CN103344778A - Microsample injection apparatus and sample injection method - Google Patents
Microsample injection apparatus and sample injection method Download PDFInfo
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- CN103344778A CN103344778A CN2013102371904A CN201310237190A CN103344778A CN 103344778 A CN103344778 A CN 103344778A CN 2013102371904 A CN2013102371904 A CN 2013102371904A CN 201310237190 A CN201310237190 A CN 201310237190A CN 103344778 A CN103344778 A CN 103344778A
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Abstract
The invention discloses a microsample injection apparatus and a sample injection method to mainly overcome the problems of great metering errors and cross contamination caused by retention of residual liquid on a wall in the process of microsample injection for a chemical analysis instrument. The apparatus comprises a sample injection pump, a metering tube, an upper liquid-deficiency detector, an upper liquid level detector, a lower liquid level detector, a lower liquid-deficiency detector, a multichannel changeover valve, a residual liquid barrel, a reagent A, a reagent B, a cleaning fluid, a two-position three-way cleaning valve, a colorimetric ware and a controller. The sample injection method is as follows: the upper liquid level detector and the lower liquid level detector are mounted on the elongated metering tube, and the volume of sample injection is a difference between the volumes of the upper liquid level detector and the lower liquid level detector in the metering tube, i.e., the volume of a reagent discharged during falling from the upper liquid level detector to the lower liquid level detector. With the apparatus and the sample injection method provided by the invention, influence of retention of residual liquid on a wall can be eliminated, and accurate microsample injection of reagents can be realized; and the apparatus and the method are applicable to microsample injection of reagents for chemical analysis instruments.
Description
Technical field
The present invention relates to a kind of micro-sampling device and sample injection method, be applicable to chemical analysis instrument reagent micro-sampling.
Background technology
Along with development of technology, analytical instrument more and more is widely used in every field, " miniaturization ", " intellectuality ", " modularization " become development trend, and the performance requirement of analytical instrument also progressively improves, as detection speed, measuring accuracy, reagent consumption etc.For the analytical instrument of micro-sampling, will consider following influence factor in the sample introduction process: the influence of sample introduction error, wall built-up raffinate, reagent lack liquid and detect.The sample introduction error generally adopts relative error, that is: relative error=| measured value-true value |/true value x100%, wherein, measured value is actual sample size, and true value is theoretical sample size, under the constant situation of systematic error, relative error and the theoretical sample size relation of being inversely proportional to, sample size is more big, and relative error is more little, and vice versa.Sampling volume generally adopts measures that liquid level measures in the fixed inner diameter gauge line, identical sampling volume, the internal diameter of gauge line is more little, the height of liquid level is just more high, the gauge line length that needs is just more long, and error in dipping is just more little, still, because the increase of contact area, the raffinate wall cling phenomenon is also more obvious during discharge opeing.Traditional input mode reduces error in dipping and the influence of raffinate wall built-up by increasing reagent dosage and increasing the pipeline wash number, wherein, when pipeline cleans, cleaning fluid and sample introduction reagent are entered and are discharged gauge line by equidirectional, this mode not only reagent consumption is big, secondary pollution is serious, sample injection time is long, the more important thing is for density lighter, be insoluble in the wall built-up raffinate of cleaning fluid, can not be along with cleaning fluid is discharged fully, after finishing, cleaning still is attached on the metering tube wall, disturb reagent metering next time, even meeting and down a kind of reagent chemical reaction takes place in advance, the testing result of impact analysis instrument; Traditional approach adopts single detector that the gauge line liquid level is detected to judge scarce liquid status, the shortcoming of this mode is when reagent does not reach sampling volume, there is air in the reagent lower end in the gauge line, single detector still can detect liquid level signal, and be judged as mistakenly and lack liquid, proceed to measure, cause and detect failure.
Summary of the invention
The present invention proposes a kind of micro-sampling device and sample injection method, can realize accurately sample introduction of sample introduction trace, reduce the influence of raffinate wall built-up effectively, detect accurately and reliably lacking liquid simultaneously, method is reasonable, simple in structure, cost is low, be applicable to chemical analysis instrument reagent micro-sampling.
For achieving the above object, adopt following technical scheme:
Device of the present invention comprises: sampling pump 1, gauge line 2, upward lack liquid detecting device 3, go up liquid level detector 4, liquid level detector 5, scarce liquid detecting device 6, hyperchannel transfer valve 7, waste liquid barrel 8, reagent B9, reagent A 10, cleaning fluid 11, two-bit triplet cleaning valve 12, cuvette 13, controller 14 down down; Wherein, the public passage of hyperchannel transfer valve 7 is connected with gauge line 2 lower ends, and other passages of hyperchannel transfer valve 7 are connected with waste liquid barrel 8, reagent B9, reagent A 10, cuvette 13 respectively; Gauge line 2 upper ends are connected with sampling pump 1 one ends, and sampling pump 1 other end is connected with two-bit triplet cleaning valve 12 common ports; Often the opening of two-bit triplet cleaning valve 12, normal-closed end connects air respectively and cleaning fluid 11; Go up to lack liquid detecting device 3, go up liquid level detector 4, down liquid level detector 5, down scarce liquid detecting device 6 from top to bottom order be installed on the gauge line 2, and can the shift position.
Further, sampling pump (1) is peristaltic pump.
Further, gauge line 2 is the elongated tubular of little internal diameter.
Further, controller 14 control sampling pumps 1, hyperchannel transfer valve 7, two-bit triplet cleaning valve 12 and to last scarce liquid detecting device 3, go up liquid level detector 4, liquid level detector 5, scarce liquid detecting device 6 input down down.
Further, a public passage and a plurality of obstructed passage are mutually arranged on the hyperchannel transfer valve 7, passage switches can realize that each passage is connected with public passage respectively.
Further, the sample injection method of described micro-sampling device is:
1., the sampling flow process, hyperchannel transfer valve 7 is switched to reagent A 10 passages, two-bit triplet cleaning valve 12 is switched to normal open walk, connect air, start sampling pump 1 and extract reagent A 10 in gauge line 2;
2., lack the liquid testing process, go up in the stipulated time and lack liquid detecting device 3 or down scarce liquid detecting device 6 each does not detect reagent and has signal, then be judged as scarce liquid, report to the police, carry out 8., otherwise be normally, carry out 3.;
3., push away the sample flow process, sampling pump 1 counter-rotating, with the reagent of gauge line 2 by shifting liquid level detector 4 positions onto under last scarce liquid detecting device 3 positions;
4., the sample introduction flow process, hyperchannel transfer valve 7 is switched to cuvette 13 interface channels, sampling pump 1 counter-rotating is shifted down the reagent A 10 of gauge line 2 onto liquid level detector 5 positions by last liquid level detector 4 positions, reagent A 10 enters cuvette 13;
5., continue sample introduction reagent A 10 as needs, carry out 1.; Otherwise, carry out 6.;
6., cleaning process, hyperchannel transfer valve 7 is switched to waste liquid barrel 8 interface channels, two-bit triplet cleaning valve 12 is switched to cleaning fluid 11 passages, sampling pump 1 counter-rotating is injected cleaning fluid 11 in the gauge lines 2, and is pushed waste liquid barrel 8;
7., the emptying flow process, hyperchannel transfer valve 7 is switched to waste liquid barrel 8 interface channels, two-bit triplet cleaning valve 12 is switched to air duct, sampling pump 1 counter-rotating pushes waste liquid barrel 8 with the reagent in the gauge line 2;
8., finish.
The advantage of described micro-sampling device is: (1) gauge line is elongated tubular, and the filling length of reagent in gauge line is long, reduces liquid level detector and detects error to metering result's influence, and micro-measurement is accurate, relative error is little; (2) go up scarce liquid detecting device and down scarce liquid detector combination and judge that reagent lacks liquid, scarce liquid detects accurately and reliably; (3) sampling volume is the volume differences between last liquid level detector and the following liquid level detector, that is: reagent is fallen down the volume that the liquid level detector gauge line is discharged from last liquid level detector, because the wall built-up raffinate is positioned at the upper strata of reagent, the wall built-up raffinate is not discharged from, and effectively reduces the interference that the reagent wall built-up causes; (4) reagent injects from the gauge line lower end, and cleaning fluid injects from the gauge line upper end, and reverse detergent line is cleaned thoroughly,
Avoid cross pollution between reagent.Adopt this device can realize accurately sample introduction of trace, eliminate the influence of raffinate wall built-up, accurately judge reagent lack liquid, simple in structure, cost is low, be applicable to chemical analysis instrument reagent micro-sampling.
Description of drawings
Fig. 1 is apparatus of the present invention structural representation
Fig. 2 is embodiment 1 sampling schematic flow sheet
Fig. 3 is that embodiment 1 lacks liquid testing process synoptic diagram
Fig. 4 pushes away the sample schematic flow sheet for embodiment 1
Fig. 5 is embodiment 1 sample introduction schematic flow sheet
Fig. 6 is embodiment 1 cleaning process synoptic diagram
Fig. 7 is embodiment 1 emptying schematic flow sheet
Embodiment
As shown in Figure 1, described micro-sampling device comprises: sampling pump 1, gauge line 2, upward lack liquid detecting device 3, go up liquid level detector 4, liquid level detector 5, scarce liquid detecting device 6, hyperchannel transfer valve 7, waste liquid barrel 8, reagent B9, reagent A 10, cleaning fluid 11, two-bit triplet cleaning valve 12, cuvette 13, controller 14 down down; Connected mode is: the public passage of hyperchannel transfer valve 7 is connected with gauge line 2 lower ends, and other passages of hyperchannel transfer valve 7 are connected with waste liquid barrel 8, reagent B9, reagent A 10, cuvette 13 respectively; Gauge line 2 upper ends are connected with sampling pump 1 one ends, and sampling pump 1 other end is connected with two-bit triplet cleaning valve 12 common ports, and often the opening of two-bit triplet cleaning valve 12, normal-closed end connects air respectively and cleaning fluid 11; Install scarce liquid detecting device 3 on the gauge line 2 from top to bottom in proper order, go up liquid level detector 4, following liquid level detector 5, following scarce liquid detecting device 6; Controller 14 connects the electric interfaces of described pump, valve, detecting device.
Present embodiment is described micro-sampling device sample introduction flow process:
1., sampling flow process (as shown in Figure 2)
Hyperchannel transfer valve 7 is switched to reagent A 10 passages, two-bit triplet cleaning valve 12 is switched to normal open walk, connect air, start sampling pump 1 and extract reagent A 10 in gauge line 2.
2., lack liquid testing process (as shown in Figure 3)
Interior scarce liquid detecting device 3 of stipulated time and following liquid level detector 5 all detect reagent and have signal, and be normal, carry out 3., otherwise, being judged as scarce liquid, 8. warning is carried out
3., push away sample flow process (as shown in Figure 4)
4., sample introduction flow process (as shown in Figure 5)
Hyperchannel transfer valve 7 is switched to cuvette 13 interface channels, and sampling pump 1 counter-rotating is shifted down the reagent A of gauge line 2 onto liquid level detector 5 positions by last liquid level detector 4 positions, and reagent A enters cuvette 13.
5., continue the sample introduction reagent A as needs, carry out 1.; Otherwise, carry out 6..
6., cleaning process (as shown in Figure 6)
Hyperchannel transfer valve 7 is switched to waste liquid barrel 8 interface channels, two-bit triplet cleaning valve 12 is switched to cleaning fluid 11 passages, sampling pump 1 counter-rotating is injected cleaning fluid 11 in the gauge line 2, and is pushed waste liquid barrel 8.
7., emptying flow process (as shown in Figure 7)
Hyperchannel transfer valve 7 is switched to waste liquid barrel 8 interface channels, two-bit triplet cleaning valve 12 is switched to air duct, sampling pump 1 counter-rotating pushes waste liquid barrel 8 with the reagent in the gauge line 2.
8., finish.
Claims (6)
1. micro-sampling device, comprise: sampling pump (1), gauge line (2), go up and lack liquid detecting device (3), last liquid level detector (4), following liquid level detector (5), following scarce liquid detecting device (6), hyperchannel transfer valve (7), waste liquid barrel (8), reagent B (9), reagent A (10), cleaning fluid (11), two-bit triplet cleaning valve (12), cuvette (13), controller (14), wherein, the public passage of hyperchannel transfer valve (7) is connected with gauge line (2) lower end, other passages of hyperchannel transfer valve (7) respectively and waste liquid barrel (8), reagent B (9), reagent A (10), cuvette (13) connects, gauge line (2) upper end is connected with sampling pump (1) one end, sampling pump (1) other end is connected with two-bit triplet cleaning valve (12) common port, often opening of two-bit triplet cleaning valve (12), normal-closed end connects air and cleaning fluid (11) respectively, go up and lack liquid detecting device (3), last liquid level detector (4), following liquid level detector (5), scarce liquid detecting device (6) is installed on the gauge line (2) down, it is characterized in that: upward lack liquid detecting device (3), last liquid level detector (4), following liquid level detector (5), scarce liquid detecting device (6) is installed on the gauge line (2) from top to bottom in proper order down, and can the shift position.
2. micro-sampling device according to claim 1, it is characterized in that: sampling pump (1) is peristaltic pump.
3. micro-sampling device according to claim 1, it is characterized in that: gauge line (2) is little internal diameter elongated tubular.
4. micro-sampling device according to claim 1 is characterized in that: controller (14) control sampling pump (1), hyperchannel transfer valve (7), two-bit triplet cleaning valve (12) and to last scarce liquid detecting device (3), go up liquid level detector (4), liquid level detector (5), scarce liquid detecting device (6) input down down.
5. micro-sampling device according to claim 1 is characterized in that: a public passage and a plurality of obstructed passage are mutually arranged on the hyperchannel transfer valve (7), and passage switches can realize that each passage is connected with public passage respectively.
6. utilize the sample injection method of the described micro-sampling device of claim 1:
1., the sampling flow process, hyperchannel transfer valve (7) is switched to reagent A (10) passage, two-bit triplet cleaning valve (12) is switched to normal open walk, connect air, start sampling pump (1) and extract reagent A (10) in gauge line (2);
2., lack the liquid testing process, go up in the stipulated time lack liquid detecting device (3) or down scarce liquid detecting device (6) each do not detect reagent and have signal, then be judged as scarce liquid, report to the police, carry out 8., otherwise be normally, carry out 3.;
3., push away the sample flow process, sampling pump (1) counter-rotating, with the reagent of gauge line (2) by shifting liquid level detector (4) position under last scarce liquid detecting device (3) position onto;
4., sample introduction flow process, hyperchannel transfer valve (7) is switched to cuvette (13) interface channel, sampling pump (1) counter-rotating is shifted down the reagent A (10) of gauge line (2) onto liquid level detector (5) position by last liquid level detector (4) position, and reagent A (10) enters cuvette (13);
5., continue sample introduction reagent A (10) as needs, carry out 1.; Otherwise, carry out 6.;
6., cleaning process, hyperchannel transfer valve (7) is switched to waste liquid barrel (8) interface channel, two-bit triplet cleaning valve (12) is switched to cleaning fluid (11) passage, sampling pump (1) counter-rotating, cleaning fluid (11) is injected in the gauge line (2), and push waste liquid barrel (8);
7., the emptying flow process, hyperchannel transfer valve (7) is switched to waste liquid barrel (8) interface channel, two-bit triplet cleaning valve (12) is switched to air duct, sampling pump (1) counter-rotating pushes waste liquid barrel (8) with the reagent in the gauge line (2);
8., finish.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104897669A (en) * | 2015-06-25 | 2015-09-09 | 无锡点创科技有限公司 | Three-way valve metering device of online water quality monitor |
| CN105004874A (en) * | 2015-07-03 | 2015-10-28 | 深圳世绘林科技有限公司 | Autoinjection and dosage measuring method |
| CN108072767A (en) * | 2016-11-18 | 2018-05-25 | 上海安杰环保科技股份有限公司 | A kind of autosampler for possessing sample dilution function |
| CN108889354A (en) * | 2018-07-06 | 2018-11-27 | 上海兰博贸易有限公司 | A kind of high-precision liquor-transferring system |
| CN110007102A (en) * | 2019-04-02 | 2019-07-12 | 深圳市智创环保科技有限公司 | A kind of liquid relief accurate quantification sampling device |
| CN110665553A (en) * | 2019-09-25 | 2020-01-10 | 广东顺德工业设计研究院(广东顺德创新设计研究院) | Micro-droplet detection sample introduction system and use method |
| CN114870737A (en) * | 2022-05-18 | 2022-08-09 | 深圳市中成环境科技有限公司 | Method for extracting medicament by metering any volume |
| CN116256476A (en) * | 2023-05-15 | 2023-06-13 | 江苏一脉科技有限公司 | Hydrogen chloride concentration on-line analysis detector |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104897669A (en) * | 2015-06-25 | 2015-09-09 | 无锡点创科技有限公司 | Three-way valve metering device of online water quality monitor |
| CN105004874A (en) * | 2015-07-03 | 2015-10-28 | 深圳世绘林科技有限公司 | Autoinjection and dosage measuring method |
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| CN110007102A (en) * | 2019-04-02 | 2019-07-12 | 深圳市智创环保科技有限公司 | A kind of liquid relief accurate quantification sampling device |
| CN110665553A (en) * | 2019-09-25 | 2020-01-10 | 广东顺德工业设计研究院(广东顺德创新设计研究院) | Micro-droplet detection sample introduction system and use method |
| CN110665553B (en) * | 2019-09-25 | 2021-11-09 | 广东顺德工业设计研究院(广东顺德创新设计研究院) | Micro-droplet detection sample introduction system and use method |
| CN114870737A (en) * | 2022-05-18 | 2022-08-09 | 深圳市中成环境科技有限公司 | Method for extracting medicament by metering any volume |
| CN116256476A (en) * | 2023-05-15 | 2023-06-13 | 江苏一脉科技有限公司 | Hydrogen chloride concentration on-line analysis detector |
| CN116256476B (en) * | 2023-05-15 | 2023-10-20 | 江苏一脉科技有限公司 | Hydrogen chloride concentration on-line analysis detector |
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Application publication date: 20131009 |