CN105606718A - High performance liquid chromatography and Fourier transform infrared spectroscopy combined interface device - Google Patents
High performance liquid chromatography and Fourier transform infrared spectroscopy combined interface device Download PDFInfo
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- CN105606718A CN105606718A CN201510800397.7A CN201510800397A CN105606718A CN 105606718 A CN105606718 A CN 105606718A CN 201510800397 A CN201510800397 A CN 201510800397A CN 105606718 A CN105606718 A CN 105606718A
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Abstract
The invention discloses a high performance liquid chromatography (HPLC) and Fourier transform infrared spectroscopy (FTIR) combined interface device, and belongs to the field of environmental studies. The device is composed of seven components: an optical table, a zinc selenide (ZnSe) crystal, a round drive rotary table, a heating casing pipe, an atomizer, a cleaning device and a drying device. A target pollutant enters a heating casing pipe and atomizer integrated device after being separated by a chromatography column, is heated and atomized, and then is evenly sprayed on the surface of the ZnSe crystal, and the ZnSe crystal is rotated to the optical table from the round drive rotary table. Infrared light enters the ZnSe crystal at a certain angle through the optical table, is reflected, then enters an FTIR detector and is subjected to atlas analysis. The ZnSe crystal having testing completed is transferred to the cleaning device and the drying device successively, is washed and dried respectively and then is re-used. The round rotary table carries the crystal and a sample for reciprocating detection by means of rotation, and sample batch processing and on-line detection are realized.
Description
Technical field:
The present invention relates to a kind of high performance liquid chromatography and Fourier transform infrared spectroscopy combination interface device, particularly realize in water bodyThe successful separation of pollutant, the effectively qualitative analysis of detection.
Background technology:
At present, current widely used separation, analysis, purified organic compound effective ways are gas chromatography and liquid chromatogramMethod. And in known organic compound, approximately have 80% organic compound higher boiling, difficult gasification volatilization, gas chromatography incapabilityEffectively separate. High performance liquid chromatography (HighPerformanceLiquidChromatography, HPLC) is due to itPart gentleness, not destroying sample, is the effective means that separates difficult volatility complex material. But, use conventional chromatogram detection techniqueBut poor effect aspect Structural Identification and isomers discriminating.
FTIS (Fouriertransforminfraredspectroscopy, FTIR) is with its high-resolution, heightThe feature such as sensitivity and rapid scanning has been brought up to a new height the qualitative speciality of infrared spectrum, and this technology is called as compound" fingerprint " detection means, be the main method of organic compound calibrating and structural analysis. And FTIR technology is had together to heightThe chromatographic technique of separating power combines, and can obtain the infrared spectrum of each component in complex mixture, has made up chromatogram fixedProperty analyze in deficiency. Gas-chromatography (gaschromatography, GC) has realized online connection with FTIR, successfullyMeasure the infrared spectrum of various chromatographic peaks. But, need to measure structure the compound complex material that molecular weight is larger often,Boiling point also higher, many materials is not suitable for separating with GC; Although or GC can separate, require FTIR light pipe temperatureHeight, has reduced sensitivity, so the application of GC-FTIR has certain limitation. For these reasons, high-efficient liquid phase color in recent yearsSpectrum (HPLC) and the research of FTIR GC-MS start to receive publicity. The mobile phase using due to HPLC is often organic solvent,They often have the absorption band of its characteristic frequency at infrared region, having a strong impact on the infrared spectrum qualification of chromatographic fraction. At present, oneAbout HPLC-FTIR interface, development makes some progress a bit, but also has some problems, such as solvent needs heating, rightThe compound of measuring thermal decomposition is very unfavorable; Owing to adopting, reflectance spectrum energy loss is large, very large on the impact of detection sensitivity;Mechanical system complexity, processing and manufacturing difficulty etc. Therefore, this research and design HPLC-FTIR combination interface device, realizes water bodyThe qualitative analysis that middle pollutant successfully separates, effectively detects.
Summary of the invention:
The invention provides a kind of HPLC-FTIR interface arrangement, by the efficient separation function of liquid chromatogram and infrared spectrum " fingerprint "Qualitative ability combines, and has realized the mutual supplement with each other's advantages of the two, and sample in environment is carried out to batch on-line analysis.
The present invention is by optical table, zinc selenide (ZnSe) crystal, circular transmission turntable, heating muff, atomizer, cleaning dressPut and seven assemblies compositions such as drying unit. Concrete operations are, when target contaminant and mobile phase are through the chromatogram of high performance liquid chromatographyAfter post separates, biased sample can enter in heating muff (logical nitrogen protection) and start heating, and process is higher than mobile phase boiling pointAfter temperature, remaining sample carries out atomization and it is evenly sprayed to ZnSe plane of crystal through atomizer, transmits turntable by circleBe rotated to optical table place. In optical table warehouse, be provided with two aluminium mirrors, its effect is reflects infrared light, makes it with certain incidentAngle enters ZnSe crystal, IR be attached to the sample multiple-contact of plane of crystal after, carrying a large amount of sample messagesEnter FTIR detector and carry out atlas analysis. When detector obtains after infrared spectrum, circular transmission turntable reception & disposal signalThe crystal to be measured next one is written into optical table, and the ZnSe crystal that has completed test is moved to cleaning place by circular rotating platform, and cleaning fluid is logicalCross pump and import, ZnSe crystal is cleaned, remove the remaining organic matter that is attached to plane of crystal, make crystal recycling. ClearlyAfter washing into, crystal is moved to oven dry place by circular rotating platform, purges, to reach further clean object through high-temperature gas. CircleShape turntable carries crystal and sample carries out reciprocal testing through over-rotation, has realized sample batch process and online detection analyzed.
Major advantage of the present invention:
(1) the peculiar molecular structure identification capacity of HPLC high efficient separation technology and FTIR combines, and can complete in water body multipleThe qualitative analysis of pollutant, makes up the deficiency of chromatographic technique qualitative analysis.
(2) device has incorporated nitrogen protection heating technique, sample atomization technique and attenuate total reflection (AttenuatedtotalFefraction, ATR) technology, regulate the interference can effectively remove liquid chromatogram mobile to examination of infrared spectrum time by temperature,ATR technology increases IR and sample contact probability and has amplified detection signal, is more conducive to the detection of detector.
(3) circular transmission turntable, cleaning and drying unit have been realized the batch of sample, online detection analyzed.
Fig. 1: the main diagram of HPLC-FTIR interface arrangement;
Fig. 2: the left diagram of HPLC-FTIR interface arrangement;
Fig. 3: the HPLC-FTIR interface arrangement diagram of bowing;
In figure: the circular transmission turntable of 1-, 2-optical table, 3-ZnSe crystal, 4-heating muff, atomizer integrated apparatus,5-cleaning device, 6-drying unit.
Detailed description of the invention:
1. buy the standard liquid of target contaminant to be measured (Single Pollution thing or combined pollutant), prepare certain density standardUse liquid. First target contaminant standard liquid is entered to high performance liquid chromatography and separate, determine target contaminant going out separatelyPeak time, this time is the infrared signal acquisition time of HPLC-FTIR.
By target contaminant with corresponding mobile phase after the chromatographic column of high performance liquid chromatography separates, enter HPLC-FTIRCombination interface device. First sample enters heating muff, atomizer integrated apparatus 4, completes the pretreatment of sample. According to streamThe boiling point of moving phase, water and target contaminant is different, regulates the temperature of heating muff, interfering material in mobile phase is removed, simultaneouslyEnter atomizer atomization after nitrogen protection heating after, be injected to ZnSe crystal 3 surfaces.
3. the ZnSe crystal 3 that contains processed sample is gone to optical table 2 places by circular transmission turntable 1. The storehouse of optical table 2In body, be provided with two aluminium mirrors by reflects infrared light, make it enter ZnSe crystal 2 with certain incident angle, IR with adhere toAfter the sample multiple-contact of plane of crystal, carrying a large amount of sample messages and entering detector and obtain infrared spectrum.
4, next crystal is written into optical table by circular transmission turntable 2, and the crystal that has completed test is moved to clearly by circular rotating platformCleaning device 5, imports corresponding cleaning fluid by pump. After cleaning completes, crystal is moved to drying unit 6 by circular rotating platform to carry outDry, purge through high-temperature gas, reach further clean object. Circular rotating platform carries crystal and sample carries out through over-rotationReciprocal online detection in batches.
Claims (5)
1. high performance liquid chromatography and a Fourier transform infrared spectroscopy combination interface device, by optical table, zinc selenide (ZnSe)The assembly compositions such as crystal, circular transmission turntable, heating muff, atomizer, cleaning device and drying unit.
2. according to described in claim 1, its feature is: target contaminant with mobile phase after chromatographic column separates, target dirtDye thing and after chromatographic column separates, enter that heating jacket, atomizer integrated apparatus heat, atomization, be evenly sprayed at ZnSe crystalSurface, transmits turntable by circle and is rotated to optical table place.
3., described in requiring according to right 1 and right 2, its feature is: the infrared light of being launched by FTISEnter ZnSe crystal through optical table by certain firing angle and reflect, then enter FTIR detector and carry out atlas analysis.
4., described in requiring according to right 1, right 2 and right 3, its feature is: when FTIS obtainsAfter infrared spectrum, next crystal is written into optical table by circular transmission turntable, and the crystal that has completed test is moved by circular rotating platformTo cleaning, drying unit, purge totally to be measured through high-temperature gas.
5., described in requiring according to right 1, right 2, right 3 and right 4, its feature is: circular rotating platform is through over-rotationCarry crystal and sample and carry out reciprocal testing, sample batch process and online detection are analyzed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510800397.7A CN105606718A (en) | 2015-11-19 | 2015-11-19 | High performance liquid chromatography and Fourier transform infrared spectroscopy combined interface device |
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| CN201510800397.7A CN105606718A (en) | 2015-11-19 | 2015-11-19 | High performance liquid chromatography and Fourier transform infrared spectroscopy combined interface device |
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| CN105606718A true CN105606718A (en) | 2016-05-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908533A (en) * | 2016-12-14 | 2017-06-30 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN107144659A (en) * | 2017-05-26 | 2017-09-08 | 宁海德宝立新材料有限公司 | A kind of device and its application method for improving infrared detection signal |
| GB2592965A (en) * | 2020-03-12 | 2021-09-15 | Agilent Technologies Inc | Rotatable analytical device |
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| US6689104B2 (en) * | 1997-11-14 | 2004-02-10 | Venetec International, Inc. | Medical line securement device |
| CN103383344A (en) * | 2013-06-24 | 2013-11-06 | 西安近代化学研究所 | Multi-crystal integrated attenuated total reflection accessory of infrared spectroscopy |
| CN104535539A (en) * | 2014-12-23 | 2015-04-22 | 南京航空航天大学 | Intermediate-infrared hollow optical fiber ATR coupling probe |
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2015
- 2015-11-19 CN CN201510800397.7A patent/CN105606718A/en active Pending
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|---|---|---|---|---|
| US6689104B2 (en) * | 1997-11-14 | 2004-02-10 | Venetec International, Inc. | Medical line securement device |
| CN103383344A (en) * | 2013-06-24 | 2013-11-06 | 西安近代化学研究所 | Multi-crystal integrated attenuated total reflection accessory of infrared spectroscopy |
| CN104535539A (en) * | 2014-12-23 | 2015-04-22 | 南京航空航天大学 | Intermediate-infrared hollow optical fiber ATR coupling probe |
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| ALAN M. ROBERTSON，ET AL: "Assessment of a thermospray interface for the coupling of high-performance liquid chromatography and Fourier transform infrared spectrometry", 《JOURNAL OF CHROMATOGRAPHY》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908533A (en) * | 2016-12-14 | 2017-06-30 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN106908533B (en) * | 2016-12-14 | 2019-11-12 | 宁海德宝立新材料有限公司 | A kind of application of metal oxide |
| CN107144659A (en) * | 2017-05-26 | 2017-09-08 | 宁海德宝立新材料有限公司 | A kind of device and its application method for improving infrared detection signal |
| CN107144659B (en) * | 2017-05-26 | 2019-02-01 | 宁海德宝立新材料有限公司 | A kind of device and its application method improving infrared detection signal |
| GB2592965A (en) * | 2020-03-12 | 2021-09-15 | Agilent Technologies Inc | Rotatable analytical device |
| GB2592965B (en) * | 2020-03-12 | 2023-02-22 | Agilent Technologies Inc | Rotatable analytical device |
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