CN207457152U - A kind of On-chip derivatization device detected for polar compound gas-chromatography or gas chromatography-mass spectrometry - Google Patents
A kind of On-chip derivatization device detected for polar compound gas-chromatography or gas chromatography-mass spectrometry Download PDFInfo
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- CN207457152U CN207457152U CN201720341988.7U CN201720341988U CN207457152U CN 207457152 U CN207457152 U CN 207457152U CN 201720341988 U CN201720341988 U CN 201720341988U CN 207457152 U CN207457152 U CN 207457152U
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Abstract
The utility model is related to a kind of On-chip derivatization devices detected for polar compound gas-chromatography or gas chromatography-mass spectrometry, it is made of derivative reagent bottle, three-way interface, three-way valve, double trocars and connecting line through connection.The utility model is simple in structure, easy to operate, and derivative reagent utilization rate is high, and derivative is efficient.
Description
Technical field
The utility model is related to the online pretreatment technology apparatus fields of gas-chromatography, are that one kind is used for polarity specifically
Compound gas phase chromatography or the On-chip derivatization device of gas chromatography-mass spectrometry detection.
Background technology
Polar organic compound steam forces down, and chromatographic isolation effect difference is, it is necessary to its derivatization is transformed into nonpolar easy
Volatile substance, while improve chromatographic column separating effect.Common derivatization method includes silanization, butyl ester and methylation method etc..
However this conventional analysis complicated process steps, process is cumbersome, takes time and effort, and consumes a large amount of solvents.Since derivative reagent is special
It is that silylating reagent easily reacts with water in air, must be used at once behind Kaifeng, and how unstable derivative products are, it is derivative to complete
Upper machine at once is also needed afterwards, and the time limit tested after the preservation and reaction of derivative reagent is more demanding, tests difficulty and consumables all
It increases, process is cumbersome, can not accomplish timely conventional detection.
German Orasche et al. attempts that derivative reagent is applied directly on sample filter membrane upper machine manually, while aids in deriving
Polar organic matter in the mode On-chip derivatization analysis particulate matter of reagent gas purging.[J.Orasche,J.Schnelle-Kreis,
G.Abbaszade, and R.Zimmermann Technical Note:In-situ derivatization thermal
desorption GC-TOFMS for direct analysis of particle-bound non-polar and polar
Organic species Atmos.Chem.Phys., 2011,11,8977-8993] a kind of patent " air-flow of On-chip derivatization
Formula the dynamic liquid phase micro-extraction method " (patent No.：CN103245544A) also attempt to introduce during liquid-phase micro-extraction and spread out online
Raw, to simplify sample pretreatment process, but method still needs to solvent after manual adding liquid derivative reagent and manually transfer extraction
Sample introduction.
Utility model content
The purpose of this utility model be solve the above problems and provide it is a kind of simple in structure, without adding derivative examination manually
Agent, easy to operate, derivative reagent utilization rate is high, the On-chip derivatization device of derivative efficient gas chromatography-mass spectrometry.
The utility model proposes a kind of detect for polar compound gas-chromatography or gas chromatography-mass spectrometry
On-chip derivatization device is made of, structure derivative reagent bottle, three-way connection, three-way valve, double trocars and connecting line through connection
As shown in Fig. 1.Wherein, derivative reagent bottle (4) is used to store derivative reagent (6)；Quartz capillary (7) penetrates double trocars (5)
It is inserted to pin bottom；Double trocar (5) tops are connected with the second three-way interface (2)；Quartz capillary (7) passes through the second three-way connection
(2) and the first three-way connection (1) accesses gas chromatographic sample introduction mouth (8)；First three-way connection (1) and the second three-way connection (2) warp
Three-way valve (3) connects；The flow direction of three-way valve control helium (11).
Compared with prior art, the utility model achieves following technique effect：
1st, this utility model can realize polar compound On-chip derivatization and for gas chromatography-mass spectrometry, structure letter
It is single, it is easy to operate, experimenter's labor intensity can be reduced, reduces sample loss.
2nd, the sample that this utility model is applicable in can be gaseous state, liquid or solid sample, expanded gas-chromatography and located online
Manage the application range of sample.
3rd, derivative reagent and derivatization reaction process whole process are sealed in atmosphere of inert gases by the device, have prevented water in air
Divide the loss to derivative reagent, improve derivative reagent service efficiency, and extend the derivative reagent holding time.
Description of the drawings
Fig. 1 is the utility model planar structure schematic diagram.
Fig. 2 is the chromatogram obtained using the utility model ten kinds of organic acids of analysis.
Figure label：The double sets of the first three-way interfaces of 1-, the second three-way interfaces of 2-, 3- three-way valves, 4- derivative reagents bottle, 5-
Pin, 6- derivative reagents, 7- quartz capillaries, 8- gas chromatographic sample introductions mouth, 9- chromatographic columns, 10- detectors, 11- helium.
Specific embodiment
The embodiment of the utility model is further illustrated below in conjunction with the accompanying drawings.
With reference to Fig. 1, it is using the analytical procedure of the utility model：
1) 4 inside of derivative reagent bottle is packed into derivative reagent 6, double trocars 5 are maintained at 6 top of derivative reagent.
2) for gaseous state or liquid sample, injection port is directly injected a sample into；For solid sample, sample is packed into sample introduction
Mouth internal lining pipe, bushing pipe underfill mineral wool seal post-purge, injection port are risen to 300 degrees Celsius by room temperature.
3) open three-way valve 3 to turn right, carrier gas is introduced into derivative reagent bottle 4, top gaseous state derivative reagent in bottle is led to
The quartz capillary in double trocars is crossed by the second three-way interface 2, the first three-way interface 1 is introduced, and eventually enters into gas-chromatography
Injection port 8 carries out derivatization reaction.
4) after the completion of derivatization reaction, swivel tee valve 3 is introduced directly into gas chromatographic sample introduction mouth 8 to the left, by carrier gas.
5) gas-chromatography temperature programming is opened, the derivative products of injection port will be directly entered chromatographic column with carrier gas, carry out
Gas chromatography combined with mass spectrometry is analyzed.
Exemplified by ten kinds of organic acids, illustrate the using effect of the present invention on quartz filter to analyze below.
Ten kinds of organic acids are respectively：N-hexadecanoic, n-octadecanoic acid, malonic acid, glutaric acid, adipic acid, suberic acid, nonyl two
Acid, phthalic acid, suitable pinic acid and pinonic acid.
Gas chromatography-mass spectrometry analysis condition：Chromatographic column：The derivative stream of HP-5MS columns (300mmx0.25 μm of x0.25mm)
Amount：1mL/min, derivative time：10min, derivative temperature：100 DEG C -310 DEG C (12min), GC column temperatures：35 DEG C (1min) are with 15
DEG C/min rises to 280 DEG C.
Analytic process：Ten kinds of organic acids with acetone are diluted, obtain the test solution of 200mg/L, 1 μ L is taken to be injected into blank
Quartz filter is put into injection port bushing pipe, enables the utility model device and carries out On-chip derivatization analysis.
Fig. 2 is the chromatogram after ten kinds of organic acids derive, by NIST database retrievals and literature search, ten kinds of organic acids
It is fully completed derivative.Simultaneously investigate device reaction reappearance and method it is linear, the results are shown in Table 1, sample peak area standard
Deviation is less than 7.8%, and linear coefficient shows the device favorable reproducibility between 0.976 to 0.993, and precision is high, reliable results,
Routine analysis needs can be met.
The reappearance of Information in Mass Spectra and method, the range of linearity and related coefficient after 1. each compound of table derives
。
Claims (1)
1. a kind of On-chip derivatization device detected for polar compound gas-chromatography or gas chromatography-mass spectrometry, feature
It is：It is made of derivative reagent bottle, three-way connection, three-way valve, double trocars and connecting line through connection, wherein derivative reagent
Bottle (4) is used to store derivative reagent (6)；Quartz capillary (7) penetrates double trocars (5) and is inserted to pin bottom；Double trocar (5) tops with
Second three-way connection (2) connects；Quartz capillary (7) accesses gas phase through the second three-way connection (2) and the first three-way connection (1)
Chromatography column feed materials mouth (8)；First three-way connection (1) and the second three-way connection (2) are connected through three-way valve (3), three-way valve control
The flow direction of helium (11).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720341988.7U CN207457152U (en) | 2017-04-01 | 2017-04-01 | A kind of On-chip derivatization device detected for polar compound gas-chromatography or gas chromatography-mass spectrometry |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720341988.7U CN207457152U (en) | 2017-04-01 | 2017-04-01 | A kind of On-chip derivatization device detected for polar compound gas-chromatography or gas chromatography-mass spectrometry |
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| CN207457152U true CN207457152U (en) | 2018-06-05 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187797A (en) * | 2018-09-29 | 2019-01-11 | 延边大学 | A kind of method that the gaseous state derivatization reagent of flowing is used for On-chip derivatization |
| CN114570183A (en) * | 2022-03-01 | 2022-06-03 | 西安热工研究院有限公司 | Derivatization reaction device of urea hydrolysis sediment |
| CN114577933A (en) * | 2022-03-01 | 2022-06-03 | 西安热工研究院有限公司 | Derivatization experiment system and method for urea hydrolysis sediment |
-
2017
- 2017-04-01 CN CN201720341988.7U patent/CN207457152U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187797A (en) * | 2018-09-29 | 2019-01-11 | 延边大学 | A kind of method that the gaseous state derivatization reagent of flowing is used for On-chip derivatization |
| CN114570183A (en) * | 2022-03-01 | 2022-06-03 | 西安热工研究院有限公司 | Derivatization reaction device of urea hydrolysis sediment |
| CN114577933A (en) * | 2022-03-01 | 2022-06-03 | 西安热工研究院有限公司 | Derivatization experiment system and method for urea hydrolysis sediment |
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