vitreous digestion container that is installed in the shell, and the top of said digestion container and bottom are respectively equipped with into water appearance mouth and discard solution discharge port; The top is connected to a refrigeratory; Metal-plated membrane adds hot-dip coating on the outside wall surface of digestion container, and the two ends that metal film adds hot-dip coating are connected to lead respectively, and the bottom of digestion container is provided with the magnetic stirring apparatus; Said digestion container two ends also are provided with optical transmission/reception device; Said optical transmission/reception device comprises light expelling plate, light receiving plate and lamp guide; Light expelling plate and light receiving plate are positioned at the two ends of lamp guide, are linked to each other by two lamp guides between light expelling plate, light receiving plate and the digestion container bottle; Said digestion container is provided with built-in platinum resistor temperature measuring device.This utility model patent only between about 1/3 height of the outer wall of digestion container and bottom metal-plated membrane add hot-dip coating, exist firing rate slow equally, heat inhomogeneously, cause thermometric inaccurate, chromogenic reaction waits defective slowly.
Summary of the invention
The present invention is directed to that the titration colorimetric device exists firing rate slow in the prior art; Heat inhomogeneously, cause thermometric inaccurate, chromogenic reaction is slow; And in the optic path process, receive defectives such as the various interference of external electromagnetism; Provide a kind of firing rate fast, homogeneous heating, and optical fiber can not receive the constant temperature fiber ratio color titration apparatus of various interference such as external electromagnetism in conductive process.
A kind of constant temperature fiber ratio color titration apparatus comprises magnetic stirring apparatus, light emitting diode, incident optical, cuvette, glass cap, vent port, framework, outgoing optical fiber, selenium cell, lens, liquid in-out mouth, temperature sensor; Said magnetic stirring apparatus is installed in the bottom of said cuvette, and the said glass cap that has said vent port is on said cuvette, and the bottom of said cuvette is provided with said liquid in-out mouth; The both sides, lower end of said cuvette are installed said light emitting diode and said extinction battery respectively; Connect incident optical between said cuvette and the light emitting diode; Be connected with lens and outgoing optical fiber between said extinction battery and the cuvette in turn, it is characterized in that: also comprise aluminium block, heating plate and heat-conducting silicone grease, the bottom of said cuvette is equipped with heating plate; The outer wall of said cuvette is enclosed with said aluminium block; Be filled with said heat-conducting silicone grease between the two, be provided with the groove that is used to place said heating plate around the outside of said aluminium block, the said frame fixation that is used for fixing said heating plate is on said aluminium block; The indoor design of said aluminium block is useful on the circular hole that holds said temperature sensor.
As preferably, said cuvette is the fiber ratio color ware.
As preferably, said incident optical and said outgoing optical fiber have 1/3 part to stretch in the cuvette respectively.
As preferably, the said aluminium block outside is provided with the groove that is used to place said heating plate has 8.
As preferably, said magnetic stirring apparatus is made up of motor, magnetic receiver, magnet and magnetic agitation, and said magnet is installed on the said magnetic receiver, and said magnetic receiver is installed on the main shaft of said motor, and said magnetic agitation places the bottom of cuvette.
As preferably, the circular hole that is used to hold said temperature sensor is positioned at the position of said aluminium block inside near the cuvette middle part.
As preferably, the light path of said light emitting diode, incident optical, outgoing optical fiber, selenium cell, lens point-blank.
The method of constant temperature fiber ratio color titration apparatus detection material comprises gauge line, liquid level detector, peristaltic pump, multi-position valve, water sample, potassium permanganate, sulfuric acid, sodium oxalate.Said water sample, potassium permanganate, sulfuric acid, sodium oxalate are connected with the distribution port of said multi-position valve respectively; The lower end of gauge line is connected with the public port of multi-position valve; Peristaltic pump is connected with the upper end of gauge line through a pipeline; Liquid level detector is installed in the upper end of gauge line, and one of multi-position valve is distributed port to be connected with the liquid in-out mouth; It is characterized in that:
Use the method for constant temperature fiber ratio color titration apparatus detection material, may further comprise the steps:
A. respectively water sample, sulfuric acid and the potassium permanganate of certain volume are pushed in the cuvette through multi-position valve, peristaltic pump, gauge line, start magnetic stirring apparatus and begin to stir, heat temperature raising to 99 ℃ carries out constant temperature digestion, and liquid does not seethe with excitement in the digestion process;
B. clear up and finish, be cooled to 80 ℃, stop to stir;
C. through multi-position valve, peristaltic pump, gauge line the sodium oxalate of certain volume is pushed in the cuvette, begin to stir, and heated at constant temperature to 75 ℃;
D. pass through in multi-position valve, peristaltic pump, the potassium permanganate suction gauge line with certain volume, peristaltic pump control gauge line splashes into potassium permanganate in cuvette then, is heated to 75 ℃ of constant temperature, and sodium oxalate and potassium permanganate are fully reacted;
E. light emitting diode emission light passes mixed solution, is received by selenium cell, judges whether the measuring light signal that selenium cell receives reaches setting value; Promptly whether reach titration end-point,, then get into next step if result of determination reaches titration end-point; If do not reach titration end-point, then get back to steps d, repeated several times; Peristaltic pump control gauge line splashes into isopyknic potassium permanganate in cuvette, for being, promptly the light signal that receives of selenium cell reaches setting value up to result of determination;
F. be cooled to 50 ℃, stop to stir, write down titration time, calculate the value of measured matter through inner equation.
Description of drawings
Shown in Figure 1 is constant temperature fiber ratio color titration apparatus structural representation of the present invention
Structural drawing for aluminium block in the constant temperature fiber ratio color titration apparatus of the present invention shown in Figure 2
Shown in Figure 3 is constant temperature fiber ratio color titration apparatus embodiment structural representation of the present invention
Embodiment
Illustrated in figures 1 and 2, constant temperature fiber ratio color titration apparatus of the present invention comprises motor 1, magnetic receiver 2, magnet 3, magnetic agitation 4, light emitting diode 5, incident optical 6, heat-conducting silicone grease 7, cuvette 8, glass cap 9, vent port 10, aluminium block 11, framework 12, outgoing optical fiber 13, selenium cell 14, lens 15, heating plate 16, liquid in-out mouth 17, temperature sensor 18; Wherein motor 1, magnetic receiver 2, magnet 3, magnetic agitation 4 are assembled into magnetic stirring apparatus, and magnetic receiver 2 is installed on the main shaft of motor 1, and magnet 3 is installed on the magnetic receiver 2, and magnetic agitation 4 places the bottom of cuvette 8; Cuvette 8 is the fiber ratio color ware; The glass cap 9 that has vent port 10 covers on cuvette 8, and the bottom of cuvette 8 is provided with liquid in-out mouth 17, and heating plate 16 is installed; The both sides, lower end of cuvette 8 are installed light emitting diode 5 and extinction battery 14 respectively; Connect incident optical 6 between cuvette 8 and the light emitting diode 5, be connected with lens 15 and outgoing optical fiber 13 between extinction battery 14 and the cuvette 8 in turn, incident optical 6 has 1/3 part to stretch in the cuvette 8 respectively with outgoing optical fiber 13; The light path of light emitting diode 5, incident optical 6, outgoing optical fiber 13, selenium cell 14, lens 15 point-blank; The outer wall of cuvette 8 is enclosed with aluminium block 11, is filled with heat-conducting silicone grease 7 between the two, is provided with 8 grooves around the outside of aluminium block 11, and heating plate 16 is placed in the groove of aluminium block 11, and the framework 12 that is used for fixing heating plate 16 is fixed on the aluminium block 11; The inside of aluminium block 11 is designed with the circular hole that is used to hold temperature sensor 18 near the medium position of cuvette 8.
Shown in Figure 3 is constant temperature fiber ratio color titration apparatus embodiment structural representation of the present invention, comprises gauge line 19, liquid level detector 20, peristaltic pump 21, multi-position valve 22, water sample, potassium permanganate, sulfuric acid, sodium oxalate.Wherein water sample, potassium permanganate, sulfuric acid, sodium oxalate are connected with the distribution port of multi-position valve 22 respectively; The lower end of gauge line 19 is connected with the public port of multi-position valve 22; Peristaltic pump 21 is connected through the upper end of a pipeline with gauge line 19, and liquid level detector 20 is installed in the upper end of gauge line 19, and one of multi-position valve 22 is distributed port to be connected with liquid in-out mouth 17; Use the method for constant temperature fiber ratio color titration apparatus detection material, may further comprise the steps:
A. respectively water sample, sulfuric acid and the potassium permanganate of certain volume are pushed in the cuvette 8 through multi-position valve 22, peristaltic pump 21, gauge line 19, start magnetic stirring apparatus and begin to stir, heat temperature raising to 99 ℃ carries out constant temperature digestion, and liquid does not seethe with excitement in the digestion process;
B. clear up and finish, be cooled to 80 ℃, stop to stir;
C. through multi-position valve 22, peristaltic pump 21, gauge line 19 sodium oxalate of certain volume is pushed in the cuvette 8, begin to stir, and heated at constant temperature to 75 ℃;
D. pass through in multi-position valve 22, peristaltic pump 21, the potassium permanganate suction gauge line 19 with certain volume, peristaltic pump 21 control gauge lines 19 splash into potassium permanganate in cuvette 8 then, are heated to 75 ℃ of constant temperature, and sodium oxalate and potassium permanganate are fully reacted;
E. light emitting diode 5 emission light pass mixed solution, are received by selenium cell 14, judge whether the measuring light signal that selenium cell 14 receives reaches setting value; Promptly whether reach titration end-point,, then get into next step if result of determination reaches titration end-point; If do not reach titration end-point; Then get back to steps d, repeated several times, peristaltic pump 21 control gauge lines 19 splash into isopyknic potassium permanganate in cuvette 8; For being, promptly the light signal that receives of selenium cell 14 reaches setting value up to result of determination;
F. be cooled to 50 ℃, stop to stir, write down titration time, calculate the value of measured matter through inner equation.
Constant temperature fiber ratio color titration apparatus of the present invention has the following advantages:
1. apparatus of the present invention have promptly all been installed heating plate in the outer wall and the bottom of cuvette around cuvette, and this design has realized the even heating and the constant temperature digestion of measured matter.
2. apparatus of the present invention have increased aluminium block and heat-conducting silicone grease on the basis of conventional art, not only realized the even heating of measured matter, and the cuvette programming rate are fast, has improved color speed.
3. the cuvette of apparatus of the present invention adopts the fiber ratio color ware, and connects incident optical and outgoing optical fiber in fiber ratio color ware both sides, has improved the conduction efficiency of light.
Apparatus of the present invention adopt clear up, titration, colorimetric integrated design scheme, improved the reliability of Monitoring Data, reduced the production cost of monitoring instrument simultaneously.
Claims (8)
1. a constant temperature fiber ratio color titration apparatus comprises magnetic stirring apparatus, light emitting diode, incident optical, cuvette, glass cap, vent port, framework, outgoing optical fiber, selenium cell, lens, liquid in-out mouth, temperature sensor; Said magnetic stirring apparatus is installed in the bottom of said cuvette, and the said glass cap that has said vent port is on said cuvette, and the bottom of said cuvette is provided with said liquid in-out mouth; The both sides, lower end of said cuvette are installed said light emitting diode and said extinction battery respectively; Connect incident optical between said cuvette and the light emitting diode; Be connected with lens and outgoing optical fiber between said extinction battery and the cuvette in turn, it is characterized in that: also comprise aluminium block, heating plate and heat-conducting silicone grease, the bottom of said cuvette is equipped with heating plate; The outer wall of said cuvette is enclosed with said aluminium block; Be filled with said heat-conducting silicone grease between the two, be provided with the groove that is used to place said heating plate around the outside of said aluminium block, the said frame fixation that is used for fixing said heating plate is on said aluminium block; The indoor design of said aluminium block is useful on the circular hole that holds said temperature sensor.
2. constant temperature fiber ratio color titration apparatus according to claim 1 is characterized in that: said cuvette is the fiber ratio color ware.
3. constant temperature fiber ratio color titration apparatus according to claim 1 is characterized in that: said incident optical and said outgoing optical fiber have 1/3 part to stretch in the cuvette respectively.
4. constant temperature fiber ratio color titration apparatus according to claim 1 is characterized in that: being provided with the groove that is used to place said heating plate around the said aluminium block outside has 8.
5. constant temperature fiber ratio color titration apparatus according to claim 1; It is characterized in that: said magnetic stirring apparatus is made up of motor, magnetic receiver, magnet and magnetic agitation; Said magnet is installed on the said magnetic receiver; Said magnetic receiver is installed on the main shaft of said motor, and said magnetic agitation places the bottom of cuvette.
6. constant temperature fiber ratio color titration apparatus according to claim 1 is characterized in that: the circular hole that is used to hold said temperature sensor is positioned at the position of said aluminium block inside near the cuvette middle part.
7. constant temperature fiber ratio color titration apparatus according to claim 1 is characterized in that: the light path of said light emitting diode, incident optical, outgoing optical fiber, selenium cell, lens point-blank.
8. a method of using the described constant temperature fiber ratio color of claim 1 titration apparatus detection material comprises gauge line, liquid level detector, peristaltic pump, multi-position valve, water sample, potassium permanganate, sulfuric acid, sodium oxalate.Said water sample, potassium permanganate, sulfuric acid, sodium oxalate are connected with the distribution port of said multi-position valve respectively; The lower end of gauge line is connected with the public port of multi-position valve; Peristaltic pump is connected with the upper end of gauge line through a pipeline; Liquid level detector is installed in the upper end of gauge line, and one of multi-position valve is distributed port to be connected with the liquid in-out mouth; It is characterized in that:
Use the method for constant temperature fiber ratio color titration apparatus detection material, may further comprise the steps:
A. respectively water sample, sulfuric acid and the potassium permanganate of certain volume are pushed in the cuvette through multi-position valve, peristaltic pump, gauge line, start magnetic stirring apparatus and begin to stir, heat temperature raising to 99 ℃ carries out constant temperature digestion, and liquid does not seethe with excitement in the digestion process;
B. clear up and finish, be cooled to 80 ℃, stop to stir;
C. through multi-position valve, peristaltic pump, gauge line the sodium oxalate of certain volume is pushed in the cuvette, begin to stir, and heated at constant temperature to 75 ℃;
D. pass through in multi-position valve, peristaltic pump, the potassium permanganate suction gauge line with certain volume, peristaltic pump control gauge line splashes into potassium permanganate in cuvette then, is heated to 75 ℃ of constant temperature, and sodium oxalate and potassium permanganate are fully reacted;
E. light emitting diode emission light passes mixed solution, is received by selenium cell, judges whether the measuring light signal that selenium cell receives reaches setting value; Promptly whether reach titration end-point,, then get into next step if result of determination reaches titration end-point; If do not reach titration end-point, then get back to steps d, repeated several times; Peristaltic pump control gauge line splashes into isopyknic potassium permanganate in cuvette, for being, promptly the light signal that receives of selenium cell reaches setting value up to result of determination;
F. be cooled to 50 ℃, stop to stir, write down titration time, calculate the value of measured matter through inner equation.
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| CN102928363A (en) * | 2012-10-24 | 2013-02-13 | 重庆川仪分析仪器有限公司 | Photoelectric detection device and hydrazine analyzer |
| CN103018168A (en) * | 2012-11-30 | 2013-04-03 | 江苏德林环保技术有限公司 | Cross integral digestion colorimetric pool |
| CN103018169A (en) * | 2012-11-30 | 2013-04-03 | 江苏德林环保技术有限公司 | Integrated digestion colorimetric pool |
| CN104535401A (en) * | 2014-12-26 | 2015-04-22 | 河北先河环保科技股份有限公司 | Digestion colorimetric stirring device applicable to automatic monitoring instrument of permanganate index |
| CN105445192A (en) * | 2015-12-14 | 2016-03-30 | 天津港东科技发展股份有限公司 | Embedded magnetic stirring constant-temperature sample rack |
| CN106124287A (en) * | 2016-06-13 | 2016-11-16 | 山东思睿环境设备科技有限公司 | High Temperature High Pressure clears up fiber ratio color system |
| CN106501066A (en) * | 2016-12-27 | 2017-03-15 | 钦州市明大检测认证技术有限公司 | Clear up the heating and temperature controlling device for catching up with sour instrument |
| CN109444132A (en) * | 2018-12-25 | 2019-03-08 | 广州市怡文环境科技股份有限公司 | A kind of resolution colorimetric device and equipment |
| CN109718736A (en) * | 2019-02-25 | 2019-05-07 | 水利部南京水利水文自动化研究所 | A kind of photovoltaic determines the drop reaction device and method of titration end-point |
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| CN112229797A (en) * | 2020-09-29 | 2021-01-15 | 江西怡杉环保股份有限公司 | Novel cuvette for water quality online monitoring equipment |
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| CN103018169A (en) * | 2012-11-30 | 2013-04-03 | 江苏德林环保技术有限公司 | Integrated digestion colorimetric pool |
| CN104535401A (en) * | 2014-12-26 | 2015-04-22 | 河北先河环保科技股份有限公司 | Digestion colorimetric stirring device applicable to automatic monitoring instrument of permanganate index |
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| CN106501066A (en) * | 2016-12-27 | 2017-03-15 | 钦州市明大检测认证技术有限公司 | Clear up the heating and temperature controlling device for catching up with sour instrument |
| CN109444132B (en) * | 2018-12-25 | 2024-07-05 | 广州市怡文环境科技股份有限公司 | Digestion colorimetric device and equipment |
| CN109444132A (en) * | 2018-12-25 | 2019-03-08 | 广州市怡文环境科技股份有限公司 | A kind of resolution colorimetric device and equipment |
| CN109718736A (en) * | 2019-02-25 | 2019-05-07 | 水利部南京水利水文自动化研究所 | A kind of photovoltaic determines the drop reaction device and method of titration end-point |
| CN111307777A (en) * | 2020-03-30 | 2020-06-19 | 上海市计量测试技术研究院 | Trace uranium analyzer |
| CN112229797A (en) * | 2020-09-29 | 2021-01-15 | 江西怡杉环保股份有限公司 | Novel cuvette for water quality online monitoring equipment |
| CN113029962A (en) * | 2021-03-03 | 2021-06-25 | 贵阳学通仪器仪表有限公司 | Reaction tank colorimetric device for high-precision water quality detector and manufacturing method thereof |
| CN113029962B (en) * | 2021-03-03 | 2024-03-12 | 贵阳学通仪器仪表有限公司 | Reaction tank colorimetric device for high-precision water quality detector and manufacturing method thereof |
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| CN116609279B (en) * | 2023-05-29 | 2023-12-22 | 上海博取仪器有限公司 | Calibrating device of water quality testing equipment light source |
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Application publication date: 20120613 |