CN115616130A - Chromatographic detection method and system - Google Patents
Chromatographic detection method and system Download PDFInfo
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- CN115616130A CN115616130A CN202211133669.9A CN202211133669A CN115616130A CN 115616130 A CN115616130 A CN 115616130A CN 202211133669 A CN202211133669 A CN 202211133669A CN 115616130 A CN115616130 A CN 115616130A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention provides a chromatographic detection method and a chromatographic detection system, wherein the chromatographic detection method comprises the following steps: the gas to be detected enters a first separation unit; a plurality of components in the gas to be detected are separated in the first separation unit and sequentially enter a first detector; the first detector outputs initial measurement parameters of the plurality of components, the initial measurement parameters comprise initial measurement concentration and retention time, and the initial measurement concentration of part of the components deviates from the range of the second detector; according to the initial measurement parameters, adjusting the concentration and the split ratio of the part of components in the gas to be measured which is discharged out of the first separation unit in real time to enable the concentration to be within the range of the second detector; and the components with adjusted and unadjusted concentrations sequentially enter the second detector, and the second detector outputs the concentrations of the multiple components in the gas to be detected. The invention has the advantages of detection accuracy and the like.
Description
Technical Field
The invention relates to a chromatographic technique, in particular to a chromatographic detection method and a chromatographic detection system.
Background
The online real-time monitoring of Volatile Organic Compounds (VOCs) is a key research content in recent years, and common online monitoring instruments include GC and GCMS, but because of different monitoring scenes (factory-bound unorganized or fixed pollution source emission and the like), concentration values of substances to be detected are greatly different, some substances even have dozens of times or hundreds of times of difference, each instrument has a fixed upper detection limit and a fixed lower detection limit, the instrument generally responds to overload when the upper detection limit is exceeded, so that the detection cannot be performed, and sometimes, even if the response is not overloaded, the response value does not fall within the concentration range where the instrument is calibrated, and the inaccuracy of the measurement result is also caused.
At present, the common solution is to change the sampling time of the pre-concentration device or adjust the split ratio according to the difference of the concentration in the monitoring field, but the above measures all result in inconsistency of the previous and subsequent methods, and moreover, the background concentration changes in real time, the method may need to be changed continuously, and the concentrations of different substances in the sample to be measured are also greatly different, for example, increasing the split ratio may result in too low a substance B response value and inaccurate measurement while ensuring that the substance a response is not overloaded.
Disclosure of Invention
In order to overcome the defects in the prior art scheme, the invention provides a chromatographic detection method.
The purpose of the invention is realized by the following technical scheme:
the chromatographic detection method comprises the following steps:
the gas to be detected enters a first separation unit;
a plurality of components in the gas to be detected are separated in the first separation unit and sequentially enter a first detector;
the first detector outputs initial measurement parameters of the plurality of components, the initial measurement parameters comprise initial measurement concentration and retention time, and the initial measurement concentration of part of the components deviates from the range of the second detector;
according to the initial measurement parameters, adjusting the concentration and the split ratio of the part of components in the gas to be measured which is discharged out of the first separation unit in real time to enable the concentration to be within the range of the second detector;
and the components with adjusted and unadjusted concentrations sequentially enter the second detector, and the second detector outputs the concentrations of the multiple components in the gas to be detected.
The invention also aims to provide a chromatographic detection system, and the aim is realized by the following technical scheme:
the chromatographic detection system comprises a first separation unit and a first detector which are sequentially connected in series; the chromatographic detection system further comprises:
a judging unit which judges whether the separated components need to be adjusted according to the initial measurement parameters output by the first detector, wherein the adjustment comprises the adjustment of concentration and split ratio;
the calculating unit is used for giving out adjustment targets of the concentration and the split ratio according to the judgment result of the judging unit and sending the adjustment targets to the concentration adjusting unit and the split ratio adjusting unit;
the output end of the first separation unit is sequentially connected with the second separation unit and the second detector;
the output end of the concentration adjusting unit is communicated with a pipeline, and the pipeline is communicated with the second separation unit and the first separation unit;
a split ratio adjusting unit connected to the pipe.
Compared with the prior art, the invention has the beneficial effects that:
1. the accuracy is good;
the concentration levels of different components of a sample to be detected can be fed back in advance, and the split ratio of each substance can be dynamically adjusted in real time, so that the optimal response value suitable for an instrument is obtained, and the detection accuracy is improved;
the concentration of each component in the sample to be measured is ensured to fall on the optimal position (such as the middle position of the standard curve concentration) of the linear concentration range of the standard curve, the accuracy of the measurement result is improved, and the standard curve does not need to be changed according to the difference of the concentration of the components on site;
2. the applicability is good;
the device greatly widens the detection upper limit of the instrument by adjusting the split ratio of each substance in real time, and theoretically, the response value of the instrument is never overloaded.
Drawings
The present disclosure 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 solution of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic diagram of the structure of a chromatographic detection system according to an embodiment of the 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 use 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:
the chromatographic detection method of embodiment 1 of the invention specifically comprises the following steps:
the gas to be detected enters a first separation unit;
a plurality of components in the gas to be detected are separated in the first separation unit and sequentially enter a first detector;
the first detector outputs initial measurement parameters of the plurality of components, the initial measurement parameters comprise initial measurement concentration and retention time, and the initial measurement concentration of part of the components deviates from the range of the second detector;
according to the initial measurement parameters, adjusting the concentration and the split ratio of the part of components in the gas to be measured which is discharged out of the first separation unit in real time to enable the concentration to be within the range of the second detector;
and the components with adjusted and unadjusted concentrations sequentially enter the second detector, and the second detector outputs the concentrations of the multiple components in the gas to be detected.
In order to adjust the concentration and the split ratio of the partial components so that the adjusted concentration is in the linear concentration range of the second detector, further, the adjustment mode is as follows:
when the part of the components reach the adjusting position, the dilution gas enters the adjusting position and is mixed with the part of the components, and the mixed gas flows to the downstream;
and adjusting the split ratio of the mixed gas, and enabling part of the mixed gas to sequentially pass through a second separation unit and the second detector.
In order to accurately determine whether adjustment is necessary, further, the determination method of whether the initial concentration deviates from the range is as follows:
if it is
k If the concentration is the threshold value, the initial measured concentration deviates from the measuring range; C1 is the initial measured concentration of the component output by the first detector, C2 is the upper limit of the linear concentration range of the component on the second detector;
if it is
The initially measured concentration is in the range of the measuring range。
In order to enable the components in the gas to be detected to be accurately detected by the second detector, further, the flow rate of the dilution gas
Split ratio of
V1 Is the flow rate of the first separation unit, V2 is the flow rate of the second separation unit.
In order to detect the concentration of the component in the gas to be detected quickly and accurately, further, the first detector has lower accuracy than the second detector, and the response time of the second detector is longer than that of the first detector.
In order to quickly detect the content of each component in the gas to be detected, further, the first detector is a nondestructive detector, and the concentration of a plurality of components discharged from the first detector is adjusted as required and enters the second detector in sequence.
In order to detect the components with lower content, the gas to be detected enters an enrichment unit, part of the gas to be detected which is discharged from the enrichment unit enters the first separation unit, and part of the gas to be detected enters an additional channel (the channel can be additionally provided with the enrichment unit);
after the first detector outputs the initial measurement parameters of multiple components in the gas to be measured, the gas to be measured in the additionally arranged channel sequentially enters the first separation unit and the second detector.
Fig. 1 schematically shows a structural diagram of a chromatography detection system according to an embodiment of the present invention, and as shown in fig. 1, the chromatography detection system includes:
the first separation unit and the first detector are sequentially connected in series;
a judging unit which judges whether the separated components need to be adjusted according to the initial measurement parameters output by the first detector, wherein the adjustment comprises the adjustment of concentration and split ratio;
the calculating unit is used for giving out adjustment targets of the concentration and the split ratio according to the judgment result of the judging unit and sending the adjustment targets to the concentration adjusting unit and the split ratio adjusting unit;
the output end of the first separation unit is sequentially connected with the second separation unit and the second detector;
the output end of the concentration adjusting unit is communicated with a pipeline, and the pipeline is communicated with the second separation unit and the first separation unit;
a split ratio adjusting unit connected to the pipe.
In order to reduce the structural complexity, further, the first detector is a nondestructive detector, the output end of the first separation unit is connected with the first detector and the second separation unit in sequence, or the output end of the first separation unit is connected with the first detector and the second separation unit respectively.
In order to detect the gas to be detected quickly and accurately, further, the first detector has lower precision than the second detector, and the response time of the second detector is longer than that of the first detector.
Example 2:
an example of an application of the chromatographic detection method and system according to embodiment 1 of the present invention.
In this application example, the chromatographic detection method specifically includes:
the gas to be detected enters an enrichment unit such as an enrichment tube, and the enriched gas to be detected enters a first separation unit such as an LTM column;
a plurality of components in the gas to be detected are separated in the first separation unit and sequentially enter a lossless first detector (PID detector);
the first detector outputs initial measurement parameters of the multiple components, the initial measurement parameters comprise initial measurement concentration and retention time, the initial measurement concentration of part of the components deviates from the range of the second detector (conventional detector), and the judgment mode of whether the initial measurement concentration deviates is as follows:
if it is
k If the concentration is the threshold value, if 0.5 is taken, the initial measured concentration deviates from the measuring range; C1 is the initial measured concentration of the component output by the first detector, C2 is the upper limit of the linear concentration range of the component on the second detector;
if it is
The initial measurement concentration is in the range of the measuring range;
according to the initial measurement parameters, adjusting the concentration and the split ratio of the part of components in the gas to be measured which is discharged out of the first separation unit in real time to enable the concentration to be within the range of the second detector; the adjustment mode is as follows:
when the part of the components reach the adjusting position, the dilution gas enters the adjusting position and is mixed with the part of the components, and the mixed gas flows to the downstream; flow rate of the dilution gas
V1 Is the flow rate of the first separation unit, V2 is the flow rate of the second separation unit;
adjusting the split ratio of the mixed gas
Part of the mixed gas sequentially passes through a second separation unit and the second detector;
the components with adjusted concentrations and components without adjustment sequentially enter a second separation unit (a conventional chromatographic column) and a second detector, namely, a plurality of components separated from the first separation unit sequentially pass through the first detector, the second separation unit and the second detector, and the second detector outputs the concentrations of the plurality of components in the gas to be detected;
the first detector is less accurate than the second detector, which has a response time greater than the first detector.
Fig. 1 schematically shows a structural diagram of a chromatography detection system (a system for implementing the method of the present embodiment) according to an embodiment of the present invention, and as shown in fig. 1, the chromatography detection system includes:
an enrichment unit, a first separation unit (such as an enrichment tube) and a lossless first detector (such as a PID detector) which are sequentially connected in series;
a judging unit, which judges whether the separated components need to be adjusted according to the initial measurement parameters output by the first detector (see the description of the method part for the manner of judgment), wherein the adjustment comprises the adjustment of concentration and split ratio;
a calculating unit, configured to give an adjustment target (a specific calculation manner is described in the method section) of the concentration and the split ratio according to a judgment result of the judging unit, and send the adjustment target to the concentration adjusting unit and the split ratio adjusting unit;
the output end of the first separation unit is connected with the first detector, the second separation unit and the second detector in sequence; the first detector is less accurate than a second detector, the second detector having a response time greater than the first detector;
the output end of the concentration adjusting unit is communicated with a pipeline, and the pipeline is communicated with the second separating unit and the first separating unit;
a split ratio adjusting unit connected to the pipe.
Example 3:
according to the application example of the chromatographic detection method and the chromatographic detection system in the embodiment 1 of the invention, the difference from the embodiment 2 is that:
part of the gas to be detected which is discharged from the enrichment unit enters the first separation unit, and part of the gas enters another channel (the channel can be additionally provided with the enrichment unit);
after the first detector outputs the initial measurement parameters of multiple components in the gas to be measured, the gas to be measured in the additionally arranged channel sequentially enters the first separation unit and then enters the first detector or the pipeline as required, and the pipeline is sequentially connected with the second separation unit and the second detector.
Claims (10)
1. The chromatographic detection method comprises the following steps:
the gas to be detected enters a first separation unit;
a plurality of components in the gas to be detected are separated in the first separation unit and sequentially enter a first detector;
the first detector outputs initial measurement parameters of the plurality of components, the initial measurement parameters comprise initial measurement concentration and retention time, and the initial measurement concentration of part of the components deviates from the range of the second detector;
according to the initial measurement parameters, adjusting the concentration and the split ratio of the part of components in the gas to be measured which is discharged out of the first separation unit in real time to enable the concentration to be within the range of the second detector;
and the components with adjusted and unadjusted concentrations sequentially enter the second detector, and the second detector outputs the concentrations of the multiple components in the gas to be detected.
2. The chromatography detection method according to claim 1, wherein the adjustment is performed in a manner that:
when the part of the components reach the adjusting position, the dilution gas enters the adjusting position and is mixed with the part of the components, and the mixed gas flows to the downstream;
and adjusting the split ratio of the mixed gas, and enabling part of the mixed gas to sequentially pass through a second separation unit and the second detector.
3. The chromatography detection method according to claim 2, wherein the determination of whether the initial concentration deviates from the range is performed by:
if it is
k If the concentration is the threshold value, the initial measured concentration deviates from the measuring range; C1 is the initial measured concentration of the component output by the first detector, C2 is the component atAn upper limit of a linear concentration range on the second detector;
if it is
The initial concentration is within the range.
4. The chromatography detection method according to claim 3, wherein a flow rate of the dilution gas
Split ratio
V1 Is the flow rate of the first separation unit, V2 is the flow rate of the second separation unit.
5. The chromatography detection method of claim 1, wherein the first detector is less accurate than a second detector having a response time greater than the first detector.
6. The chromatography detection method according to claim 1, wherein the first detector is a nondestructive detector, and the plurality of components discharged from the first detector are adjusted in concentration as necessary and sequentially entered into the second detector.
7. The chromatographic detection method according to claim 1, wherein the gas to be detected enters an enrichment unit, part of the gas to be detected which is discharged from the enrichment unit enters the first separation unit, and part of the gas to be detected enters an additional channel;
after the first detector outputs the initial measurement parameters of multiple components in the gas to be measured, the gas to be measured in the additionally arranged channel sequentially enters the first separation unit and the second detector.
8. The chromatographic detection system comprises a first separation unit and a first detector which are sequentially connected in series; characterized in that the chromatography detection system further comprises:
the judging unit judges whether the separated components need to be adjusted according to the initial measurement parameters output by the first detector, wherein the adjustment comprises adjustment of concentration and a split ratio;
the calculating unit is used for providing adjustment targets of the concentration and the split ratio according to the judgment result of the judging unit and sending the adjustment targets to the concentration adjusting unit and the split ratio adjusting unit;
the output end of the first separation unit is sequentially connected with the second separation unit and the second detector;
the output end of the concentration adjusting unit is communicated with a pipeline, and the pipeline is communicated with the second separation unit and the first separation unit;
a split ratio adjusting unit connected to the pipe.
9. The chromatography detection system of claim 8, wherein the first detector is a non-destructive detector and the output of the first separation unit is connected to the first detector and the second separation unit in series, or the output of the first separation unit is connected to the first detector and the second separation unit, respectively.
10. The chromatography detection system of claim 8, wherein the first detector is less accurate than a second detector having a response time greater than the first detector.
Applications Claiming Priority (2)
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| CN202210284022X | 2022-03-22 | ||
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117147671A (en) * | 2023-10-30 | 2023-12-01 | 杭州盈创环境科技有限公司 | Non-methane total hydrocarbon detection device and method based on dilution technology |
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- 2022-09-19 CN CN202211133669.9A patent/CN115616130A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117147671A (en) * | 2023-10-30 | 2023-12-01 | 杭州盈创环境科技有限公司 | Non-methane total hydrocarbon detection device and method based on dilution technology |
| CN117147671B (en) * | 2023-10-30 | 2024-02-06 | 杭州盈创环境科技有限公司 | Non-methane total hydrocarbon detection device and method based on dilution technology |
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