CN102564837A - Novel ultraviolet preprocessing device - Google Patents
Novel ultraviolet preprocessing device Download PDFInfo
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- CN102564837A CN102564837A CN2010105975226A CN201010597522A CN102564837A CN 102564837 A CN102564837 A CN 102564837A CN 2010105975226 A CN2010105975226 A CN 2010105975226A CN 201010597522 A CN201010597522 A CN 201010597522A CN 102564837 A CN102564837 A CN 102564837A
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- fluorescent tube
- quartz ampoule
- violet
- tube
- pretreating device
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Abstract
The invention provides a novel ultraviolet preprocessing device, which relates to the interface technology of the coupling technology in the field of morphological analysis of elements. The purpose of the invention is to provide the novel ultraviolet preprocessing device which has the advantages of simple structure and high dissolving efficiency and further increases ultraviolet illumination. The novel ultraviolet preprocessing device comprises a low pressure mercury lamp and a quartz tube, wherein the low pressure mercury lamp comprises a lamp tube, an electrode and a power supply, the quartz tube is positioned in the lamp tube, two ends of the quartz tube are fixedly connected with the tube wall of the lamp tube respectively, the inner wall of the lamp tube and the outer wall of the quartz tube form an airtight gas chamber, and the electrode is positioned in the gas chamber.
Description
Technical field
The present invention relates to a kind of interfacing that is used for Elemental Speciation Analysis field coupling technique, particularly relate to a kind of utilization ultraviolet ray and clear up or photochemically reactive device.
Background technology
It is very extensive that the ultraviolet pretreating device is used in the morphological analysis field of element at present, almost is indispensable accessory, because some elements have various forms; Like inorganic form and organic form, lower valency and high valence state, the inorganic form of As has arsenous anion [As (III)] and arsenate [As (V)]; Organic form has dimethyl arsenate (DMA), monomethyl arsenic acid (MMA) or the like; The different shape of element shows different toxicity, and As (III) and As (V) are hypertoxic, and DMA and MMA are harmless basically; For the toxicity of contained element in the accurate assess sample, just need carry out morphological analysis to element.The morphological analysis instrument that extensively adopts at present is the coupling of liquid chromatography and spectroscopic detector, at first on chromatogram, separates, and the separator that flows out behind the post then generates the hydride of gaseous state through hydride reaction, enters into spectroscopic detector again and detects.In the derivatization process that hydride takes place; The hydride luminous efficiency of different element morphologies is different, and the luminous efficiency of As in the arsenic morphology (III) is the highest, and the arsenic betaine (AsB) in the animal food; The Luo Kesha arsine (Roxarsone) in the feed and the direct hydrogenation thing luminous efficiency of arsanilic acid (p-ASA) are very low; Very difficult to be detected, other organic form like elements such as mercury, selenium, tin, antimony also is similar situation, and general solution is before deriving, through the ultraviolet pre-treatment organic form of element to be cleared up into inorganic form; Improve the hydride luminous efficiency, thus the enhancing detection signal; The hydride signal of selenate radical [Se (VI)] does not have basically in addition, also need through the ultraviolet pre-treatment provide energy with its online selenite radical [Se (IV)] that is reduced into to improve detection signal.
Another important use of ultraviolet pretreating device is exactly as photochemical reactor; Discover a lot of elements, comprise that traditional hydride unit takes place have arsenic, antimony, selenium, tin, mercury etc., transitional element has nickel, cobalt, copper, iron; Precious metal element has silver, gold, platinum; Nonmetalloid has iodine, sulphur, exists in the medium of some low-molecular-weight organic solvent (like formic acid, acetate, propionic acid, formaldehyde etc.) at solution, just can generate the corresponding gaseous material of these elements through ultraviolet irradiation; Its principle is exactly that the organic solvent of small-molecular weight is behind ultraviolet irradiation; Generate the free radical molecule of excited state, the free radical molecule of excited state and the reaction of the object element in the solution generate gaseous state thing separately.Especially mercury does not add the auxiliary of low-molecular-weight organic reagent, under ultraviolet irradiation, directly just can generate simple substance mercury, and in the photochemistry of mercury reacted, the low-molecular-weight organic reagent just played the effect of disturbing of eliminating.
Traditional ultraviolet pretreating device; For example Chinese utility model patent CN201184876Y disclosed a kind of " the online ultraviolet that is used for liquid chromatography and atomic fluorescence coupling is cleared up/restoring system "; Be exactly to twine quartz ampoule simply on uviol lamp surface, the sample solution uviol lamp surface of flowing through then, this mode has several shortcomings; At first be that intensity of illumination is not enough; The light that is sent by uviol lamp will see through the lamp wall, and then sees through the quartz ampoule irradiation sample solution that twines, and the intensity of illumination that affacts on the solution significantly weakens; Matrix in the sample solution disturbs greatly besides, in sample solution, has organic solvent such as methyl alcohol, the acetonitrile etc. of high concentration, and their can absorb the ultraviolet lights of incidents in a large number, and the efficient intensity that causes acting on the solution is very low, has had a strong impact on and has cleared up efficient.Experiment show AsB signal detected at all that sample solution contains 0.5% methyl alcohol less than; This has just limited the organic solvent that can not use high concentration in the moving phase; Make some need use the Elemental Speciation Analysis of high levels of organic solvents moving phase to carry out; Separating like the form of tin just needs at least 90% methyl alcohol as moving phase, and sample solution needs to mix with oxygenant (potassium persulfate or oxydol) earlier, and efficient is cleared up in auxiliary enhancing.
Summary of the invention
The technical matters that the present invention will solve provides a kind of simple in structure, further improves ultraviolet illumination, clears up the high new ultra-violet pretreating device of efficient.
New ultra-violet pretreating device of the present invention; Comprise low pressure mercury lamp and quartz ampoule; Said low pressure mercury lamp comprises fluorescent tube, electrode and power supply, and wherein said quartz ampoule is positioned at said fluorescent tube, and the two ends of quartz ampoule are fixedly connected with the tube wall of fluorescent tube respectively; The inwall of said fluorescent tube and quartz ampoule outer wall constitute airtight air chamber, and said electrode is positioned at air chamber.
New ultra-violet pretreating device of the present invention, the two ends of wherein said quartz ampoule are connected with entrance point and endpiece respectively, and it is outside that said entrance point and endpiece are positioned at said fluorescent tube.
New ultra-violet pretreating device of the present invention, wherein said quartz ampoule comprise some direct current sections and bending segment, and some said direct current sections are distributed in the fluorescent tube along said fluorescent tube length direction is parallel, are connected through bending segment between the direct current section.
New ultra-violet pretreating device of the present invention, wherein said bending segment is the U type substantially, and the outer wall of bending segment is fixedly connected with the tube wall of said fluorescent tube.
New ultra-violet pretreating device of the present invention, the material of wherein said fluorescent tube are quartzy, adopt the mode of sintering to fix between said quartz ampoule and the fluorescent tube.
New ultra-violet pretreating device difference from prior art of the present invention is that the pipeline that new ultra-violet pretreating device of the present invention is flowed through sample solution is placed in the low pressure mercury lamp; Pipeline is processed by quartz; Light transmission rate is fabulous; When mercury lamp was worked, the ultraviolet light that sends acted on the solution in the quartz ampoule fully, has improved intensity of illumination greatly.The mechanism of its effect has two aspects, and the one, quartz ampoule receives the irradiation of a plurality of directions in the lamp, so it is improved by the powerful width of cloth of irradiation; The 2nd, behind the adding quartz ampoule, the glow discharge meeting of mercury is carried out along its surface, has further strengthened illumination in the lamp.Novel ultraviolet pretreating device has overcome some shortcomings of traditional ultraviolet pretreating device fully; It at first is the very big raising of intensity of illumination; Also solved simultaneously the interference problem of sample solution middle and high concentration organic matrix to a great extent, experiment shows even solution contains the AsB of 30% methyl alcohol reasonable signal is arranged also; Broken through the restriction of moving phase middle and high concentration organic solvent; Form that make to analyze tin, lead and other elements becomes possibility, and without any need for oxygenant as secondary solvent, saved the consumption of solvent.
Below in conjunction with accompanying drawing new ultra-violet pretreating device of the present invention is described further.
Description of drawings
Fig. 1 is the structural representation of new ultra-violet pretreating device of the present invention;
Fig. 2 clears up efficient for AsB in variable concentrations methyl alcohol;
Fig. 3 is the photochemistry generation spectrogram of mercury shape.
Embodiment
As shown in Figure 1; New ultra-violet pretreating device of the present invention comprises low pressure mercury lamp 1 and quartz ampoule 2; Low pressure mercury lamp 1 comprises quartz burner 3, electrode 4 and power supply 5, and quartz ampoule 2 is positioned at fluorescent tube 3, and the two ends of quartz ampoule 2 are fixed together with the tube wall of fluorescent tube 3 mode through sintering respectively; Quartz ampoule 2 comprises some direct current sections 9 and bending segment 10; Some direct current sections 9 are distributed in the fluorescent tube 3 along fluorescent tube 3 length directions are parallel, are connected through U type bending segment 10 between the direct current section 9, and the tube wall of the outer wall of bending segment 10 and fluorescent tube 3 is fixedly connected through the mode of sintering.The inwall of fluorescent tube 3 and quartz ampoule 2 outer walls constitute airtight air chamber 6, are full of low-pressure mercury vapour in the air chamber 6, and electrode 4 is positioned at air chamber 6.The two ends of quartz ampoule 2 are connected with entrance point 7 and endpiece 8 respectively, and entrance point 7 is positioned at fluorescent tube 3 outsides with endpiece 8, and solution to be measured can get into quartz ampoule 2 from entrance point 7, flows out from endpiece 8 then.
Embodiment one
The AsB solution of preparation 50 μ g/L in the PBS of pH=6.0, it is auxiliary need not add any oxygenant, under different peristaltic pump rotating speeds; Directly, detect with the morphological analysis appearance, obtain the conversion ratio of clearing up of AsB through postradiation solution through the irradiation of new ultra-violet pretreating device; Referring to table 1; And investigated the variation that AsB clears up efficient in different methanol concentrations, referring to Fig. 2, the result shows; Because the ability of clearing up of new ultra-violet pretreating device of the present invention strengthens, the signal of AsB does not receive the influence of methanol concentration basically.
Table 1AsB clears up the conversion ratio result
Embodiment two.
Compound concentration is inorganic mercury, the methyl mercury of 50 μ g/L, the mixed solution of ethyl mercury; Behind the sample introduction under the promotion of moving phase on the C18 chromatographic column absorb-elute separate; Effluent directly takes place through new ultra-violet pretreating device photochemistry of the present invention behind the post; The mercury simple substance that produces is taken in the detecting device by carrier gas and detects, and obtains the signal of each mercury shape, referring to Fig. 3.
Above-described embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (5)
1. new ultra-violet pretreating device; Comprise low pressure mercury lamp (1) and quartz ampoule (2); Said low pressure mercury lamp (1) comprises fluorescent tube (3), electrode (4) and power supply (5), it is characterized in that: said quartz ampoule (2) is positioned at said fluorescent tube (3), and the two ends of quartz ampoule (2) are fixedly connected with the tube wall of fluorescent tube (3) respectively; The inwall of said fluorescent tube (3) and quartz ampoule (2) outer wall constitute airtight air chamber (6), and said electrode (4) is positioned at air chamber (6).
2. new ultra-violet pretreating device according to claim 1 is characterized in that: the two ends of said quartz ampoule (2) are connected with entrance point (7) and endpiece (8) respectively, and said entrance point (7) and endpiece (8) are positioned at said fluorescent tube (3) outside.
3. new ultra-violet pretreating device according to claim 2; It is characterized in that: said quartz ampoule (2) comprises some direct current sections (9) and bending segment (10); Some said direct current sections (9) are connected through bending segment (10) between the direct current section (9) along parallel being distributed in the fluorescent tube (3) of said fluorescent tube (3) length direction.
4. new ultra-violet pretreating device according to claim 3 is characterized in that: said bending segment (10) is the U type substantially, and the outer wall of bending segment (10) is fixedly connected with the tube wall of said fluorescent tube (3).
5. new ultra-violet pretreating device according to claim 4 is characterized in that: the material of said fluorescent tube (3) adopts the mode of sintering to fix for quartzy between said quartz ampoule (2) and the fluorescent tube (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105975226A CN102564837A (en) | 2010-12-20 | 2010-12-20 | Novel ultraviolet preprocessing device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105975226A CN102564837A (en) | 2010-12-20 | 2010-12-20 | Novel ultraviolet preprocessing device |
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| CN102564837A true CN102564837A (en) | 2012-07-11 |
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| CN2010105975226A Pending CN102564837A (en) | 2010-12-20 | 2010-12-20 | Novel ultraviolet preprocessing device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107894511A (en) * | 2017-10-27 | 2018-04-10 | 河北莱博瑞特电子科技有限公司 | A kind of Elemental Speciation Analysis instrument |
| CN114354550A (en) * | 2021-11-23 | 2022-04-15 | 中国恩菲工程技术有限公司 | Antimony online reduction detection device and method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3117307A1 (en) * | 1980-06-26 | 1982-03-18 | Vituki Vizgazdálkodási Tudományos Kutatóközpont, 1095 Budapest | Tube reactor for carrying out photochemical reactions |
| TW436303B (en) * | 1998-10-02 | 2001-05-28 | Common Services Agency | A method and apparatus for use in the UV-irradiation of a biological fluid |
| JP3227278B2 (en) * | 1993-07-24 | 2001-11-12 | 株式会社堀場製作所 | UV light reaction vessel |
| CN2741964Y (en) * | 2004-11-15 | 2005-11-23 | 中国海洋大学 | Ultraviolet digestion device for dissolving organic nitrogen and phospherus in sea water |
| CN1837824A (en) * | 2006-04-25 | 2006-09-27 | 北京吉天仪器有限公司 | Ultraviolet auxiliary extraction and hydride generation-atomic fluorescence spectrometry method for determining lead content in blood and extractor therefor |
-
2010
- 2010-12-20 CN CN2010105975226A patent/CN102564837A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3117307A1 (en) * | 1980-06-26 | 1982-03-18 | Vituki Vizgazdálkodási Tudományos Kutatóközpont, 1095 Budapest | Tube reactor for carrying out photochemical reactions |
| JP3227278B2 (en) * | 1993-07-24 | 2001-11-12 | 株式会社堀場製作所 | UV light reaction vessel |
| TW436303B (en) * | 1998-10-02 | 2001-05-28 | Common Services Agency | A method and apparatus for use in the UV-irradiation of a biological fluid |
| CN2741964Y (en) * | 2004-11-15 | 2005-11-23 | 中国海洋大学 | Ultraviolet digestion device for dissolving organic nitrogen and phospherus in sea water |
| CN1837824A (en) * | 2006-04-25 | 2006-09-27 | 北京吉天仪器有限公司 | Ultraviolet auxiliary extraction and hydride generation-atomic fluorescence spectrometry method for determining lead content in blood and extractor therefor |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107894511A (en) * | 2017-10-27 | 2018-04-10 | 河北莱博瑞特电子科技有限公司 | A kind of Elemental Speciation Analysis instrument |
| CN107894511B (en) * | 2017-10-27 | 2023-09-15 | 河北莱博瑞特电子科技有限公司 | Elemental morphology analyzer |
| CN114354550A (en) * | 2021-11-23 | 2022-04-15 | 中国恩菲工程技术有限公司 | Antimony online reduction detection device and method |
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Application publication date: 20120711 |