CN101403732A - Gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus - Google Patents
Gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus Download PDFInfo
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- CN101403732A CN101403732A CNA2008100797884A CN200810079788A CN101403732A CN 101403732 A CN101403732 A CN 101403732A CN A2008100797884 A CNA2008100797884 A CN A2008100797884A CN 200810079788 A CN200810079788 A CN 200810079788A CN 101403732 A CN101403732 A CN 101403732A
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Abstract
The invention provides a gas chromatography static headspace column head temperature-control pressure difference feeding device, consisting of a gasification chamber, a sample chamber and a carrier passage which is communicated with the gasification chamber and the sample chamber. The feeding device is characterized in that: the sample chamber is arranged in the gasification chamber; and the gasification chamber is connected with a chromatographic column by a capillary connection pipe. Compared with the prior art, the feeding device has the technical progress effects as follows: 1. a solid sample is fixed in a quartz glass liner pipe, thus effectively ensuring the constant temperature during the feeding process; 2. the gasification chamber is connected with the chromatographic column by the capillary connection pipe, therefore, the dead volume is extremely slight, the feeding is concentrative, and the sealed design ensures no cross contamination and sample loss during the feeding process; and 3. a carrier passage is added above the column head and on the lower surface of the capillary connection pipe; the on/off of the carrier passage is controlled by a carrier valve; furthermore, pressure difference is generated by the carrier valve with a feeding valve in a mode that one is switched on and the other is switched off so as to control the feeding of the sample; and the feeding quantity is convenient for adjustment, the repeatability is good, the operation is simple, convenient and economical, and the feeding quantity is convenient to be controlled.
Description
Technical field
The present invention relates to a kind of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus and method, belong to gas chromatographicanalyzer device matching component technical field.
Background technology
The headspace gas chromatography analysis is the most effectual way that the volatile ingredient in the liquid or solid sample is analyzed, as the analysis of volatile ingredient in the plastic packing bag, and after the people works in poisonous environment, poisonous component analysis on Content etc. in the body fluid.The headspace gas chromatography analysis normally places sample airtight constant temperature system, when gas--liquid (Gu gas---) after two-phase reached thermodynamic equilibrium, sampling was measured gas phase with gas chromatographic analysis and is formed.Sampling device commonly used comprises:
1) balanced type compression system (Balanced-Pressure System), working method is:
Reach thermal equilibrium state after the sample heating; Feed the carrier gas pressurization with conduit; Sample is with the carrier gas sample introduction.The environment of balanced type pressurization input mode is airtight, does not almost have movably parts in the whole sample introduction process, and sample enters the gas phase inner analysis with carrier gas, so reappearance is very excellent.But the absolute sample volume of this input mode can't know, and also suitable big of its dead volume.
2) quantitatively encircling compression system (Pressure-Loop System) working method is:
Reach thermal equilibrium state after the sample heating; Pressurization is introduced quantitatively ring with sample; Carrier gas is squeezed into the transmission channel sample introduction with sample.This mode is squeezed into the transmission channel sample introduction after with six-way valve sample being full of quantitative ring, and sample size is known.Sample also is to be brought in the gas chromatograph by carrier gas, thereby has the problem of carrier gases dilute in quantitatively encircling, and causes the decline of sensitivity.The shortcoming of this mode maximum is the problem that cross pollution takes place unavoidablely, causes the appearance of " ghost peak ".
Except the above-mentioned defective of listing respectively, no matter be balanced type compression system or pressurization sampling system, after sample is extracted out by the head space bottle, all be to enter gas chromatograph by transmission pipeline.The material that adopts mostly is inert metals such as nickel or Silcosteel alloy.Because its tube wall is rugged and rough, the generation of dead volume, cross pollution and sample residence time in pipeline is long and cause the peak type to widen, and these all are the problems that transmission channel is brought.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art defective, a kind of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus is provided, change traditional sample intake passage, to reduce dead volume and to ensure that n.s. runs off in the sample introduction process.
Technical scheme of the present invention is achieved in that this gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus, constitute by vaporizer, sample chamber and the carrier gas passage that communicates with it, it is characterized in that: the sample chamber is placed in the vaporizer, and vaporizer is connected by the capillary connecting pipe with chromatographic column.
Described gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus, the vaporizer top is provided with nut, the vaporizer bottom is provided with the capillary connecting pipe and is connected with the injection port of chromatographic column, sidewall is provided with carrier gas passage, the other end of carrier gas passage communicates with injection port, described sample chamber is the quartz glass internal lining pipe that places vaporizer, and internal lining pipe is provided with the carrier gas air admission hole.
Described gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus is characterized in that: described vaporizer outer wall is provided with temperature control modules.
Described gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus, the link of described carrier gas passage and vaporizer and injection port is provided with carrier gas valve and sampling valve respectively.
The sample injection method of described gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus, step is as follows:
A, solid sample is ground into a certain size particle, with the glass wool fixed placement in the bottom of quartz glass internal lining pipe;
B, quartz glass internal lining pipe top with rubber gasket through the nut sealing of exerting pressure; Open the carrier gas valve, close sampling valve, with temperature control module the quartz glass internal lining pipe is heated then;
C, treat that under design temperature the gas-solid two-phase of sample reaches thermodynamic equilibrium after, open sampling valve, close the carrier gas valve, sample enters chromatographic column through the capillary connecting pipe under air pressure promotes separates;
D, character and chromatographic column type are adjusted sample injection time per sample, after sample introduction finishes, close sampling valve, open the carrier gas valve, and a sample introduction circulation is finished, and sample can repeat sample introduction repeatedly.
The technical solution used in the present invention compared with prior art its technical progress effect shows:
1, solid sample is fixed in the quartz glass internal lining pipe, has ensured temperature constant in the sample introduction process effectively.
2, be connected by the capillary connecting pipe between vaporizer and the chromatographic column, dead volume is extremely small, and sample introduction is concentrated, and its airtight design has also ensured in the sample introduction process not have cross pollution, and n.s. runs off.
3, above column cap, increased by one tunnel carrier gas below the capillary connecting pipe,, and produce pressure reduction by this mode of opening those passes with sampling valve by carrier gas valve control carrier gas break-make, the control sample feeding, sample size is convenient to regulate, and favorable reproducibility, is convenient to control sample size at easy and simple to handle, economy.
Description of drawings
Fig. 1 is among the structural representation figure of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus:
1, sealing rubber pad 2, nut 3, quartz glass internal lining pipe 4, temperature control module
5, sampling valve 6, vaporizer 7, solid sample 8, glass wool
9, tensimeter 10, carrier gas 11, capillary connecting pipe 12, injection port
13, carrier gas valve 14, chromatographic column 15, carrier gas passage 16, carrier gas air admission hole
Embodiment
Gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus shown in Figure 1, by vaporizer 6, sample chamber and the carrier gas passage 15 that communicates with it with there is capillary connecting pipe 11 to constitute, innovative point of the present invention is that the sample chamber is placed in the vaporizer, and vaporizer is connected by capillary connecting pipe 11 with chromatographic column.
The vaporizer bottom is provided with capillary connecting pipe 11 and is connected with the injection port 12 of chromatographic column, and dead volume is extremely small, and sample introduction is concentrated, and its airtight design has also ensured in the sample introduction process not have cross pollution, and n.s. runs off.
Vaporizer of the present invention 6 tops are provided with nut 2, sidewall is provided with carrier gas passage 15, the other end of carrier gas passage communicates with injection port, the link of carrier gas passage and vaporizer and injection port is provided with carrier gas valve 5 and sampling valve 13 respectively, produce pressure reduction by carrier gas valve and sampling valve by this mode of opening those passes, the control sample feeding.
Sample chamber of the present invention is the quartz glass internal lining pipe 3 that places vaporizer, internal lining pipe is provided with carrier gas air admission hole 16, the vaporizer outer wall is provided with temperature control modules 4, and solid sample is fixed in the quartz glass internal lining pipe, has ensured temperature constant in the sample introduction process effectively.
The course of work of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus of the present invention is as follows:
A, at first solid sample 7 is ground into a certain size particle, with glass wool 8 fixed placement in the bottom of quartz glass internal lining pipe 3;
B, quartz glass internal lining pipe 3 tops with rubber gasket 1 through the sealing of exerting pressure of heat radiation nut 2; Open carrier gas valve 13, close sampling valve 5, using 4 pairs of quartz glass internal lining pipes of temperature control module (3) to be heated to then needs temperature;
C, treat that under design temperature the gas-solid two-phase of sample reaches thermodynamic equilibrium after, open sampling valve 5, close carrier gas valve 13, sample enters chromatographic column 14 through capillary connecting pipe 11 under air pressure promotes separates;
D, character and chromatographic column type are adjusted sample injection time per sample, are generally 3-10 second, after sample introduction finishes, close sampling valve, open the carrier gas valve, and a sample introduction circulation is finished, and sample can repeat sample introduction repeatedly.
Foregoing description only proposes as the enforceable technical scheme of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus of the present invention, not as the single restrictive condition to its structure itself.
Claims (5)
1, a kind of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus is made of vaporizer (6), sample chamber and the carrier gas passage (15) that communicates with it, and it is characterized in that: the sample chamber is placed in the vaporizer, and vaporizer is connected by the capillary connecting pipe with chromatographic column.
2, gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus according to claim 1, it is characterized in that: the vaporizer top is provided with nut (2), the vaporizer bottom is provided with capillary connecting pipe (11) and is connected with the injection port (12) of chromatographic column (14), sidewall is provided with carrier gas passage (15), the other end of carrier gas passage communicates with injection port, described sample chamber is the quartz glass internal lining pipe (3) that places vaporizer, and internal lining pipe is provided with carrier gas air admission hole (16).
3, gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus according to claim 1 is characterized in that: described vaporizer outer wall is provided with temperature control modules (4).
4, gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus according to claim 1 is characterized in that: the link of described carrier gas passage and vaporizer and injection port is provided with carrier gas valve (5) and sampling valve (13) respectively.
5, the sample injection method of gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus according to claim 1 is characterized in that step is as follows:
A, solid sample (7) is ground into a certain size particle, with glass wool (8) fixed placement in the bottom of quartz glass internal lining pipe (3);
B, quartz glass internal lining pipe (3) top with rubber gasket (1) through nut (2) sealing of exerting pressure; Open carrier gas valve (13), close sampling valve (5), use temperature control module (4) that quartz glass internal lining pipe (3) is heated then;
C, treat that under design temperature the gas-solid two-phase of sample reaches thermodynamic equilibrium after, open sampling valve (5), close carrier gas valve (13), sample enters chromatographic column (14) through capillary connecting pipe (11) under air pressure promotes separates;
D, character and chromatographic column type are adjusted sample injection time per sample, after sample introduction finishes, close sampling valve, open the carrier gas valve, and a sample introduction circulation is finished, and sample can repeat sample introduction repeatedly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100797884A CN101403732A (en) | 2008-11-19 | 2008-11-19 | Gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus |
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| CNA2008100797884A CN101403732A (en) | 2008-11-19 | 2008-11-19 | Gas-chromatography static top hollow column dead temperature-control pressure-difference sampling apparatus |
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| CN101403732A true CN101403732A (en) | 2009-04-08 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104950057A (en) * | 2015-04-03 | 2015-09-30 | 常州磐诺仪器有限公司 | Sample inlet of micro packed column |
| CN106706745A (en) * | 2017-02-17 | 2017-05-24 | 神华集团有限责任公司 | Measuring device and measuring method of water content in coal liquefaction oil product |
| CN108693282A (en) * | 2017-03-29 | 2018-10-23 | 赛默飞世尔科学股份有限公司 | The method of sampling for carrying out chromatography to headspace |
| CN115184511A (en) * | 2022-08-25 | 2022-10-14 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenols in white spirit |
| RU217236U1 (en) * | 2022-09-22 | 2023-03-23 | Федеральное государственное бюджетное учреждение науки Институт нефтегазовой геологии и геофизики им. А.А. Трофимука Сибирского отделения Российской академии наук | GAS CHROMATOGRAPHIC SAMPLE INTRODUCER |
| CN117686638A (en) * | 2024-02-04 | 2024-03-12 | 中国科学院合肥物质科学研究院 | Detection device and detection method for residual solvent in solid medicine |
-
2008
- 2008-11-19 CN CNA2008100797884A patent/CN101403732A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104950057A (en) * | 2015-04-03 | 2015-09-30 | 常州磐诺仪器有限公司 | Sample inlet of micro packed column |
| CN106706745A (en) * | 2017-02-17 | 2017-05-24 | 神华集团有限责任公司 | Measuring device and measuring method of water content in coal liquefaction oil product |
| CN108693282A (en) * | 2017-03-29 | 2018-10-23 | 赛默飞世尔科学股份有限公司 | The method of sampling for carrying out chromatography to headspace |
| CN115184511A (en) * | 2022-08-25 | 2022-10-14 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenols in white spirit |
| CN115184511B (en) * | 2022-08-25 | 2023-09-19 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenolic substances in white spirit |
| RU217236U1 (en) * | 2022-09-22 | 2023-03-23 | Федеральное государственное бюджетное учреждение науки Институт нефтегазовой геологии и геофизики им. А.А. Трофимука Сибирского отделения Российской академии наук | GAS CHROMATOGRAPHIC SAMPLE INTRODUCER |
| RU218361U1 (en) * | 2023-03-20 | 2023-05-23 | Федеральное государственное бюджетное учреждение науки Институт нефтегазовой геологии и геофизики им. А.А. Трофимука Сибирского отделения Российской академии наук | DEVICE FOR SELECTION AND SUBMISSION OF SAMPLES OF LABORLY SUBSTANCES FOR CHEMICAL ANALYSIS |
| RU218361U9 (en) * | 2023-03-20 | 2023-06-08 | Федеральное государственное бюджетное учреждение науки Институт нефтегазовой геологии и геофизики им. А.А. Трофимука Сибирского отделения Российской академии наук | DEVICE FOR SELECTION AND SUBMISSION OF SAMPLES OF LABORLY SUBSTANCES FOR CHEMICAL ANALYSIS |
| CN117686638A (en) * | 2024-02-04 | 2024-03-12 | 中国科学院合肥物质科学研究院 | Detection device and detection method for residual solvent in solid medicine |
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