CN109342349B - TOC wet chemical analysis device and method - Google Patents

TOC wet chemical analysis device and method Download PDF

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CN109342349B
CN109342349B CN201811443193.2A CN201811443193A CN109342349B CN 109342349 B CN109342349 B CN 109342349B CN 201811443193 A CN201811443193 A CN 201811443193A CN 109342349 B CN109342349 B CN 109342349B
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pipe
blow
air
toc
stripping
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CN109342349A (en
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汪水吉
翁灼斌
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Fujian Jilongde Environmental Protection Technology Co ltd
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Fujian Jilongde Environmental Protection Technology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation

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Abstract

The invention discloses a TOC wet chemical analysis device which comprises a multi-way direct discharge valve, a peristaltic pump, a UV digestion device, a blow-off pipe, an NDIR detector and an air pump. The bottom of the stripping pipe is respectively connected with an air pump and a peristaltic pump, a CO2 absorber is arranged at the joint of the air pump and the bottom of the stripping pipe, the multi-way direct vent valve is connected with the peristaltic pump, the upper part of the stripping pipe is respectively connected with an NDIR detector and a UV digestion device, and the UV digestion device is connected with the multi-way direct vent valve. The multi-way direct vent valve, the middle part of the blow-off pipe and the lower part of the blow-off pipe are all connected with an emptying pipeline. The invention also discloses a TOC wet chemical analysis method. The invention has the advantages that: rational in infrastructure, analysis process automation degree is high, and the TOC analytic process is quick, high-efficient, and the analytic process need not high temperature, instrument long service life.

Description

TOC wet chemical analysis device and method
Technical Field
The invention relates to the technical field of water quality analysis, in particular to a TOC wet chemical analysis device and method.
Background
The existing TOC (total organic carbon) analysis method at home and abroad is mainly a combustion oxidation-non-dispersive infrared absorption method, and although the sensitivity of the method is high, the method has the following defects: the sample needs to be subjected to high-temperature catalytic oxidation by a high-temperature combustion tube, so that both organic compounds and inorganic carbonate are converted into carbon dioxide, the generated carbon dioxide is sequentially introduced into a non-dispersive infrared detector, and the TOC in water is measured, while the temperature of the high-temperature combustion tube is as high as 900 ℃, the lowest temperature also needs 150 ℃, and the instrument is easily damaged by overhigh temperature for conventional measurement.
Disclosure of Invention
In view of the above problems, the present invention provides a TOC wet chemical analysis apparatus and method with fast and efficient analysis process and without high temperature.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a TOC wet chemical analysis device comprises a multi-way direct discharge valve, a peristaltic pump, a UV digestion device, a blow-off pipe, an NDIR detector and an air pump. The bottom of the stripping pipe is respectively connected with an air pump and a peristaltic pump, a CO2 absorber is arranged at the joint of the air pump and the bottom of the stripping pipe, the multi-way direct vent valve is connected with the peristaltic pump, the upper part of the stripping pipe is respectively connected with an NDIR detector and a UV digestion device, and the UV digestion device is connected with the multi-way direct vent valve. The multi-way direct vent valve, the middle part of the blow-off pipe and the lower part of the blow-off pipe are all connected with an emptying pipeline.
Furthermore, the multi-way direct-discharge valve is an eight-way direct-discharge valve, and the eight-way direct-discharge valve comprises valves Q1, Q2, Q3, Q4, Q5, Q6, Q7 and Q8. Wherein, Q1, Q2 are connected with R1 medicament pipe, R2 medicament pipe respectively, Q3 is connected with the pure water pipe, Q4 is connected with the intake pipe, Q5 is connected with the water sample pipe, Q6 is connected with the mark liquid pipe, Q7 is connected with the evacuation pipeline, Q8 is connected with the UV digestion ware.
Further, a three-way valve QA is arranged at the joint of the upper part of the stripping pipe and the UV digestion device, the three-way valve QA comprises a normally-open end, a normally-closed end and a common end, the upper part of the stripping pipe is connected with the common end of the QA, and the normally-closed end of the QA is connected with the UV digestion device.
Furthermore, the connection part of the upper part of the blow-off pipe and the NDIR detector is provided with three-way valves QB and QC, a copper wire filter and a filter membrane, and the three-way valves QB and QC respectively comprise a normally open end, a normally closed end and a public end. The upper portion of blow-off pipe is connected with the end of blowing off QC normally, and the public end of QC is connected with the public end of QB, and the end of blowing off QC normally closed is connected with the middle part of blow-off pipe, and the end of blowing off QB normally is connected with the copper wire filter, and the evacuation pipeline is connected to the end of blowing off QB normally open.
Wherein the aperture of the filter membrane is 0.3-0.6 um.
Furthermore, the device also comprises a T-shaped tee joint, and three valve ports of the T-shaped tee joint are respectively connected with the peristaltic pump, the bottom of the blow-off pipe and the CO2 absorber.
Wherein, the joint of the CO2 absorber and the T-shaped tee joint is provided with a pressure valve and a flowmeter.
Furthermore, a water sample detector is arranged at the joint of the peristaltic pump and the multi-way direct discharge valve.
The invention also discloses a TOC wet chemical analysis method, which adopts the TOC wet chemical analysis device and comprises the following steps:
step 1: and (4) emptying the blow-off pipe and the UV digester.
Step 2: and a water sample is pumped into the stripping pipe from the bottom of the stripping pipe through a peristaltic pump, redundant water samples are discharged from an emptying pipeline in the middle of the stripping pipe, and the water samples in the common pipeline of the multi-way direct vent valve are all blown into the stripping pipe by air.
And step 3: the reagent R1 is pumped into the air-stripping pipe from the bottom of the air-stripping pipe through a peristaltic pump, wherein R1 is sulfuric acid solution with the concentration of 8% -12%, the redundant reagent R1 is discharged from an emptying pipe at the middle part of the air-stripping pipe, and the reagent R1 in the common pipeline of the multi-way direct vent valve is completely blown into the air-stripping pipe by air.
And 4, step 4: and (3) starting the air pump, filtering CO2 from air by a CO2 absorber, blowing the air into the stripping pipe from the bottom of the stripping pipe, carrying out aeration stripping on a sample in the stripping pipe, and blowing CO2 generated by reaction with R1 to an NDIR detector to measure a TIC peak value.
And 5: and slowly rotating the peristaltic pump, adding the medicament R2 into the air-stripping tube from the bottom of the air-stripping tube, wherein the R2 is a mixed solution of sulfuric acid with the concentration of 0.4-0.6% and sodium sulfate with the concentration of 10-15%, discharging redundant medicament R2 from an emptying pipeline in the middle of the air-stripping tube, and blowing all the medicaments R2 in the common pipeline of the multi-way direct vent valve into the air-stripping tube by using air.
Step 6: and (4) reversing the peristaltic pump, and continuously oxidizing and digesting the sample in the stripping pipe in the UV digestion device.
And 7: and the air pump is started, air enters from the bottom of the stripping pipe after CO2 is filtered by the CO2 absorber, samples in the stripping pipe are continuously aerated and stripped, CO2 generated by reaction in the stripping pipe is blown to an NDIR detector to measure a TOC peak value, and the TOC value is calculated according to data in the instrument.
And 8: and emptying the blow-off pipe and the UV digester and then cleaning with pure water.
The invention has the following beneficial effects: the invention has reasonable structure, high automation degree of the analysis process, quick and efficient TOC analysis process, no need of high temperature in the analysis process and long service life of the instrument.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Description of the main component symbols: 1. an eight-way straight exhaust valve; 101. r1 vial; 102. r2 vial; 103. a pure water pipe; 104. an air inlet pipe; 105. a water sample pipe; 106. a marking liquid pipe; 2. a peristaltic pump; 3. a UV digestion device; 4. blowing off the pipe; 5. an NDIR detector; 6. an air pump; 7. t-shaped tee joints; 8. a CO2 absorber; 9. a water sample detector; 10. a pressure valve; 11. a flow meter; 12. a copper wire filter; 13. 0.45u filter.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
As shown in FIG. 1, the TOC wet chemical analysis device comprises an eight-way straight exhaust valve 1, a peristaltic pump 2, a UV digestion device 3, a blow-off pipe 4, an NDIR detector 5 and an air pump 6. The eight-way straight-through valve 1 comprises valves Q1, Q2, Q3, Q4, Q5, Q6, Q7 and Q8. Wherein, Q1, Q2 are connected with R1 medicament pipe 101, R2 medicament pipe 102 respectively, Q3 is connected with pure water pipe 103, Q4 is connected with intake pipe 104, Q5 is connected with water sampling pipe 105, Q6 is connected with standard liquid pipe 106, Q7 is connected with W1 evacuation pipe, Q8 is connected with UV digestion device 3.
The bottom of the stripping tube 4 is respectively connected with the air pump 6 and the peristaltic pump 2, a T-shaped tee 7 is arranged below the stripping tube 4, three valve ports of the T-shaped tee 7 are respectively connected with the peristaltic pump 2, the bottom of the stripping tube 4 and the CO2 absorber 8, the other end of the peristaltic pump 2 is connected with the eight-way straight exhaust valve 1, and a water sample detector 9 is arranged at the joint of the peristaltic pump 2 and the eight-way straight exhaust valve 1. The joint of the CO2 absorber 8 and the T-shaped tee joint 7 is provided with a pressure valve 10 and a flow meter 11, and the CO2 absorber 8 is connected with the air pump 6. The upper part of the stripping pipe 4 is respectively connected with the NDIR detector 5 and the UV digestion device 3, a three-way valve QA is arranged at the joint of the stripping pipe 4 and the UV digestion device 3, the three-way valve QA comprises a normally-open end (NO end), a normally-closed end (NC end) and a common end (COM end), the upper part of the stripping pipe 4 is connected with the common end of the QA, and the normally-closed end of the QA is connected with the UV digestion device 3.
The junction of the blow-off pipe 4 and the NDIR detector 5 is provided with three-way valves QB and QC, a copper wire filter 12 and a 0.45u filter membrane 13, and the three-way valves QB and QC respectively comprise a normally open end, a normally closed end and a public end. The upper portion of blow-off pipe 4 is connected with the normal start of QC, and the common end of QC is connected with the common end of QB, and the normal close end of QC is connected with the middle part of blow-off pipe 4, and the normal start of QB is connected with copper wire filter 12, and the normal start of QB is connected W2 evacuation pipeline.
The invention also discloses a TOC wet chemical analysis method, which adopts the TOC wet chemical analysis device and comprises the following steps:
step 1: after the instrument starts measurement, firstly, emptying liquid in the TOC waterway stripping tube 4, performing Q3 action, reversely rotating the peristaltic pump 2, and discharging the liquid from the lower end of the stripping tube 4; q7 and QB act, the liquid in the upper pipeline of the blow-off pipe 4 is discharged from the upper part of the blow-off pipe 4; the QA and QB valves are actuated to rotate the peristaltic pump 2 forward, the liquid in the UV sterilizer 3 is pumped to the stripping tube 4, then Q7 is actuated to rotate the peristaltic pump 2 backward, and the remaining liquid is completely discharged from the lower end of the stripping tube 4.
Step 2: taking in a sample, actuating valves Q5, QB and QC, rotating the peristaltic pump 2 positively, taking in a water sample from the end 105 of the water sample pipe, then entering from the bottom of the blow-off pipe 4, and allowing the redundant sample to pass through QC and then flow into a W2 emptying pipe from the normally closed end of the QB due to the quantitative action of a pipe valve; the Q4, QB and QC valves act, and all samples in the common pipeline of the eight-way straight exhaust valve 1 are blown into the blow-off pipe 4 by air, so that the effect of mixing the samples is achieved.
And step 3: the Q1, QB and QC valves are actuated, the peristaltic pump 2 is slowly turned, R1 (10% sulfuric acid solution) is quantitatively added into the stripping tube 4, and the redundant liquid is discharged into the W2 emptying pipe from the normally closed end of the QB. After the medicine is added, the Q5 and the QB valves act, and all the medicines in the common pipeline of the eight-way straight exhaust valve 1 are blown into the air stripping pipe 4 by air, so that the sample and the medicines are fully mixed and reacted.
And 4, step 4: the air pump 6 is started, air enters from the bottom of the air stripping pipe 4 through the T-shaped tee joint 7 after CO2 is filtered by the CO2 absorber 8, samples in the pipe are continuously aerated and stripped, and CO2 generated by reaction with the reagent R1 is blown to the NDIR detector 5 to measure the TIC peak value.
And 5: the Q2 valve was actuated, the peristaltic pump 2 was turned slowly, and R2 (0.5% sulfuric acid and 12% sodium persulfate) was added to the stripping tube 4. After the medicine is added, the valve Q5 acts, all the medicines in the common pipeline of the eight-way straight exhaust valve 1 are blown into the blow-off pipe 4 by air, so that the sample and the medicines are fully mixed and reacted.
Step 6: the QA valve and the Q8 act, the peristaltic pump 2 is reversed, the sample in the pipeline is continuously oxidized and digested in the UV digestor 3, and the liquid in the pipeline is fully mixed and reacted.
And 7: the air pump 6 is started, air enters from the bottom of the stripping pipe 4 through the T-shaped tee joint 7 after CO2 is filtered by the CO2 absorber 8, samples in the pipe are continuously aerated and stripped, and CO2 generated by the reaction of total organic carbon and the medicament R2 is blown to the NDIR detector 5 to measure the TOC peak value. The TOC value was calculated from the data in the meter in mg/L.
And 8: and emptying the blow-off pipe 4 and the UV digester 3, and then cleaning with pure water.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (8)

1. A TOC wet chemical analysis method, characterized in that: adopt wet chemical analysis device of TOC, wet chemical analysis device of TOC include multi-ported direct vent, peristaltic pump, UV digestion ware, blow off pipe, NDIR detector and air pump, the bottom of blow off pipe is connected with air pump and peristaltic pump respectively, and air pump and blow off bottom of the tubes junction are equipped with CO2 absorber, multi-ported direct vent be connected with the peristaltic pump, the upper portion of blow off pipe is connected with NDIR detector and UV digestion ware respectively, and UV digestion ware is connected with multi-ported direct vent, the middle part and the lower part of multi-ported direct vent, blow off pipe all be connected with the evacuation pipeline, wet chemical analysis method of TOC, include following step:
step 1: emptying the blow-off pipe and the UV digestion device;
step 2: pumping a water sample into the blow-off pipe from the bottom of the blow-off pipe through a peristaltic pump, discharging redundant water samples from an emptying pipeline in the middle of the blow-off pipe, and blowing all the water samples in the multi-way direct vent common pipeline into the blow-off pipe by using air;
and step 3: the reagent R1 is pumped into the air-stripping pipe from the bottom of the air-stripping pipe through a peristaltic pump, wherein R1 is sulfuric acid solution with the concentration of 8-12%, the redundant reagent R1 is discharged from an emptying pipe at the middle part of the air-stripping pipe, and the reagent R1 in the common pipeline of the multi-way direct vent valve is completely blown into the air-stripping pipe by air;
and 4, step 4: the air pump is started, air is blown into the blow-off pipe from the bottom of the blow-off pipe after CO2 is filtered out by the CO2 absorber, samples in the blow-off pipe are aerated and blown off, and CO2 generated by reaction with R1 is blown to an NDIR detector to measure a TIC peak value;
and 5: slowly rotating the peristaltic pump, adding the medicament R2 into the air stripping pipe from the bottom of the air stripping pipe, wherein the R2 is a mixed solution of sulfuric acid with the concentration of 0.4-0.6% and sodium sulfate with the concentration of 10-15%, discharging redundant medicament R2 from an emptying pipeline in the middle of the air stripping pipe, and blowing all the medicaments R2 in the common pipeline of the multi-way direct vent valve into the air stripping pipe by using air;
step 6: reversing the peristaltic pump, and continuously oxidizing and digesting the sample in the blow-off pipe in a UV digestion device;
and 7: the air pump is started, air enters from the bottom of the stripping pipe after CO2 is filtered by the CO2 absorber, samples in the stripping pipe are continuously aerated and stripped, CO2 generated by reaction in the stripping pipe is blown to an NDIR detector to measure a TOC peak value, and the TOC value is calculated according to data in the instrument;
and 8: and emptying the blow-off pipe and the UV digester and then cleaning with pure water.
2. A TOC wet chemical analysis method according to claim 1, wherein: the multi-way direct-discharging valve is an eight-way direct-discharging valve which comprises valves Q1, Q2, Q3, Q4, Q5, Q6, Q7 and Q8, wherein Q1 and Q2 are respectively connected with a R1 medicament pipe and a R2 medicament pipe, Q3 is connected with a pure water pipe, Q4 is connected with an air inlet pipe, Q5 is connected with a water sampling pipe, Q6 is connected with a standard liquid pipe, Q7 is connected with an emptying pipe, and Q8 is connected with a UV digestion device.
3. A TOC wet chemical analysis method according to claim 1, wherein: the junction of the upper part of the stripping pipe and the UV digestion device is provided with a three-way valve QA, the three-way valve QA comprises a normally-open end, a normally-closed end and a common end, the upper part of the stripping pipe is connected with the common end of the QA, and the normally-closed end of the QA is connected with the UV digestion device.
4. A TOC wet chemical analysis method according to claim 1, wherein: the upper portion of blow-off pipe is equipped with three-way valve QB and QC, copper wire filter and filter membrane with the junction of NDIR detector, three-way valve QB and QC include the end of opening always, normally closed end and public end respectively, the upper portion of blow-off pipe is connected with the end of opening always of QC, the public end of QC is connected with the public end of QB, the end of closing always of QC is connected with the middle part of blow-off pipe, the end of opening always of QB is connected with the copper wire filter, the evacuation pipeline is connected to the end of opening always of QB.
5. The method of claim 4, wherein said TOC wet chemical analysis comprises: the aperture of the filter membrane is 0.3-0.6 um.
6. A TOC wet chemical analysis method according to claim 1, wherein: the three valve ports of the T-shaped tee joint are respectively connected with the peristaltic pump, the bottom of the blow-off pipe and the CO2 absorber.
7. A TOC wet chemical analysis method according to claim 6 wherein: and a pressure valve and a flowmeter are arranged at the joint of the CO2 absorber and the T-shaped tee joint.
8. A TOC wet chemical analysis method according to claim 1, wherein: and a water sample detector is arranged at the joint of the peristaltic pump and the multi-way direct discharge valve.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101178392A (en) * 2007-10-26 2008-05-14 山西大学 Organic matter in water enriching concentrating instrument and control method thereof
CN201392315Y (en) * 2008-12-26 2010-01-27 马三剑 Automatic on-line monitoring device for ammonia nitrogen
CN202421060U (en) * 2011-11-25 2012-09-05 北京瑞升特科技有限公司 Cyanide measuring system
CN107367475A (en) * 2017-07-20 2017-11-21 福建省吉龙德环保科技有限公司 Water sample total cyanogen analytical equipment and analysis method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101178392A (en) * 2007-10-26 2008-05-14 山西大学 Organic matter in water enriching concentrating instrument and control method thereof
CN201392315Y (en) * 2008-12-26 2010-01-27 马三剑 Automatic on-line monitoring device for ammonia nitrogen
CN202421060U (en) * 2011-11-25 2012-09-05 北京瑞升特科技有限公司 Cyanide measuring system
CN107367475A (en) * 2017-07-20 2017-11-21 福建省吉龙德环保科技有限公司 Water sample total cyanogen analytical equipment and analysis method

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