CN114324718A - Organic sulfur detection method based on chromatographic technique - Google Patents
Organic sulfur detection method based on chromatographic technique Download PDFInfo
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- CN114324718A CN114324718A CN202111557678.6A CN202111557678A CN114324718A CN 114324718 A CN114324718 A CN 114324718A CN 202111557678 A CN202111557678 A CN 202111557678A CN 114324718 A CN114324718 A CN 114324718A
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- 238000001514 detection method Methods 0.000 title claims abstract description 18
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 17
- 125000001741 organic sulfur group Chemical group 0.000 title claims abstract description 14
- 239000012159 carrier gas Substances 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention provides an organic sulfur detection method based on a chromatographic technique, which comprises the following steps: (A1) switching the multi-way valve, wherein the object to be detected enters an enrichment unit, and two ends of the enrichment unit are respectively communicated with the ports of the multi-way valve; (A2) the multi-way valve is switched, and carrier gas passes through the pressure control unit, then sequentially enters the enrichment unit and the pre-column at a first pressure, is discharged from a first port of the multi-way valve, and enters a pipeline between the first port and the switching valve; the two ends of the enrichment unit and the pre-column are respectively communicated with the ports of the multi-way valve; (A3) and (3) switching the multi-way valve, wherein after passing through the pressure control unit, carrier gas passes through the first port at a second pressure, and carries the gas in the pipeline to sequentially enter the switching valve, the chromatographic column and the detector, the flow between the chromatographic column and the detector is the same as the flow in the pipeline in the step (A2), and the second pressure is greater than the first pressure. The invention has the advantages of accurate detection result and the like.
Description
Technical Field
The invention relates to a chromatographic technique, in particular to an organic sulfur detection method based on the chromatographic technique.
Background
The conventional organic sulfur detection device has the problems of peak type and non-ideal response.
In order to solve the above technical problems, the existing solution is to increase a pre-analysis timing sequence, so that the temperature of the enrichment tube reaches the analysis temperature before the sample injection stage, and there is no gradual temperature rise process in the sample injection timing sequence. This solution has the disadvantage of being prone to tailing and bifurcation.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides an organic sulfur detection method based on a chromatographic technique.
The purpose of the invention is realized by the following technical scheme:
the organic sulfur detection method based on the chromatographic technique comprises the following steps:
(A1) switching the multi-way valve, wherein the object to be detected enters an enrichment unit, and two ends of the enrichment unit are respectively communicated with the ports of the multi-way valve;
(A2) the multi-way valve is switched, and carrier gas passes through the pressure control unit, then sequentially enters the enrichment unit and the pre-column at a first pressure, is discharged from a first port of the multi-way valve, and enters a pipeline between the first port and the switching valve;
the two ends of the enrichment unit and the pre-column are respectively communicated with the ports of the multi-way valve;
(A3) and (3) switching the multi-way valve, wherein after passing through the pressure control unit, carrier gas passes through the first port at a second pressure, and carries the gas in the pipeline to sequentially enter the switching valve, the chromatographic column and the detector, the flow between the chromatographic column and the detector is the same as the flow in the pipeline in the step (A2), and the second pressure is greater than the first pressure.
Compared with the prior art, the invention has the beneficial effects that:
the pressure is changed in time, so that the enrichment unit desorbs when the pressure is lower, the target compound is quickly analyzed, and the risks of peak tailing and bifurcation are avoided; when the pressure is large, the separation is carried out during detection, and in the pressure adjustment, the flow rate after the pre-column and the flow rate after the chromatographic column are kept unchanged, so that the detection accuracy is ensured.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
fig. 1 is a schematic flow chart of an organic sulfur detection method based on a chromatographic technique according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of explaining the technical solution of the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 is a schematic flow chart of an organic sulfur detection method based on chromatography, according to an embodiment of the present invention, and as shown in fig. 1, the organic sulfur detection method based on chromatography includes the following steps:
(A1) switching the multi-way valve, wherein the object to be detected enters an enrichment unit, and two ends of the enrichment unit are respectively communicated with the ports of the multi-way valve;
(A2) the multi-way valve is switched, and carrier gas passes through the pressure control unit, then sequentially enters the enrichment unit and the pre-column at a first pressure, is discharged from a first port of the multi-way valve, and enters a pipeline between the first port and the switching valve;
the two ends of the enrichment unit and the pre-column are respectively communicated with the ports of the multi-way valve;
(A3) and (3) switching the multi-way valve, wherein after passing through the pressure control unit, carrier gas passes through the first port at a second pressure, and carries the gas in the pipeline to sequentially enter the switching valve, the chromatographic column and the detector, the flow between the chromatographic column and the detector is the same as the flow in the pipeline in the step (A2), and the second pressure is greater than the first pressure.
In order to clean the pre-column simultaneously with sampling, further, in step (a1), the carrier gas enters the pre-column and then is discharged.
To clean the enrichment cell while feeding the sample, further, in step (a3), a carrier gas is introduced into the enrichment cell and then discharged.
Example 2:
an example of the application of the method for detecting organosulfur based on chromatographic technique according to example 1 of the present invention.
In the present application example, as shown in fig. 1, the method for detecting organic sulfur based on the chromatography comprises the following steps:
(A1) switching a ten-way valve, wherein the object to be detected enters an enrichment pipe, and two ends of the enrichment pipe are respectively communicated with the ports of the ten-way valve;
the carrier gas enters the pre-column and then is discharged, so that the pre-column is cleaned;
(A2) the ten-way valve is switched, and carrier gas sequentially enters the enrichment pipe and the pre-column at a first pressure, such as 5kPa, after passing through a pressure control unit (EPC), is discharged from a first port of the ten-way valve and enters a pipeline between the first port and the switching valve;
two ends of the enrichment pipe and the pre-column are respectively communicated with the port of the ten-way valve;
(A3) the ten-way valve is switched, after passing through the pressure control unit, carrier gas passes through the first port at a second pressure of 95kPa and carries the gas in the pipeline to sequentially enter the switching valve, the chromatographic column and the detector, and the flow between the chromatographic column and the detector is the same as the flow in the pipeline in the step (A2), and is 1.5 ml/min;
simultaneously, carrier gas enters the enrichment tube and is then discharged, thereby cleaning the enrichment tube.
Claims (5)
1. The organic sulfur detection method based on the chromatographic technique comprises the following steps:
(A1) switching the multi-way valve, wherein the object to be detected enters an enrichment unit, and two ends of the enrichment unit are respectively communicated with the ports of the multi-way valve;
(A2) the multi-way valve is switched, and carrier gas passes through the pressure control unit, then sequentially enters the enrichment unit and the pre-column at a first pressure, is discharged from a first port of the multi-way valve, and enters a pipeline between the first port and the switching valve;
the two ends of the enrichment unit and the pre-column are respectively communicated with the ports of the multi-way valve;
(A3) and (3) switching the multi-way valve, wherein after passing through the pressure control unit, carrier gas passes through the first port at a second pressure, and carries the gas in the pipeline to sequentially enter the switching valve, the chromatographic column and the detector, the flow between the chromatographic column and the detector is the same as the flow in the pipeline in the step (A2), and the second pressure is greater than the first pressure.
2. The organic sulfur detection method based on the chromatography technique as claimed in claim 1, wherein in the step (a1), a carrier gas enters the pre-column and then is discharged.
3. The organic sulfur detection method based on the chromatography technology as claimed in claim 1, wherein in the step (A3), a carrier gas enters the enrichment unit and then is discharged.
4. The chromatography-based organosulfur detection method of claim 1, wherein the flow control unit is EPC.
5. The chromatography-based organosulfur detection method of claim 1, wherein the multi-way valve is a ten-way valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111557678.6A CN114324718A (en) | 2021-12-20 | 2021-12-20 | Organic sulfur detection method based on chromatographic technique |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111557678.6A CN114324718A (en) | 2021-12-20 | 2021-12-20 | Organic sulfur detection method based on chromatographic technique |
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| CN114324718A true CN114324718A (en) | 2022-04-12 |
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| CN202111557678.6A Pending CN114324718A (en) | 2021-12-20 | 2021-12-20 | Organic sulfur detection method based on chromatographic technique |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002250722A (en) * | 2001-02-27 | 2002-09-06 | Taiyo Toyo Sanso Co Ltd | Method and equipment for analyzing extremely low concentration hydrogen sulfide |
| CN1584589A (en) * | 2004-05-27 | 2005-02-23 | 上海烟草（集团）公司 | Automatic multi-dimensional gas-phase chromatographic system and use with non-valve pressure switching |
| CN1632564A (en) * | 2004-12-27 | 2005-06-29 | 天津大学 | Apparatus and process for improving detection sensitivity by modulating outlet pressure or flow of chromatographic column |
| JP2006064646A (en) * | 2004-08-30 | 2006-03-09 | Shimadzu Corp | Gas chromatograph device and gas chromatograph analysis method |
| CN103760283A (en) * | 2013-12-31 | 2014-04-30 | 聚光科技(杭州)股份有限公司 | Adsorption and thermal desorption feeding device and method |
| CN111257473A (en) * | 2020-03-25 | 2020-06-09 | 常州磐诺仪器有限公司 | Non-methane total hydrocarbon on-line detection device |
| CN213903428U (en) * | 2020-09-20 | 2021-08-06 | 杭州谱育科技发展有限公司 | Non-methane total hydrocarbon analysis device |
-
2021
- 2021-12-20 CN CN202111557678.6A patent/CN114324718A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002250722A (en) * | 2001-02-27 | 2002-09-06 | Taiyo Toyo Sanso Co Ltd | Method and equipment for analyzing extremely low concentration hydrogen sulfide |
| CN1584589A (en) * | 2004-05-27 | 2005-02-23 | 上海烟草（集团）公司 | Automatic multi-dimensional gas-phase chromatographic system and use with non-valve pressure switching |
| JP2006064646A (en) * | 2004-08-30 | 2006-03-09 | Shimadzu Corp | Gas chromatograph device and gas chromatograph analysis method |
| CN1632564A (en) * | 2004-12-27 | 2005-06-29 | 天津大学 | Apparatus and process for improving detection sensitivity by modulating outlet pressure or flow of chromatographic column |
| CN103760283A (en) * | 2013-12-31 | 2014-04-30 | 聚光科技(杭州)股份有限公司 | Adsorption and thermal desorption feeding device and method |
| CN111257473A (en) * | 2020-03-25 | 2020-06-09 | 常州磐诺仪器有限公司 | Non-methane total hydrocarbon on-line detection device |
| CN213903428U (en) * | 2020-09-20 | 2021-08-06 | 杭州谱育科技发展有限公司 | Non-methane total hydrocarbon analysis device |
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