CN102072945A - Chromatographic photoionization detector - Google Patents
Chromatographic photoionization detector Download PDFInfo
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- CN102072945A CN102072945A CN2010105948483A CN201010594848A CN102072945A CN 102072945 A CN102072945 A CN 102072945A CN 2010105948483 A CN2010105948483 A CN 2010105948483A CN 201010594848 A CN201010594848 A CN 201010594848A CN 102072945 A CN102072945 A CN 102072945A
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- photoionization detector
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Abstract
The invention relates to a chromatographic photoionization detector which comprises a tail blowing connector and a nozzle, wherein the tail blowing connector is arranged on a chromatographic connecting column connected with a chromatographic column and used for preventing the peak of a sample curve to be detected from widening or trailing; the nozzle is embedded into an ionization chamber and taken as an electrode to be connected with a collector connector through a probe to realize transmission and acquisition of voltage signals; the ionization chamber is provided with two air passages, wherein one is an exhaust port through which the residual gas in the detecting course is exhausted, and the other one is a curtain exhaust port and is used for blowing and cleaning the window of an ultraviolet lamp in the detecting course; the ionization chamber is connected with the fixed sleeve of the lamp through screw threads; the fixed sleeve of the lamp is tightly pressed with a lamp pressing sleeve embedded with the base of the ultraviolet lamp; the protective cover of the lamp is tightly pressed and sheathed with the ultraviolet lamp through the pressing spring of the lamp; and the ultraviolet lamp activates a voltage lead joint to be fixedly connected to the protective cover of the lamp through a tacking nut. The chromatographic photoionization detector improves the insufficient design of the conventional chromatographic photoionization detector and enhances the sensitivity, selectivity and stability of a PID (Proportion Integration Differentiation) detector.
Description
Technical field
The invention belongs to technical field of analytical instruments, particularly a kind of chromatogram photoionization detector.
Background technology
One of gas chromatography detector commonly used is got up in a year fast development surplus chromatogram photoionization detector (Photo Ionization Detector, the abbreviation PID) nearly 20.It utilizes optical radiation to make tested component ionization, produces signal.Its remolding sensitivity FID height 100-1000 doubly, especially to aromatic series and unsaturated compound.Selectivity is different because of light source.The existing many reports of the development of China PID and application, traditional PID detecting device, nozzle and electrode be design separately, complex structure; Uviol lamp intensifies general employing of voltage and is rigidly connected, and contact is bad, and reliability is low; The fixing spring compression that adopts of uviol lamp base, sealing is poor; The ionization chamber volume is bigger, is unfavorable for that component absorbs ultraviolet light and fully ionization, and inconvenience connection capillary column, has limited the sensitivity of detecting device; The uviol lamp window does not have automatic purging and cleans design, and residue attached to the window minute surface, influences ionizing efficiency in a large number, and generally, the user need pull down the uviol lamp clean window after using a period of time, has increased the maintenance difficulties of instrument like this, brings inconvenience to the user.
Summary of the invention
The purpose of this invention is to provide a kind of photoionization detector, as the detecting device of universality, advantages such as anti-interference, anti-poisoning can be widely used in the detecting device of gas chromatograph, online detection/monitor and portable or hand-held tester.
Can solve chromatogram photoionization detector reliability and all not high problem of sensitivity that present gas chromatographic detection adopts when being used for gas chromatograph.
Technical scheme of the present invention is that a kind of chromatogram photoionization detector comprises: a tail blown joint mouth is set on the chromatogram joint pin that is connected with chromatographic column, broadens or trail in order to prevent sample curve peak; One nozzle embeds ionization chamber and is connected with a collector joint by a probe as electrode, realizes voltage signal transmission and collection; Described ionization chamber is provided with two tunnel gas circuits, and one the tunnel is exhausr port so that the residual gas in the testing process is discharged by this exhausr port, and another road is that the curtain exhausr port is in order to purge cleaning to the uviol lamp window in testing process; Described ionization chamber is threaded with the lamp fixed cover; Described lamp fixed cover presses the lamp gland nested with the uviol lamp base; The lamp protective cover presses socket by lamp holddown spring and uviol lamp; Uviol lamp intensifies the voltage lead joint and is fixed in described lamp protective cover by marking closely nut.
Further, the material of described lamp gland is a teflon.
Further, the material of described lamp fixed cover is a stainless steel.
Further, the internal diameter of described ionization chamber is 2.5 millimeters to 6 millimeters, highly is 4.5 millimeters to 10 millimeters.
The chromatogram photoionization detector (PID) of microminiaturization of the present invention has comprised the body design of detecting device, the control of testing circuit and the innovative design of curtain gas circuit.Chromatographic column is packed column or capillary column.
Uviol lamp of the present invention intensifies the voltage connected mode and has changed existing design concept, uviol lamp intensifies outer employing of pressure-wire to be marked closely nut and fixes, the interior lamp holddown spring that connects, the lamp holddown spring is nested with uviol lamp, changed the elasticity connection into by original being rigidly connected, adopt spring compression type, improved reliability greatly.
The design of nozzle and electrode is to be one with nozzle and electrode design, and functional equivalent has been realized optimization in original separate design on the structure.
The uviol lamp fixed mode is nested with the uviol lamp base with teflon, and external application stainless steel lamp fixed cover compresses teflon, the stainless steel holder is threadedly connected to PID ionization pond body simultaneously, realization compresses, and the reliability height has thoroughly solved the sealing problem of PID ionization chamber and uviol lamp.
Ionization chamber volume of the present invention is less than 45ul (chamber body physical size diameter phi 2.5mm-φ 6mm, height 4.5mm-10mm), accomplished real miniaturized design, in the process that detects, sample has improved the sensitivity of PID detecting device greatly in indoor sufficient ionization.
Ionization chamber gas circuit design of the present invention, be in ionization chamber, to have increased the miniature gas circuit design of two-way, one the tunnel is gas discharge outlet, all residual gas all pass through this mouth and discharge, one the tunnel is that window purges gas circuit, in the process of using, can directly purge cleaning, reduce residual sample greatly, improve the service efficiency of uviol lamp in the adhering to of uviol lamp window to the uviol lamp window.
Miniature optical ionization detecting device of the present invention (PID) external physical dimensions diameter phi 25mm-φ 35mm, height 60mm-90mm.
Each parts of miniature optical ionization detecting device of the present invention (PID) adopt stainless steel, teflon, brass.
The invention has the beneficial effects as follows, broken existing P ID detector design thought, improved existing P ID detector design deficiency, improved the sensitivity of PID detecting device, selectivity and stability are particularly in nozzle and the incorporate design concept of electrode, to the futures analysis instrument, the particularly development of modern miniature analytical instrument has far-reaching reference.
Description of drawings
Fig. 1 is that chromatogram photoionization detector structure is formed synoptic diagram in one embodiment of the invention
Wherein, 2---the chromatographic column joint pin;
3---tail blown joint mouth;
4---nozzle;
5---the PID ionization chamber;
6---exhausr port;
7---the curtain air intake opening;
8---the stainless steel lamp fixed cover;
9---tygon tetrafluoro lamp gland;
10---uviol lamp;
11---the lamp holddown spring;
12---intensify the voltage lead joint;
13---the lamp protective cover;
14---the collector joint.
Fig. 2 is a gas chromatogram that adopts photoionization detector actual measurement of the present invention
Fig. 3 is another gas chromatogram that adopts photoionization detector actual measurement of the present invention
Fig. 4 is another gas chromatogram that adopts photoionization detector actual measurement of the present invention
Embodiment
Embodiment 1, and as shown in Figure 1, whole chromatogram photoionization detector main body is cylindrical, and external physical dimensions is diameter phi 27mm, height 81mm.Chromatographic column connects by chromatogram joint pin 2, broadens or trails in order to prevent the sample peak, has designed tail blown joint mouth 3 on the chromatogram joint pin.Nozzle 4 and electrode are one and are embedded in PID ionization chamber 5, are connected with collector joint 14 by probe, realize the transmission of voltage and the collection of signal.The volume of PID ionization chamber is 35 μ L, the design of two-way gas circuit is arranged in the PID ionization chamber, one the tunnel is exhausr port 6, all residual gas all pass through this mouth and discharge, one the tunnel is curtain air intake opening 7, in the process of using, can directly purge cleaning, reduce residual sample, improve the service efficiency of uviol lamp greatly in the adhering to of uviol lamp window to the uviol lamp window.Teflon lamp gland 9 is nested with uviol lamp 10 bases, external application stainless steel lamp fixed cover 8 compresses teflon lamp gland, and the stainless steel holder is threadedly connected to the PID ionization chamber simultaneously, realizes compressing, the reliability height has thoroughly solved the sealing problem of PID ionization chamber and uviol lamp.Uviol lamp intensifies voltage lead joint 12 and is fixed on the lamp protective cover 13 by marking closely nut; the interior lamp holddown spring 11 that connects, spring is nested with uviol lamp, has changed the elasticity connection into by original being rigidly connected; adopt spring compression type, in the contact performance that improves, also improved reliability.
Each parts of chromatogram photoionization detector adopt stainless steel, teflon, brass.
Below, by some experiments, verify chromatogram photoionization detector practical function of the present invention.
Shanghai Precision Scientific Apparatus Co., Ltd's GC126 gas chromatograph is joined PID detecting device of the present invention, chromatographic column: OV-101,, carrier gas: high purity nitrogen, air, hydrogen, flow velocity: 30mL/min, the flow velocity of make-up gas?: 5mL/min, sample size: 1mL, the injector temperature: 70 ℃, column temperature: 80 ℃, detector temperature: 100 ℃.
Test sample is benzene standard specimen (gas), and concentration: 0.1ppm, spirit are nitrogen.
Fig. 2 does carrier gas for the benzene standard specimen by nitrogen, the gas chromatogram that adopts the embodiment of the invention 1 described photoionization detector to detect.Continuous 5 sample introductions, as can be seen from the figure, PID detecting device of the present invention has very high response to the benzene standard model of 0.1ppm level, and noise is low to moderate 10 μ V, and signal to noise ratio (S/N ratio) is positioned at homemade analytical instrument industry prostatitis.The peak shape symmetry is sharp-pointed, no conditions of streaking.No matter retention time or peak area show good repeatability.Eventually the above, the PID detecting device of the present invention's design has high sensitivity and reliability.
Fig. 3 does carrier gas for the benzene standard specimen by air, the gas chromatogram that adopts the embodiment of the invention 1 described photoionization detector to detect.Continuous 5 sample introductions, as can be seen from the figure, the response that air is done carrier gas is 2/3 of a nitrogen, but it is convenient, and cheapness can be used for portable commercial apparatus.The peak shape symmetry is sharp-pointed, no conditions of streaking.No matter retention time or peak area show good repeatability.
Fig. 4 does carrier gas for the benzene standard specimen by helium, the gas chromatogram that adopts the embodiment of the invention 1 described photoionization detector to detect.Continuous 6 sample introductions, this figure show, when PID detecting device of the present invention is done carrier gas with hydrogen, and height when response is done carrier gas than nitrogen.The peak shape symmetry is sharp-pointed, no conditions of streaking.No matter retention time or peak area show good repeatability, can replace fid detector to be installed on portable chromatograph, the TOVC in analysis environments and the product.
Photoionization detector of the present invention pond volume is 35 μ L only, can directly link to each other with kapillary, and PID is to the benzene class, and the compound of band carbonyl has higher selectivity and sensitivity for analysis, so the PID detecting device that can be used as miniature chromatogram is used for TVOC and analyzes.Under the normal temperature, but TVOC need not just direct injected acquisition analysis result of enrichment.And PID detecting device available air of the present invention is done carrier gas, and is simple and safe.Signal to noise ratio (S/N ratio) has reached the standard of international advanced detecting device, and good repeatability becomes the reliable analysis tool of client.
Claims (4)
1. a chromatogram photoionization detector is characterized in that, comprising:
One tail blown joint mouth is set on the chromatogram joint pin that is connected with chromatographic column, broadens or trail in order to prevent sample curve peak;
One nozzle embeds ionization chamber and is connected with a collector joint by a probe as electrode, realizes voltage signal transmission and collection;
Described ionization chamber is provided with two tunnel gas circuits, and one the tunnel is exhausr port so that the residual gas in the testing process is discharged by this exhausr port, and another road is that the curtain exhausr port is in order to purge cleaning to the uviol lamp window in testing process;
Described ionization chamber is threaded with the lamp fixed cover;
Described lamp fixed cover presses the lamp gland nested with the uviol lamp base;
The lamp protective cover presses socket by lamp holddown spring and uviol lamp;
Uviol lamp intensifies the voltage lead joint and is fixed in described lamp protective cover by marking closely nut.
2. chromatogram photoionization detector as claimed in claim 1 is characterized in that the material of described lamp gland is a teflon.
3. chromatogram photoionization detector as claimed in claim 1 is characterized in that the material of described lamp fixed cover is a stainless steel.
4. chromatogram photoionization detector as claimed in claim 1 is characterized in that, the internal diameter of described ionization chamber is 2.5 millimeters to 6 millimeters, highly is 4.5 millimeters to 10 millimeters.
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| CN2010105948483A CN102072945A (en) | 2010-12-20 | 2010-12-20 | Chromatographic photoionization detector |
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| CN2010105948483A CN102072945A (en) | 2010-12-20 | 2010-12-20 | Chromatographic photoionization detector |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018164A (en) * | 2012-12-06 | 2013-04-03 | 深圳市南油诺安电子有限公司 | Automatic cleaning and zero setting system for light ion organic volatile gas detector |
| CN103575839A (en) * | 2012-07-18 | 2014-02-12 | 中国科学院电子学研究所 | High sensitivity photoionization detector |
| CN105842369A (en) * | 2016-03-10 | 2016-08-10 | 深圳市世纪龙晟科技发展有限公司 | Photoionization detector capable of realizing automatic flow control |
| CN106562676A (en) * | 2016-11-03 | 2017-04-19 | Tcl家用电器（中山）有限公司 | Water dispenser cold tank and water dispenser |
| CN109073612A (en) * | 2016-07-29 | 2018-12-21 | 霍尼韦尔国际公司 | Photoionization detector automates zero level calibration |
| US11162917B2 (en) | 2019-02-28 | 2021-11-02 | Honeywell International Inc. | Device for improving gas detection in photoionization detector |
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| CN2524244Y (en) * | 2002-02-10 | 2002-12-04 | 复旦大学 | Miniature flame ionizing detector |
| WO2008035634A1 (en) * | 2006-09-21 | 2008-03-27 | Hamamatsu Photonics K.K. | Ionizing device, mass analyzer, ion movability meter, electron capturing detector, and charged particle measuring device for chromatograph |
| CN101308125A (en) * | 2007-05-18 | 2008-11-19 | 华瑞科学仪器(上海)有限公司 | Photoionization detector, gas-chromatography detection system and chromatographic detector method |
| CN101750463A (en) * | 2008-12-19 | 2010-06-23 | 中国科学院大连化学物理研究所 | Small-size hydrogen flame ionization detector |
| CN201926650U (en) * | 2010-12-20 | 2011-08-10 | 上海精密科学仪器有限公司 | Chromatographic photoionization detector |
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2010
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2524244Y (en) * | 2002-02-10 | 2002-12-04 | 复旦大学 | Miniature flame ionizing detector |
| WO2008035634A1 (en) * | 2006-09-21 | 2008-03-27 | Hamamatsu Photonics K.K. | Ionizing device, mass analyzer, ion movability meter, electron capturing detector, and charged particle measuring device for chromatograph |
| CN101308125A (en) * | 2007-05-18 | 2008-11-19 | 华瑞科学仪器(上海)有限公司 | Photoionization detector, gas-chromatography detection system and chromatographic detector method |
| CN101750463A (en) * | 2008-12-19 | 2010-06-23 | 中国科学院大连化学物理研究所 | Small-size hydrogen flame ionization detector |
| CN201926650U (en) * | 2010-12-20 | 2011-08-10 | 上海精密科学仪器有限公司 | Chromatographic photoionization detector |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103575839A (en) * | 2012-07-18 | 2014-02-12 | 中国科学院电子学研究所 | High sensitivity photoionization detector |
| CN103575839B (en) * | 2012-07-18 | 2015-04-22 | 中国科学院电子学研究所 | High sensitivity photoionization detector |
| CN103018164A (en) * | 2012-12-06 | 2013-04-03 | 深圳市南油诺安电子有限公司 | Automatic cleaning and zero setting system for light ion organic volatile gas detector |
| CN105842369B (en) * | 2016-03-10 | 2017-11-28 | 深圳市世纪龙晟科技发展有限公司 | A kind of self-controlling flow photoionization detector |
| CN105842369A (en) * | 2016-03-10 | 2016-08-10 | 深圳市世纪龙晟科技发展有限公司 | Photoionization detector capable of realizing automatic flow control |
| CN109073612A (en) * | 2016-07-29 | 2018-12-21 | 霍尼韦尔国际公司 | Photoionization detector automates zero level calibration |
| US10969371B2 (en) | 2016-07-29 | 2021-04-06 | Honeywell International Inc. | Photoionization detector automated zero level calibration |
| CN109073612B (en) * | 2016-07-29 | 2022-03-29 | 霍尼韦尔国际公司 | Automatic zero-order calibration of photoionization detectors |
| US11480554B2 (en) | 2016-07-29 | 2022-10-25 | Honeywell International Inc. | Photoionization detector automated zero level calibration |
| US11714073B2 (en) | 2016-07-29 | 2023-08-01 | Honeywell International Inc. | Photoionization detector automated zero level calibration |
| CN106562676A (en) * | 2016-11-03 | 2017-04-19 | Tcl家用电器（中山）有限公司 | Water dispenser cold tank and water dispenser |
| US11162917B2 (en) | 2019-02-28 | 2021-11-02 | Honeywell International Inc. | Device for improving gas detection in photoionization detector |
| US11604163B2 (en) | 2019-02-28 | 2023-03-14 | Honeywell International Inc. | Device for improving gas detection in photoionization detector |
| US11965855B2 (en) | 2019-02-28 | 2024-04-23 | Honeywell International Inc. | Device for improving gas detection in photoionization detector |
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Owner name: SHANGHAI INESA ANALYTICAL INSTRUMENT CO., LTD. Free format text: FORMER OWNER: SHANGHAI CO., LTD OF FINE SCIENTIFIC INSTRUMENTS Effective date: 20120423 |
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Effective date of registration: 20120423 Address after: 200233 -01 room, 18 West floor, 481 Guiping Road, Xuhui District, Shanghai Applicant after: Shanghai INESA Analytical Instrument Co., Ltd. Address before: 200233 No. 7, Cangwu Road, Shanghai, Xuhui District Applicant before: Shanghai Co., Ltd of Fine Scientific Instruments |
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Application publication date: 20110525 |