CN104597177A - Gas chromatography and inductively coupled plasma mass spectrometry combined electric heating hose and interface device - Google Patents
Gas chromatography and inductively coupled plasma mass spectrometry combined electric heating hose and interface device Download PDFInfo
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- CN104597177A CN104597177A CN201510037403.8A CN201510037403A CN104597177A CN 104597177 A CN104597177 A CN 104597177A CN 201510037403 A CN201510037403 A CN 201510037403A CN 104597177 A CN104597177 A CN 104597177A
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- flexible pipe
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- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title abstract description 5
- 238000005485 electric heating Methods 0.000 title abstract 8
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title abstract 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 71
- 238000004817 gas chromatography Methods 0.000 claims abstract description 48
- 239000012774 insulation material Substances 0.000 claims abstract description 9
- 238000010168 coupling process Methods 0.000 claims description 22
- 238000000918 plasma mass spectrometry Methods 0.000 claims description 21
- 230000001105 regulatory effect Effects 0.000 claims description 21
- 239000012159 carrier gas Substances 0.000 claims description 18
- 230000001276 controlling effect Effects 0.000 claims description 15
- 230000008878 coupling Effects 0.000 claims description 14
- 238000005859 coupling reaction Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000004891 communication Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 101100520231 Caenorhabditis elegans plc-3 gene Proteins 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 finally Proteins 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004092 self-diagnosis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
Abstract
The invention discloses an electric heating hose and an interface device for gas chromatography and inductively coupled plasma mass spectrometry, wherein the electric heating hose comprises: one end of the tube body is a gas chromatography access port, the other end of the tube body is an inductively coupled plasma mass spectrometry access port, and the tube body is provided with an inclined gas carrying tube communicated with the inside of the tube body; the electric heating wire is wound outside the pipe body; the heat insulation material is wrapped outside the electric heating wire; and the temperature sensor is arranged in the tube body. The interface device includes: the electrically heated hose of the present invention; the temperature control device is respectively and electrically connected with the electric heating wire of the electric heating hose and the temperature sensor; and the control computer is in communication connection with the temperature control device and is used for sending a temperature control signal to the temperature control device and displaying the temperature value of the electric heating hose sent back by the temperature control device. The interface system can not only ensure that a measured sample transmitted to the ICP-MS by the GC is always maintained in a gas phase state, but also carry out digital display control on the heating temperature of the interface and improve the temperature control precision.
Description
Technical field
The present invention relates to interface arrangement, particularly relate to electrical heating flexible pipe and the interface arrangement of a kind of gas chromatography (GC) and inductivity coupled plasma mass spectrometry (ICP-MS) coupling.
Background technology
In recent years, along with environmental science, the fast development of life science and modern Analytical Methods of Trace, the morphological analysis of element is obtained and pays close attention to more and more widely, and ICP-MS analytical technology application is increasingly universal, various coupling technique is widely used, wherein, gas chromatography-inductivity coupled plasma mass spectrometry coupling technique (GC-ICP-MS) is a kind of trace analysis methods that can be used for element morphology in several samples, it is highly sensitive to have, selectivity is high and can carry out multielement simultaneously, the feature of isotope detection and gaining great popularity, therefore very important to the development of this coupling technique interface arrangement.
In the master thesis of 2008, deliver the paper that autograph is " based on the lead of GC-ICPMS and new interface newly interior mark and the research of new deriving method of mercury morphological analysis simultaneously " severe winter, wherein describe a kind of numerical control warming module that utilizes to the gas-carrier pipeline constant temperature of GC, and the importing hydrogen of the ICP-MS of preheating simultaneously, and at kapillary overcoat one copper pipe, again copper pipe is inserted GC column oven, the new interface of copper pipe outer wrapping insulation material, hot-air in column oven diffuses in copper pipe, make temperature in copper pipe consistent with column oven, ensure that the high-temperature gas sample flowed out from gas chromatography is unlikely to time condensation and is adsorbed on capillary column inwall transmitting procedure.
2008, the autograph being published in " Anal Bioanal Chem " by Jens HeilmannKlaus G.Heumann is describe the connection of a kind of adapter glass for GC and ICP-MS in the article of " Development of a species-specific isotope dilution GC-ICP-MS method for thedetermination of thiophene derivates in petroleum products ", and settle one section of silver-colored line for heating the gas in it in adapter glass and ICP-MS plasma quarter bend, heating-up temperature regulates the power of power supply to control according to typical curve.
In the method that above document is used, all the interface arrangement needed for GC and ICP-MS coupling technique is studied, but still have the following disadvantages: the former transfer conduit between GC and numerical control warming module wraps up insulation material, but have ignored the problem that between numerical control warming module and ICP-MS, in gas circuit, sample temperature controls; The latter has settled Heating Silver line in the quarter bend of adapter glass and ICP-MS, but have ignored the problem that between GC and adapter glass, in gas circuit, sample temperature controls.
Summary of the invention
Based on the problem existing for above-mentioned prior art, the invention provides electrical heating flexible pipe and the interface arrangement of a kind of gas chromatography and inductivity coupled plasma mass spectrometry coupling, can not only ensure that the sample being transferred to ICP-MS by GC maintains gas phase state always, and digital display control can be carried out to this interface heating-up temperature, and temperature control precision can reach ± and 0.3 DEG C.
For solving the problems of the technologies described above, the invention provides the electrical heating flexible pipe of a kind of gas chromatography and inductivity coupled plasma mass spectrometry coupling, comprising:
Body, one end is gas chromatography access interface, and the other end is inductivity coupled plasma mass spectrometry access interface, and this body is provided with and the inclination carrier gas pipe be communicated with in body;
Heating wire, is wrapped in outside described body;
Insulation material, is wrapped in outside described heating wire;
Temperature sensor, is located in described body.
The embodiment of the present invention provides the interface system of a kind of gas chromatography and inductivity coupled plasma mass spectrometry coupling, comprising:
Electrical heating flexible pipe of the present invention;
Temperature regulating device, is electrically connected with the heating wire of described electrical heating flexible pipe and temperature sensor respectively;
Computer for controlling, communicates to connect with described temperature regulating device, sends temperature control signal and show the temperature value of the described electrical heating flexible pipe that described temperature regulating device is beamed back to described temperature regulating device.
Beneficial effect of the present invention is: by having gas chromatography access interface, heating wire and insulation material is set gradually outside the body of inductivity coupled plasma mass spectrometry access interface and inclination carrier gas pipe, and in body set temperature sensor, this electrical heating flexible pipe can be coordinated with outside temperature regulating device, accurate temperature controlling and in real time displays temperature, and then when making to be used in gas chromatography and inductivity coupled plasma mass spectrometry coupling, can not only ensure that the sample being transferred to ICP-MS by GC maintains gas phase state always, and digital display control can be carried out to this interface heating-up temperature, promote temperature control precision.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation of the electrical heating flexible pipe that the embodiment of the present invention provides;
Parts in Fig. 1 representated by each label are: 7: body, 8: heating wire, 9: insulation material, 10: temperature sensor, 11: gas chromatography access interface, 12: inductivity coupled plasma mass spectrometry access interface, 13: inclination carrier gas pipe;
Fig. 2 is the structural representation of the interface system that the embodiment of the present invention provides;
Parts in Fig. 2 representated by each label are: 1: computer for controlling, 2: electrical heating flexible pipe, 3: programmable logic controller (PLC) (PLC), 4: temperature survey expansion module, 5: solid-state relay, 6: alarm.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
As shown in Figure 1, the embodiment of the present invention provides the electrical heating flexible pipe of a kind of gas chromatography (GC) with inductivity coupled plasma mass spectrometry (ICP-MS) coupling, comprise: body, this body one end is gas chromatography access interface, the other end is inductivity coupled plasma mass spectrometry access interface, and this body is provided with and the inclination carrier gas pipe be communicated with in body; Preferably, body can adopt PTFE material body or stainless steel body;
Heating wire, is wound around and is located at outside body, can heat in body;
Insulation material, is wrapped in outside heating wire, can to heating wire and body inside holding;
Temperature sensor, is located in body, can obtain the temperature signal in body.
In above-mentioned electrical heating flexible pipe, inclination carrier gas tube and tube body is structure as a whole, this inclination carrier gas pipe is in the gas chromatography access interface side of described body, near gas chromatography access interface, to gas chromatography access interface lopsidedness, namely the Way in of inclination carrier gas pipe is towards inductivity coupled plasma mass spectrometry access interface.
As shown in Figure 2, the embodiment of the present invention also provides the interface arrangement of a kind of gas chromatography and inductivity coupled plasma mass spectrometry coupling, comprising:
Electrical heating flexible pipe, adopts above-mentioned electrical heating flexible pipe;
Temperature regulating device, is electrically connected with the heating wire of electrical heating flexible pipe and temperature sensor respectively;
Computer for controlling, communicates to connect with temperature regulating device, sends temperature control signal and show the temperature value of the electrical heating flexible pipe that temperature regulating device is beamed back to temperature regulating device.Function software can be installed in this computer for controlling, by the plc communication with temperature regulating device, for the temperature of target setting temperature with the flexible pipe of display electrical heating in real time, and control unlatching and the stop button of the operation of display PLC program.
In above-mentioned interface arrangement, temperature regulating device comprises: programmable logic controller (PLC) (PLC), is electrically connected respectively, and communicates to connect with computer for controlling with solid-state relay and temperature survey expansion module;
Solid-state relay, is electrically connected with the heating wire of electrical heating flexible pipe;
Temperature survey expansion module, is electrically connected with the temperature sensor of electrical heating flexible pipe.
This temperature regulating device course of work is: the electrical heating flexible pipe temperature sensed is real-time transmitted to temperature survey expansion module by the temperature sensor of electrical heating flexible pipe, temperature survey expansion module is connected with PLC, the input of the temperature value after sending PLC is become through temperature survey expansion module, PLC passes through plug-in, control the make-and-break time of solid-state relay, thus control the heating-up temperature of electrical heating flexible pipe.
Above-mentioned interface system also comprises: fault alarm, be electrically connected with the PLC of temperature regulating device, when temperature survey expansion module exist fault or other faults cause that in electrical heating flexible pipe, temperature is uncontrolled time, alarm equipment alarm, flashing light with buzzing, remind user that this system works is abnormal, PLC transports auto-line-ending simultaneously.
The specific embodiment of the present invention is described in detail below in conjunction with Fig. 2:
In Fig. 2,1 is the computer for controlling of GC, ICP-MS and interface arrangement of the present invention, for installing the control software design of this interface system, provides target temperature to set and real time temperature display panel, and the unlatching of temperature regulating device operation and stop button; 2 is electrical heating flexible pipe, for transmitting sample; 3 is programmable logic controller (PLC) (PLC), for loading temperature control program, controlling the heating-up temperature of electrical heating flexible pipe 2 and exporting the fault alarm information of this interface system; 4 is temperature survey expansion module, and the output of its respective channel, as the input of PLC 3, provides real-time temperature values; 5 is solid-state relay, and its make-and-break time decides the working time of the electrical heating wire of electrical heating flexible pipe 2; 6 is alarm, reminds this interface system operation irregularity of user, simultaneously the auto-line-ending of PLC 3 Program fortune.
The workflow of interface arrangement of the present invention is: be first connected with GC one end of electrical heating flexible pipe 2, and the other end connects ICP-MS, and the inclination carrier gas pipe in the middle of electrical heating flexible pipe 2 connects carrier gas passage, then, by being arranged on the control software design on computer for controlling 1 by the target temperature setting value of electrical heating flexible pipe 2 write PLC 3, finally, PLC 3 controls the make-and-break time of solid-state relay 5 by plug-in according to the difference between the real-time temperature values of electrical heating flexible pipe and target temperature setting value, thus control the final thermostat temperature of electrical heating flexible pipe 2, this environment temperature that namely between GC-ICP-MS, sample transmits, in this process, real-time temperature values is by the built-in temperature sensor senses of electrical heating flexible pipe 2 and send temperature survey expansion module 4 to, become by temperature survey expansion module 4 again and deliver to PLC 3, between GC and ICP-MS, the temperature value of gas circuit environment shows in real time by the control software design of computer for controlling 1.There is fault or other faults cause the uncontrolled alarm of temperature in electrical heating flexible pipe at temperature survey expansion module 4 in alarm 6, flashing light, also with buzzing, reminds this interface arrangement operation irregularity of user, simultaneously the auto-line-ending of PLC 3 Program fortune.
Structure and the function of electrical heating flexible pipe 2 of the present invention is described in detail below in conjunction with Fig. 1:
In Fig. 1,7 is the body of electrical heating flexible pipe 2, and for transmitting sample, body 7 outside is wound around heating wire 8, heating wire 8 outer wrap insulation material 9,10 is temperature sensor, and the real time temperature for electrical heating flexible pipe 2 exports, and 11 is the port connecting GC, 12 for connecting the port of ICP-MS, 13 is the carrier gas input port of inclination, and its position is held near GC, to shift to an earlier date preheated carrier gas.Electrical heating flexible pipe 2 middle tube body 7 is for meeting coupling technique specific customization, body 7 wherein for transmitting the electrical heating flexible pipe of sample is made as integrative-structure with inclination carrier gas pipe 13, overall gas circuit bore can keep size constant and frozen-free point in gas circuit, ensure the homogeneity of flow velocity in sample transfer process, carrier gas has angular slope when entering body, maximum separated sample can be loaded into ICP-MS, reduce adverse current.In addition, the length of body 2 is depending on the distance between GC and ICP-MS, inner air path diameter can customize according to different demand, heating and thermal insulation temperature determines depending on gas path pipe material in flexible pipe: if body adopts PTFE material, maximum temperature can reach 220 DEG C, if body adopts stainless steel maximum temperature can reach 400 DEG C.
Interface system of the present invention is used for GC-ICP-MS coupling technique, be different from traditional interfacing, the software operation of computer for controlling, programmable logic controller (PLC) (PLC) temperature programmed control, electrical heating flexible pipe heating and thermal insulation and fault alarm are organically combined, can precise control of temperature, performance is more stable, safe and reliable, for gas circuit between GC and ICP-MS provides stable temperature environment, make sample remain gaseous state in transmitting procedure, thus ensure that GC-ICP-MS coupling technique is used for precision and the accuracy of sample analysis.This interface system is used for GC-ICP-MS coupling technique following advantage:
1. introduce electrical heating flexible pipe, can be the temperature environment that gas circuit between GC and ICP-MS provides stable, ensure that sample maintains gas phase state all the time in transmitting procedure, thus improve analysis precision and the accuracy of GC-ICP-MS;
2. programmable logic controller (PLC) (PLC) conventional in industry control is introduced, compared with temperature controller conventional in conventional interface techniques, cost performance, reliability are higher, and use more flexible, PLC plug-in can be changed according to demand at any time with optimized interface performance, realize this invention as by coding and GC synchronization program heats up;
3. temperature-controlled precision is high, and the accessible temperature-controlled precision of traditional interfacing is usually at ± 0.5 DEG C, and this invention adopts PLC and temperature survey expansion module temperature accuracy can be controlled at ± 0.3 DEG C;
4. sample separation is effective, body and carrier gas access port for transmitting the electrical heating flexible pipe of sample are made as integrative-structure, overall gas circuit caliber size is constant, ensure the homogeneity of flow velocity in sample transfer process, and carrier gas has angular slope when entering body, maximum separated sample can be loaded into ICP-MS, reduce adverse current;
5. computer for controlling software control and Temperature displaying, operation can more convenient, monitor interface temperature intuitively;
6. the less trouble of PLC, perfect self diagnosis and Presentation Function, add the cooperation of plug-in and external alert device, make the stability of this invention and security higher;
7. easy and simple to handle, applied widely, this interface arrangement, independent of outside GC and ICP-MS, without the need to fully understanding structure or the built-in temperature controlling program of GC/ICP-MS, only can need be matched with GC, ICP-MS of each manufacturer production by the conversion head of different model.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. an electrical heating flexible pipe for gas chromatography and inductivity coupled plasma mass spectrometry coupling, is characterized in that, comprising:
Body, one end is gas chromatography access interface, and the other end is inductivity coupled plasma mass spectrometry access interface, and this body is provided with and the inclination carrier gas pipe be communicated with in body;
Heating wire, is wound around and is located at outside described body;
Insulation material, is wrapped in outside described heating wire;
Temperature sensor, is located in described body.
2. the electrical heating flexible pipe of gas chromatography according to claim 1 and inductivity coupled plasma mass spectrometry coupling, it is characterized in that, described inclination carrier gas pipe and described body are structure as a whole, this inclination carrier gas pipe is in the gas chromatography access interface side of described body, to described gas chromatography access interface lopsidedness.
3. the electrical heating flexible pipe of gas chromatography according to claim 1 and 2 and inductivity coupled plasma mass spectrometry coupling, is characterized in that, described body adopts PTFE material body or stainless steel body.
4. an interface arrangement for gas chromatography and inductivity coupled plasma mass spectrometry coupling, is characterized in that, comprising:
Electrical heating flexible pipe described in any one of claims 1 to 3;
Temperature regulating device, is electrically connected with the heating wire of described electrical heating flexible pipe and temperature sensor respectively;
Computer for controlling, communicates to connect with described temperature regulating device, sends temperature control signal and show the temperature value of the described electrical heating flexible pipe that described temperature regulating device is beamed back to described temperature regulating device.
5. the interface arrangement of gas chromatography according to claim 4 and inductivity coupled plasma mass spectrometry coupling, is characterized in that, described temperature regulating device comprises:
Programmable logic controller (PLC), is electrically connected with solid-state relay and temperature survey expansion module respectively, and communicates to connect with described computer for controlling;
Described solid-state relay, is electrically connected with the heating wire of described electrical heating flexible pipe;
Described temperature survey expansion module, is electrically connected with the temperature sensor of described electrical heating flexible pipe.
6. the interface arrangement of the gas chromatography according to claim 4 or 5 and inductivity coupled plasma mass spectrometry coupling, it is characterized in that, also comprise: fault alarm, be electrically connected with the programmable logic controller (PLC) of described temperature regulating device, report to the police when temperature regulating device breaks down.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510037403.8A CN104597177B (en) | 2015-01-23 | 2015-01-23 | Gas chromatography and inductively coupled plasma mass spectrometry combined electric heating hose and interface device |
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| CN201510037403.8A CN104597177B (en) | 2015-01-23 | 2015-01-23 | Gas chromatography and inductively coupled plasma mass spectrometry combined electric heating hose and interface device |
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| CN104597177A true CN104597177A (en) | 2015-05-06 |
| CN104597177B CN104597177B (en) | 2017-02-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110632233A (en) * | 2019-10-24 | 2019-12-31 | 上海裕达实业有限公司 | Constant temperature chromatographic device |
| CN115308324A (en) * | 2022-07-28 | 2022-11-08 | 天津国科医工科技发展有限公司 | Transmission line and device for combined use of gas chromatograph and mass spectrometer, temperature control transmission line and method |
| CN116136520A (en) * | 2021-11-18 | 2023-05-19 | 株式会社岛津制作所 | Gas chromatograph device |
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| CN104597177B (en) | 2017-02-22 |
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Effective date of registration: 20170117 Address after: 102628 Beijing City, Daxing District North Road (East) No. 22, No. 1 building, room A701 A708 Applicant after: BGRIMM DETECTION TECHNOLOGY CO.,LTD. Applicant after: BEIJING GENERAL Research Institute OF MINING AND METALLURGY Address before: 100160 Beijing City, South West Fourth Ring Road, Fengtai District, No. 188 headquarters base area, building eighteen, No. 23 Applicant before: BEIJING GENERAL Research Institute OF MINING AND METALLURGY |
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Address after: 102628 rooms a708 and A701, building 1, 22 Beixing Road (East Section), Daxing District, Beijing Patentee after: Beikuang Testing Technology Co.,Ltd. Address before: 102628 rooms a708 and A701, building 1, 22 Beixing Road (East Section), Daxing District, Beijing Patentee before: BGRIMM DETECTION TECHNOLOGY CO.,LTD. |
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