CN1314591A - Combined system of micro column high efficiency liquid phase chromatograph and surface emission flame luminosity detector - Google Patents
Combined system of micro column high efficiency liquid phase chromatograph and surface emission flame luminosity detector Download PDFInfo
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- CN1314591A CN1314591A CN 01103947 CN01103947A CN1314591A CN 1314591 A CN1314591 A CN 1314591A CN 01103947 CN01103947 CN 01103947 CN 01103947 A CN01103947 A CN 01103947A CN 1314591 A CN1314591 A CN 1314591A
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- detector
- surface emission
- combined system
- liquid phase
- flame luminosity
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- 239000007791 liquid phase Substances 0.000 title abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000002485 combustion reaction Methods 0.000 claims description 8
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 235000009781 Myrtillocactus geometrizans Nutrition 0.000 claims description 4
- 240000009125 Myrtillocactus geometrizans Species 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000012159 carrier gas Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 6
- 238000005259 measurement Methods 0.000 claims 1
- 150000002902 organometallic compounds Chemical class 0.000 claims 1
- 230000002093 peripheral effect Effects 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 4
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 230000000877 morphologic effect Effects 0.000 abstract description 3
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003256 environmental substance Substances 0.000 abstract 1
- 150000002736 metal compounds Chemical class 0.000 abstract 1
- 150000003606 tin compounds Chemical class 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 7
- PIILXFBHQILWPS-UHFFFAOYSA-N tributyltin Chemical compound CCCC[Sn](CCCC)CCCC PIILXFBHQILWPS-UHFFFAOYSA-N 0.000 description 5
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- AFCAKJKUYFLYFK-UHFFFAOYSA-N tetrabutyltin Chemical compound CCCC[Sn](CCCC)(CCCC)CCCC AFCAKJKUYFLYFK-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LUZSPGQEISANPO-UHFFFAOYSA-N butyltin Chemical compound CCCC[Sn] LUZSPGQEISANPO-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- -1 phosphorus compound Chemical class 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 206010019133 Hangover Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001348 alkyl chlorides Chemical class 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000003562 morphometric effect Effects 0.000 description 1
- 238000013425 morphometry Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to the field of chemical analysis instrument and the whole detection system consists of efficiency liquid phase chromatographic pump, sampler, capillary separating column and surface emission flame luminosity detector. During operation, certain amount of compound sample is made to enter to micro column via the sampler and separated sample components are analyzed quantitatively in the surface emission flame luminosity detector. The system features the direct detection of compound sample without derivativatization pre-treatment, is suitable for the morphological analysis of organic metal compound, especially organic tin compound and may find its wide applicatino in environmental chemical research and environmental monitoring.
Description
The invention belongs to the chemical analysis test instrument field, relate to the development of a kind of micro column high efficiency liquid phase chromatograph and surface emission flame luminosity detector combined system.Whole detection system is made up of conventional efficient liquid-phase chromatographic pump, injection port, capillary separation column and surface emission flame luminosity detector.It is a kind of new coupling instrument, be characterized in that sample compound does not need can directly measure by the pre-treatment of deriving, be suitable for the particularly morphological analysis of organo-tin compound of organometallics, in environmental chemistry study and environmental monitoring, be with a wide range of applications.
The background in present technique field and current situation are roughly as follows: because the restriction of high pressure liquid chromatography detection method, chemical compound lot can't Sensitive Detection.If can directly measure the outflow component of high pressure liquid chromatography with the flame type detecting device of gas chromatography, will obtain sensitive determination, and expand the usable range of high pressure liquid chromatography thus greatly.But the post flow of conventional high pressure liquid chromatography is in the ml/min level, and big like this flow is what to be difficult to the direct coupling of flame type detecting device of gas chromatography.And the post flow of microtrabeculae is in microlitre/classification, and the characteristics that this flow is less make and utilize the online detection of gas chromatography detector to become possibility.In recent years, the microtrabeculae high pressure liquid chromatography is with characteristics such as its high separating efficiency, low moving phase consumption and low sample demands, be subjected to the attention of researcher, particularly, in the mensuration of sulfur-bearing, phosphorus compound, brought into play vital role with micro column liquid chromatography and the coupling of gas chromatographic flame photometric detector.But present research mainly concentrates on the research of organic sulfur, phosphorus, still is not used in the Morphometric instrument system of organometallics.The research of relevant this respect can be referring to 1.McGuffin, V.L.and Novotny, M., J.Chromatogr., 1981,218,179-181.2.Kientz, C.E., Verweij, A., and Boter, H.L., J.Chromatogr.1989,467,385-394.3.Kientz, C.E and Verweij, A., Intern.J.Environ.Anal.Chem.1987,30,255-2634.Bernard, J., Nicodemo, T., Barthakur, N.N.and Blais, J.S., Analyst, 1994,119,1475-1481.
The purpose of this invention is to provide a kind of instrument system according to microtrabeculae high pressure liquid chromatography and surface emission flame luminosity detector on-line coupling, its various performance index meet the requirement of quantitative test.
Finish technical scheme of the present invention and realize that by following manner Fig. 1 is the synoptic diagram of micro column high efficiency liquid phase chromatograph and surface emission flame luminosity detector combined system.During system works, the moving phase in the liquid storage bottle 1 is pushed by pump 2, and flow control is in 30 μ L/min scopes, and 2 μ L samples enter part flow arrangement 4 through Rheodyne 7725i (25 μ L loop) sampling valve 3, and split ratio generally was controlled at 2: 1.Concrete connection is: utilize stainless-steel tube (150mm, 1/16) import of connection sampling valve and three-way connection, the two ends in addition of three-way connection directly are connected into separates with capillary column 5 and shunting capillary column 6, the emptying together of component that distributes and moving phase, and the outflow component after the chromatographic column separation is by hollow kapillary (i.d.0.22mm) connection detector 7 that links to each other with capillary column, be carried into quartzy combustion head by carrier gas, detect by surface emission flame luminosity detector 8.Experimental data is by SC-1100 type workstation 9 (Beijing Kang Lin scientific ﹠ technical corporation) record and processing.In realizing process of the present invention, the phase composition of flowing, quartz glass combustion head structure, burning gases composition and other operating parameters are optimized: 1) organic solvent is had certain tolerance in view of surface emission flame luminosity detector, non-aqueous solvent methyl alcohol is selected in this work, and butyl tin exists with the nonionic form in moving phase; On inverse bonded stationary phase, alkyl chloride and similar compound are very easily adsorbed by residual silanol groups, in moving phase, add an amount of acetate and can suppress this suction-operated, in moving phase, add 2% acetate in the experiment, the peak relaxation phenomenon that alleviates the hangover of tributyl tin and cause because of absorption.2) in quartzy combustion head, embed the passage of the stainless-steel tube of an internal diameter 0.30mm as the terminal kapillary insertion of microtrabeculae, its top is than the low about 20mm in quartz ampoule combustion head plane.During the methyl alcohol burning, except that can be to blue flame stably in quartz glass tube upper end viewed in plan, its blue light fills the whole quartz glass tube top that is not occupied by stainless-steel tube, thereby has effectively increased luminous intensity, has improved the detect ability of detecting device to the purpose compound.3) pipe can only feed oxygen-enriched combustion-supporting gas-air in the combustion head, it mixes with small uniform methyl alcohol drop in advance, burn with the hydrogen acting in conjunction of periphery then and obtain stable and bright blue flame, as in interior pipe, feeding hydrogen for increasing rich hydrogen effect merely, when being written into, can not light the methyl alcohol drop.Feeding hydrogen nitrogen mixed gas in outer tube more only feeds hydrogen and for the detection of butyl tin significantly sensitization is arranged.4) measure preceding elder generation and in chromatographic column, inject organic acid (as acetate), treat after chromatographic column balance 4～5h that the state that the remolding sensitivity of butyltin compound does not inject acid will improve 10～20%.
Under operating conditions, every index of native system has been carried out test repeatedly, system's baseline wander is less than 50 μ V/h, the instrument noise remains on 120 ± 20 μ V, TBT (5-40ngSn) continuous sample introduction detection within the specific limits with 30 μ g/ml, its peak height, peak area all have the better linearity relation to the sample size match, and γ is between 0.993～0.996.Native system is used for the mensuration of water sample organotin, and its precision and lowest detectable limit are respectively 1.9,2.9 and 0.38ng, 0.42ng.The separation case of tributyl tin and tetrabutyltin is seen Fig. 2, and wherein 1 is tributyl tin (TBT), and 2 is tetrabutyltin (TeBT).At present, this system has been used to the morphological analysis of organo-tin compound in the water sample.Can predict, this technology will be with a wide range of applications in environmental chemistry study and environmental monitoring.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01103947 CN1314591A (en) | 2001-02-16 | 2001-02-16 | Combined system of micro column high efficiency liquid phase chromatograph and surface emission flame luminosity detector |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01103947 CN1314591A (en) | 2001-02-16 | 2001-02-16 | Combined system of micro column high efficiency liquid phase chromatograph and surface emission flame luminosity detector |
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| CN1314591A true CN1314591A (en) | 2001-09-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376892C (en) * | 2004-11-11 | 2008-03-26 | 中国海洋大学 | A method for detecting tributyltin oxide in the marine environment using Philippine clams |
| CN104748970A (en) * | 2015-03-31 | 2015-07-01 | 北京航空航天大学 | Gas testing system suitable for tests of low-thrust engine |
| CN106872636A (en) * | 2017-03-31 | 2017-06-20 | 四川大学 | The method that the combination of low pressure ion chromatography inductivity coupled plasma mass spectrometry determines inorganic tin and organo-tin compound simultaneously |
| CN103575797B (en) * | 2012-08-03 | 2018-04-03 | 克洛纳测量技术有限公司 | Manufacture the method for flame ionization detector and corresponding flame ionization detector |
| CN111220747A (en) * | 2018-11-27 | 2020-06-02 | 中国科学院大连化学物理研究所 | Sulfur response signal enhancement assembly of flame photometric detector and application thereof |
-
2001
- 2001-02-16 CN CN 01103947 patent/CN1314591A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376892C (en) * | 2004-11-11 | 2008-03-26 | 中国海洋大学 | A method for detecting tributyltin oxide in the marine environment using Philippine clams |
| CN103575797B (en) * | 2012-08-03 | 2018-04-03 | 克洛纳测量技术有限公司 | Manufacture the method for flame ionization detector and corresponding flame ionization detector |
| CN104748970A (en) * | 2015-03-31 | 2015-07-01 | 北京航空航天大学 | Gas testing system suitable for tests of low-thrust engine |
| CN104748970B (en) * | 2015-03-31 | 2017-07-04 | 北京航空航天大学 | A kind of gas test system suitable for thrustor experiment |
| CN106872636A (en) * | 2017-03-31 | 2017-06-20 | 四川大学 | The method that the combination of low pressure ion chromatography inductivity coupled plasma mass spectrometry determines inorganic tin and organo-tin compound simultaneously |
| CN106872636B (en) * | 2017-03-31 | 2018-05-25 | 四川大学 | The method that low pressure ion chromatography-inductivity coupled plasma mass spectrometry combination measures inorganic tin and organo-tin compound simultaneously |
| CN111220747A (en) * | 2018-11-27 | 2020-06-02 | 中国科学院大连化学物理研究所 | Sulfur response signal enhancement assembly of flame photometric detector and application thereof |
| CN111220747B (en) * | 2018-11-27 | 2022-03-15 | 中国科学院大连化学物理研究所 | Sulfur response signal enhancement assembly of flame photometric detector and application thereof |
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