CN103349955B - Total organic carbon ultraviolet digestion reaction unit - Google Patents

Total organic carbon ultraviolet digestion reaction unit Download PDF

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CN103349955B
CN103349955B CN201310281808.7A CN201310281808A CN103349955B CN 103349955 B CN103349955 B CN 103349955B CN 201310281808 A CN201310281808 A CN 201310281808A CN 103349955 B CN103349955 B CN 103349955B
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reacting part
reaction tube
carrier gas
organic carbon
total organic
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CN103349955A (en
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吴庆华
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Chen Jiyang
Li Li
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SUZHOU ELAB ANALYTICAL INSTRUMENT CO Ltd
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Abstract

The invention discloses a kind of total organic carbon ultraviolet digestion reaction unit, comprise ultraviolet irradiation device (1) and be arranged on the reaction tube (2) outside ultraviolet irradiation device (1), it is characterized in that described reaction tube (2) is provided with the reacting part (23) that inside and outside wall (31,32) forms interlayer reaction zone (3), described reacting part (23) inwall (31) is transparent, described reacting part (23) outer wall (32) be provided be communicated with reacting part (23) respectively carrier gas port (33), injection port (34), leakage fluid dram (35) and gas outlet (36).When this device uses ultraviolet digestion method can test sample TC:5ppb-1000ppm, have good repeatability, test result is accurate.

Description

Total organic carbon ultraviolet digestion reaction unit
Technical field
The invention belongs to total organic carbon analysis technical field, be specifically related to a kind of total organic carbon ultraviolet digestion reaction unit.
Background technology
Total carbon (Total Carbon, TC) is TIC (total inorganic carbon, TIC) with the difference of total organic carbon (Total Organic Carbon, TOC).
When TOC instrument detects TC, first the total carbon (total organic carbon and TIC) in sample is oxidized to carbon dioxide, carbon dioxide is measured by carbon dioxide indicator, then carbon dioxide gas content is converted to the concentration of total carbon in sample by data processing.Method for oxidation comprises the detection methods such as wet oxidation (persulfate), high temperature catalytic combustion oxidation, Ultraviolet Oxidation.
The mensuration of DIC (TIC) generally can be undertaken by acidolysis, and joined by sample in 10% phosphoric acid, TIC generates CO with phosphatase reaction 2.By entering detector except halogen device under the carrying of carrier gas.
As total content of organic carbon very low (as the 5ppb-2ppm) of sample, when using the high-temp combustion non-dispersive infrared method test low concentration total organic carbon sample such as pure water, medicinal water, Monitoring lower-cut is limited in one's ability, and testing result is inaccurate, the poor reproducibility of testing result.The present invention therefore.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of total organic carbon ultraviolet digestion reaction unit, solve sample in prior art total content of organic carbon very low (as 5ppb-2ppm) and cannot the problem of working sample result.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of total organic carbon ultraviolet digestion reaction unit, comprise ultraviolet irradiation device and be arranged on the reaction tube outside ultraviolet irradiation device, it is characterized in that described reaction tube is provided with the reacting part that inside and outside wall forms interlayer reaction zone, described reacting part inwall is transparent, described reacting part outer wall be provided be communicated with reacting part respectively carrier gas port, injection port, leakage fluid dram and gas outlet.
Preferably, described reaction tube comprises the blind portion of reaction tube, reaction tube inlet portion, arranges reacting part between the blind portion of described reaction tube, reaction tube inlet portion; Described ultraviolet irradiation device is inserted in reaction tube by reaction tube inlet portion, and spacing by the blind portion of reaction tube.
Preferably, described gas outlet is arranged on the top of reacting part outer wall, and is communicated with reacting part; Described carrier gas port, leakage fluid dram are separately positioned on the bottom of reacting part outer wall, and are communicated with reacting part.
Preferably, described injection port is arranged in carrier gas port, and described injection port and carrier gas port form y-type structure; During sample introduction, sample is entered by injection port, is conveyed in reacting part by carrier gas port carrier gas.
Preferably, the distance between the inside and outside wall of described reacting part is within the scope of 0.5 ~ 11mm.
Preferably, described ultraviolet irradiation device is uviol lamp, and described ultraviolet irradiation device is through reacting part inwall, and its irradiation area is suitable with interlayer reaction zone.
Preferably, the axis of described carrier gas port, leakage fluid dram is 60 ° with the angle of the axis direction of reaction tube respectively; The axis of described injection port and the axis angle of carrier gas port are 60 °.
Preferably, between described reacting part inside and outside wall, the length of reaction zone is 150-200mm.
Principle of the present invention is to adopt ultra-violet oxidation method; Adopt ultraviolet irradiation device water sample as to be measured in UV light irradiation, carbon compound can decompose and is generated as CO 2, then detect the CO of generation 2total carbon content can be calculated.When using ultra-violet oxidation method, oxidability can be improved by adding persulfate etc.The method oxidation efficiency is high, and maintenance is simple, both can detect the sample of low concentration (as: 5ppb-2ppm).Also high concentration (as: 1000ppm) sample can be detected.The present invention uses ultraviolet digestion method to solve the lower limit scarce capacity problem of high-temp combustion non-dispersive infrared method detection TOC, and during test low concentration sample 5ppb-2ppm, have good repeatability, test result is accurate.
In the present invention, reaction tube adopts quartz ampoule, especially highly purified quartzy material is adopted, the ultraviolet light of ultraviolet irradiation device can as far as possible all by reaction tube (inside and outside wall be quartz ampoule), sample in interlayer reaction zone (reaction tank) between full illumination to reaction tube reacting part inside and outside wall.Total organic carbon ultraviolet digestion reaction unit of the present invention constructs through the structure that lot of experiments optimization draws and carries out the optimization of size aspect, and meet the requirement that uviol lamp can irradiate completely very well, interlayer reaction zone (reaction tank) volume obtained can obtain CO 2(organic carbon converts CO to optimum translation amount 2optimal amount), the CO of generation 2can be brought in low-level device very smoothly by exhaust port.
Total organic carbon ultraviolet digestion reaction unit of the present invention has carrier gas port, injection port, leakage fluid dram and 4, gas outlet interface, and each orifice external world and interlayer reaction zone inner chamber (reaction tank), can handled easily.Injection port is arranged in carrier gas port in addition, forms y-type structure, by carrier gas, sample accurately can be input into reaction tank during sample introduction, sample introduction operation efficiently and accurately, the specification sample introduction operation of handled easily personnel.In addition, total organic carbon ultraviolet digestion reaction unit of the present invention is also applicable to the detection that persulfuric acid oxidizing process carries out total organic carbon, can make sample under strong oxidizer exists situation in reaction tank, participate in reaction, ensures to obtain CO 2optimum translation amount, difficulty is cleared up sample and is used device of the present invention still can be reacted completely.
During specific works, first ultraviolet irradiation device is loaded reaction tube reacting part inwall, make Ultraviolet radiation region be distributed in interlayer reaction zone between reaction tube reacting part inside and outside wall; Then close leakage fluid dram, (prevent CO in air by the air of the emptying interlayer reaction zone of carrier gas port 2affect testing result); Then open ultraviolet irradiation device as UV lamp, add sample when having carrier gas by injection port, sample brings interlayer reaction zone into by carrier gas stream; In interlayer reaction zone, ultraviolet makes the carbon compound in sample be converted into CO 2, the CO then transformed 2cO is accessed by exhaust port 2detect in detector.
Therefore, technical solution of the present invention can in time, Accurate Determining TC content, both gone for measuring the water for injection in pharmaceutical industry, the TC content in purified water, also gone for the TC content of the TC content of the water for cleaning measured in semicon industry and running water, surface water.
Relative to scheme of the prior art, advantage of the present invention is:
Technical solution of the present invention is coordinated by ultraviolet irradiation device and reaction tube, and between the inside and outside wall of described reaction tube reacting part, form interlayer reaction zone, described ultraviolet irradiation device is placed in reacting part inwall, is undertaken clearing up operation by ultraviolet irradiation device.When this device uses ultraviolet digestion method can test low concentration sample 5ppb-2ppm, have good repeatability, test result is accurate.This device does not need dismounting after installing, and cleaning later does not need dismounting yet, and direct injected mode is cleaned, and from the result of many experiments, has excellent repeatability.Both be applicable to detecting low concentration sample, be also applicable to the enriched sample measuring 1000ppm simultaneously.Easy and simple to handle, only need arrange corresponding parameter in software, instrument just automatically testing is obtained a result.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described:
Fig. 1 is the structural representation of embodiment of the present invention total organic carbon ultraviolet digestion reaction unit.
Fig. 2 is the sectional view of embodiment of the present invention total organic carbon ultraviolet digestion reaction unit reaction tube 2.
Wherein, 1 is ultraviolet irradiation device; 2 is reaction tube; 3 is interlayer reaction zone; 21 is reaction tube inlet portion; 22 is the blind portion of reaction tube; 23 is reacting part; 31 is reacting part inwall; 32 is reacting part outer wall; 33 is carrier gas port; 34 is injection port; 35 is leakage fluid dram; 36 is gas outlet.
Detailed description of the invention
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiments are not limited to for illustration of the present invention limit the scope of the invention.The implementation condition adopted in embodiment can do further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
Embodiment
As shown in Fig. 1 ~ 2, this total organic carbon ultraviolet digestion reaction unit, the reaction tube 2 comprising ultraviolet irradiation device 1 and be arranged on outside ultraviolet irradiation device 1, described reaction tube 2 is provided with the reacting part 23 that inside and outside wall 31,32 forms interlayer reaction zone 3, described reacting part 23 inwall 31 is transparent, described reacting part 23 outer wall 32 be provided be communicated with reacting part 23 respectively carrier gas port 33, injection port 34, leakage fluid dram 35 and gas outlet 36.Described ultraviolet irradiation device 1 is placed in reaction tube 2, and its irradiation area spreads all over the reacting part of reaction tube.
Reacting part inwall is transparent, facilitates ultraviolet irradiation device 1 to be transmitted into interlayer reaction zone and participates in reaction.The outer wall of reacting part can be opaque, in order to reacting part technique fires the convenience of aspect, the outer wall of reacting part also together can be fired into transparent.In the present embodiment, reaction tube adopts quartz glass tube, and the blind portion of reaction tube 22, reaction tube inlet portion 21, reacting part 23 are integrated.
Described reaction tube 2 comprises the blind portion 22 of reaction tube, reaction tube inlet portion 21, arranges reacting part 23 between the blind portion 22 of described reaction tube, reaction tube inlet portion 21; Described ultraviolet irradiation device 1 is inserted in reaction tube 2 by reaction tube inlet portion 21, and spacing by reaction tube blind portion 22.
Described gas outlet 36 is arranged on the top of reacting part 23 outer wall 32, and is communicated with reacting part 23; Described carrier gas port 34, leakage fluid dram 35 are separately positioned on the bottom of reacting part 23 outer wall 32, and are communicated with reacting part 23.Described injection port 34 is arranged in carrier gas port 33, and described injection port 34 forms y-type structure with carrier gas port 33; During sample introduction, sample is entered by injection port 34, is conveyed in reacting part 23 by carrier gas port 33 carrier gas.
Distance D between the inside and outside wall 31,32 of described reacting part 23 is within the scope of 2mm.Described ultraviolet irradiation device 1 is uviol lamp, and described ultraviolet irradiation device 1 is through reacting part inwall 31, and its irradiation area is suitable with interlayer reaction zone 3.The axis of described carrier gas port 33, leakage fluid dram 35 is 60 ° with the angle of the axis direction of reaction tube respectively; The axis of described injection port 34 and the axis angle of carrier gas port 33 are 60 °.The length of the inside and outside wall of described reacting part 23 31,32 interlayer reaction zones is 150-200mm.
During work, first ultraviolet irradiation device is loaded in reaction tube reacting part inwall, make Ultraviolet radiation region be distributed in interlayer reaction zone between reaction tube reacting part inside and outside wall; Then close leakage fluid dram, (prevent CO in air by the air of the emptying interlayer reaction zone of carrier gas port 2affect testing result); Then open ultraviolet irradiation device as UV lamp, add sample when having carrier gas by injection port, sample brings interlayer reaction zone into by carrier gas stream; In interlayer reaction zone, ultraviolet makes the carbon compound in sample be converted into CO 2, the CO then transformed 2cO is accessed by exhaust port 2detect in detector.
Above-mentioned example, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalent transformations of doing according to Spirit Essence of the present invention or modification, all should be encompassed within protection scope of the present invention.

Claims (7)

1. a total organic carbon ultraviolet digestion reaction unit, comprise ultraviolet irradiation device (1) and be arranged on the reaction tube (2) outside ultraviolet irradiation device (1), it is characterized in that described reaction tube (2) is provided with inside and outside wall (31, 32) reacting part (23) of interlayer reaction zone (3) is formed, described reacting part (23) inwall (31) is transparent, described reacting part (23) outer wall (32) is provided with the carrier gas port (33) be communicated with reacting part (23) respectively, injection port (34), leakage fluid dram (35) and gas outlet (36), described reaction tube (2) comprises the blind portion of reaction tube (22), reaction tube inlet portion (21), the blind portion of described reaction tube (22), reacting part (23) is set between reaction tube inlet portion (21), described ultraviolet irradiation device (1) is inserted in reaction tube (2) by reaction tube inlet portion (21), and spacing by the blind portion of reaction tube (22).
2. total organic carbon ultraviolet digestion reaction unit according to claim 1, is characterized in that described gas outlet (36) is arranged on the top of reacting part (23) outer wall (32), and is communicated with reacting part (23); Described carrier gas port (33), leakage fluid dram (35) are separately positioned on the bottom of reacting part (23) outer wall (32), and are communicated with reacting part (23).
3. total organic carbon ultraviolet digestion reaction unit according to claim 1, it is characterized in that described injection port (34) is arranged in carrier gas port (33), described injection port (34) and carrier gas port (33) form y-type structure; During sample introduction, sample is entered by injection port (34), is conveyed in reacting part by the carrier gas of carrier gas port (33).
4. total organic carbon ultraviolet digestion reaction unit according to claim 1, is characterized in that distance between described reacting part (23) inside and outside wall (31,32) is within the scope of 0.5 ~ 11mm.
5. total organic carbon ultraviolet digestion reaction unit according to claim 1, it is characterized in that described ultraviolet irradiation device (1) is uviol lamp, described ultraviolet irradiation device (1) is through reacting part inwall (31), and its irradiation area is suitable with interlayer reaction zone (3).
6. total organic carbon ultraviolet digestion reaction unit according to claim 1, is characterized in that described carrier gas port (33), the axis of leakage fluid dram (35) is 60 ° with the angle of the axis direction of reaction tube respectively; The axis of described injection port (34) and the axis angle of carrier gas port (33) are 60 °.
7. total organic carbon ultraviolet digestion reaction unit according to claim 1, is characterized in that the length of reaction zone between described reacting part (23) inside and outside wall (31,32) is 150-200mm.
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CN107655875B (en) * 2017-05-26 2021-05-04 四川大学 Total organic carbon analysis method based on high-intensity ultraviolet light oxidation and point discharge
CN111482154A (en) * 2020-05-18 2020-08-04 嘉兴孚诺纳米科技有限公司 Two-channel efficient continuous flow photochemical mixing device and mixing method thereof
CN113218865A (en) * 2021-05-06 2021-08-06 苏州卡美利多仪器有限公司 Digestion reaction system for total organic carbon analyzer

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CN201051096Y (en) * 2007-06-14 2008-04-23 南开大学 A novel Kjeldahl nitrogen measurement device
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CN102836661A (en) * 2012-08-23 2012-12-26 金川集团股份有限公司 Gas-filling temperature-raising leaching tank
CN202974751U (en) * 2012-11-13 2013-06-05 宇星科技发展(深圳)有限公司 Ultraviolet digestion device for water quality analyzer
CN203316117U (en) * 2013-07-05 2013-12-04 苏州埃兰分析仪器有限公司 Total organic carbon ultraviolet digestion reaction device

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Publication number Priority date Publication date Assignee Title
CN2177521Y (en) * 1993-12-06 1994-09-21 中国科学技术大学 Photochemical reactor for synthesis of halohydrocarbon
CN201051096Y (en) * 2007-06-14 2008-04-23 南开大学 A novel Kjeldahl nitrogen measurement device
WO2012138260A1 (en) * 2011-04-08 2012-10-11 Vasjukov Dmitry Aleksandrovich Device for producing ozone
CN102759477A (en) * 2012-06-27 2012-10-31 西安建筑科技大学 Ultraviolet light catalytic digestion device
CN102836661A (en) * 2012-08-23 2012-12-26 金川集团股份有限公司 Gas-filling temperature-raising leaching tank
CN202974751U (en) * 2012-11-13 2013-06-05 宇星科技发展(深圳)有限公司 Ultraviolet digestion device for water quality analyzer
CN203316117U (en) * 2013-07-05 2013-12-04 苏州埃兰分析仪器有限公司 Total organic carbon ultraviolet digestion reaction device

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Effective date of registration: 20221128

Address after: No.12, Floor 1, Unit 2, Building 10, Chunguang Street, Tiedong District, Anshan City, Liaoning Province, 114000

Patentee after: Li Li

Patentee after: Chen Jiyang

Address before: 215003 A305, Innovation Science Park, No. 17, Songxianzhou Lane, Zhongjie Road, Pingjiang District, Suzhou, Jiangsu Province

Patentee before: SUZHOU ELAB ANALYTICAL INSTRUMENT Co.,Ltd.

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