阅读说明：本技术 在线离子色谱自动清洗在线测量标定进样器 (On-line ion chromatography automatic cleaning on-line measurement calibration sample injector ) 是由 龚真 魏峰 邹爽 吴佳丽 于 2021-05-24 设计创作，主要内容包括：本发明涉及一种在线离子色谱自动清洗在线测量标定进样器,注射泵通过储液环与六通阀连接,注射泵上连通载流液,载流液为超纯水,所述第一号口与混液室连通,第一号口通过排气阀与混液室上口连通,排气阀另一端与空气连通,混液阀与混液室连通,混液阀还与第三号口连接,混液阀一端连接废液收集装置,第四号口连接进样端,第五号口与高浓度标液母液通过管路连接,第六号口与进液阀,进液阀的一端与废液收集装置连接,另一端连接精密过滤器,并经过精密过滤器后注射入离子色谱内。本发明不仅可以实现在线采样和在线标定,还可以实现自动清洗,远程控制高浓度标液母液通过自动稀释成标定浓度标液,实现自动标定功能。(The invention relates to an online measurement calibration sample injector for online automatic cleaning of ion chromatography, wherein an injection pump is connected with a six-way valve through a liquid storage ring, a carrier fluid is communicated on the injection pump, the carrier fluid is ultrapure water, a first port is communicated with a liquid mixing chamber, the first port is communicated with an upper port of the liquid mixing chamber through an exhaust valve, the other end of the exhaust valve is communicated with air, the liquid mixing valve is communicated with the liquid mixing chamber, the liquid mixing valve is further connected with a third port, one end of the liquid mixing valve is connected with a waste liquid collecting device, a fourth port is connected with a sample injection end, a fifth port is connected with high-concentration standard liquid mother liquid through a pipeline, a sixth port is connected with a liquid inlet valve, one end of the liquid inlet valve is connected with the waste liquid collecting device, the other end of the liquid inlet valve is connected with a precision filter, and the liquid is injected into the ion chromatography after passing through the precision filter. The invention can realize on-line sampling and on-line calibration, and can realize automatic cleaning, and the high-concentration standard solution mother liquor is remotely controlled to automatically dilute into the calibration concentration standard solution, thereby realizing the automatic calibration function.)

1. The utility model provides an online ion chromatogram self-cleaning online measurement calibration sample injector, its characterized in that, includes syringe pump, six-way valve, feed liquor valve, high concentration mark liquid mother liquor, mixes the liquid valve, mixes liquid chamber and discharge valve, the syringe pump passes through the liquid storage ring and is connected with six-way valve, intercommunication current-carrying liquid on the syringe pump, six-way valve includes first mouth, No. two mouth, No. three mouth, No. four mouth, No. five mouth and No. six mouth, first mouth passes through discharge valve and mixes liquid chamber upper shed intercommunication, the discharge valve other end and air intercommunication, mix liquid valve and mix liquid chamber intercommunication, mix the liquid valve and still be connected with No. three mouth, the one end that mixes the liquid valve and keep away from mixing liquid and connect waste liquid collection device, No. four mouth connection introduction port, No. five mouth and high concentration mark liquid mother liquor pass through the tube coupling, No. six mouth and feed liquor valve, one end of the liquid inlet valve is connected with the waste liquid collecting device, and the other end of the liquid inlet valve is connected with the precision filter and is injected into the ion chromatograph after passing through the precision filter.

2. The on-line ion chromatography automatic cleaning on-line measurement calibration sample injector as claimed in claim 1, wherein when low concentration on-line measurement is performed, the low concentration on-line measurement is performed by pumping the low concentration on-line sample through a syringe pump, the on-line sample enters the liquid storage ring through a fourth port of the six-way valve, the syringe pump reversely pushes the low concentration on-line sample out of the liquid storage ring through a sixth port of the six-way valve, the low concentration on-line sample is injected into the ion chromatography for analysis through a normally closed port of the liquid inlet valve, and redundant samples are discharged through a normally open port of the liquid inlet valve.

3. The on-line ion chromatography automatic cleaning on-line measurement calibration sample injector as claimed in claim 1, wherein when high concentration on-line measurement is performed, if the concentration of the measured water sample is too high, the automatic dilution process is started, the sample is extracted by the injection pump, the on-line sample enters the liquid storage ring through the fourth port of the six-way valve, the injection pump reversely pushes the water sample in the liquid storage ring out through the third port of the six-way valve, the water sample enters the liquid mixing chamber through the liquid mixing valve, the sample is extracted by the injection pump, the carrier fluid enters the liquid storage ring through the third port of the six-way valve, the injection pump reversely pushes the carrier fluid, wherein the carrier fluid is ultrapure water, the carrier fluid in the liquid storage ring is pushed out through the third port of the six-way valve, the carrier fluid enters the liquid mixing chamber through the liquid mixing valve, the carrier fluid is mixed and diluted with the on-line sample, the stroke of the injection pump is controlled, the sample feeding amounts of the on-line sample and the on-line sample are controlled, the stepless dilution within 1000 times is achieved, the sample which is diluted is extracted through the injection pump and enters the liquid storage ring through the third port of the six-way valve, the injection pump reversely pushes a water sample in the liquid storage ring out through the sixth port of the six-way valve, the water sample is injected into the ion chromatograph for analysis through the normally closed port of the liquid inlet valve, and redundant samples are discharged through the normally open port of the liquid inlet valve.

4. The on-line ion chromatography automatic cleaning on-line measurement calibration sample injector as claimed in claim 1, wherein when calibration is required, high concentration standard solution mother solution is extracted by a syringe pump, the standard solution mother solution enters the solution storage ring through a fifth port of a six-way valve, the syringe pump reversely pushes the standard solution mother solution in the solution storage ring out through a third port of the six-way valve, enters the solution mixing chamber through a solution mixing valve, is extracted by the syringe pump, the carrier solution enters the solution storage ring through a third port of the six-way valve, the syringe pump reversely pushes the carrier solution in the solution storage ring out through a third port of the six-way valve, enters the solution mixing chamber through the solution mixing valve, is mixed and diluted with the standard solution mother solution, controls the stroke of the syringe pump, controls the sample feeding amount of the standard solution mother solution and the carrier solution, achieves stepless concentration dilution within 1000 times, and further inequal dilution into any part of high, medium and low concentration calibration solutions, and (3) preparing standard solutions with different concentrations according to needs, pumping the diluted sample through an injection pump, enabling the diluted sample to enter a liquid storage ring through a third port of the six-way valve, reversely pushing the injection pump, pumping out a water sample in the liquid storage ring through a sixth port of the six-way valve, injecting the water sample into the ion chromatograph for analysis through a normally closed port of a liquid inlet valve, discharging redundant standard solution through a normally open port of the liquid inlet valve, and repeating the process for a fixed number of times to finish calibration.

5. The on-line ion chromatography automatic cleaning on-line measurement calibration sample injector as claimed in claim 1, wherein when the sample injection pipeline needs cleaning, the carrier fluid is pumped into the liquid storage ring through the injection pump, and the ion chromatography sample injection pipe is cleaned through the sixth port of the six-way valve.

6. The on-line ion chromatography automatic cleaning on-line measurement calibration sample injector as claimed in claim 1, wherein when the mixed liquid chamber is required to be cleaned, the carrier liquid is pumped by the injection pump to enter the liquid storage ring, the mixed liquid chamber is cleaned by the third port of the six-way valve, after the cleaning is completed, the air is pumped to enter the liquid storage ring, the air is pumped to the mixed liquid chamber by the first port of the six-way valve, the waste liquid in the mixed liquid chamber is discharged by the liquid mixing valve, and the waste liquid is directly discharged through the independent waste discharge port without back pumping to pollute the liquid storage ring and the sample injection pipeline.

Technical Field

The invention relates to the technical field of analytical instruments, in particular to an online measurement calibration sample injector with automatic cleaning function for online ion chromatography.

Background

The ion chromatographic analyzer belongs to a pure analysis unit, and can analyze a sample only by injecting an analysis water sample into the ion chromatographic analyzer through peripheral equipment or manpower. The ion chromatography sample injector is only a disc sample injector, namely a standard sample or an online water sample is manually put into a sample bottle of the sample injector, the water samples in the sample bottle are extracted one by one in a mechanical arm sampling mode, and then the water samples are injected into the ion chromatography for analysis.

The existing ion chromatography sample injectors belong to laboratory products and are not suitable for on-line measurement. Online sampling cannot be performed: because the sample can be injected only by manually putting the water sample into the sampling bottle, the sample injector can not realize on-line continuous sample injection. The online calibration cannot be carried out: the calibration needs 5-6 standard solutions with different concentrations, namely high, medium and low concentrations, the low-concentration standard solution cannot be stored for a long time, and manual replacement is needed in a short time, so that the sample injector cannot realize online calibration. The automatic cleaning cannot be carried out: this injector needs the manual cleaning sampling bottle, so can not realize self-cleaning.

Disclosure of Invention

The invention aims to provide an online ion chromatography automatic cleaning online measurement calibration sample injector to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme:

the utility model provides an online ion chromatogram self-cleaning measures demarcation injector on line, includes syringe pump, six-way valve, feed liquor valve, high concentration mark liquid mother liquor, mixes the liquid valve, mixes liquid chamber and discharge valve, the syringe pump passes through the liquid storage ring and is connected with six-way valve, intercommunication current-carrying liquid on the syringe pump, six-way valve includes first mouth, No. two mouth, No. three mouth, No. four mouth, No. five mouth and No. six mouth, first mouth and the intercommunication of mixing the liquid chamber, first mouth passes through discharge valve and the intercommunication of mixing the liquid chamber upper shed, the discharge valve other end and air intercommunication, mix the liquid valve and mix the liquid chamber intercommunication, mix the liquid valve and still be connected with No. three mouth, mix the liquid valve and keep away from the one end of mixing the liquid chamber and connect waste liquid collection device, No. four mouth connection introduction port, No. five mouth and high concentration mark liquid mother liquor pass through the tube coupling, No. six mouth and feed liquor valve, one end of the liquid inlet valve is connected with the waste liquid collecting device, and the other end of the liquid inlet valve is connected with the precision filter and is injected into the ion chromatograph after passing through the precision filter.

Preferably, when low concentration on-line measurement is carried out, the low concentration on-line measurement is carried out through the extraction of the injection pump, an on-line sample enters the liquid storage ring through the fourth port of the six-way valve, the injection pump reversely pushes a water sample in the liquid storage ring out through the sixth port of the six-way valve, the water sample is injected into the ion chromatography for analysis through the normally closed port of the liquid inlet valve, and redundant samples are discharged through the normally open port of the liquid inlet valve.

Preferably, when high-concentration online measurement is carried out, if the concentration of the measured water sample is too high, an automatic dilution process is started, the online sample is extracted through an injection pump, the online sample enters the liquid storage ring through a fourth port of the six-way valve, the injection pump reversely pushes the online sample, the water sample in the liquid storage ring is pumped out through a third port of the six-way valve, the online sample enters the liquid mixing chamber through the liquid mixing valve and is then extracted through the injection pump, the carrier fluid enters the liquid storage ring through a third port of the six-way valve, the injection pump reversely pushes the injection pump, the carrier fluid is ultrapure water, the carrier fluid in the liquid storage ring is pumped out through the third port of the six-way valve, the carrier fluid enters the liquid mixing chamber through the liquid mixing valve and is mixed and diluted with the online sample, the stroke of the injection pump is controlled, the sample feeding amounts of the online sample and the carrier fluid are controlled, stepless concentration dilution within 1000 times is achieved, the diluted sample is pumped through the injection pump and enters the liquid storage ring through the third port of the six-way valve, and the injection pump reversely pushes the water sample in the liquid storage ring out through a sixth port of the six-way valve, the water sample is injected into the ion chromatograph for analysis through a normally closed port of the liquid inlet valve, and redundant samples are discharged through a normally open port of the liquid inlet valve.

Preferably, when calibration is required, high-concentration standard solution mother liquor is pumped by a syringe pump, the standard solution mother liquor enters a solution storage ring through a fifth port of a six-way valve, the syringe pump reversely pushes the standard solution mother liquor in the solution storage ring out through a third port of the six-way valve, the standard solution mother liquor enters a solution mixing chamber through a solution mixing valve and is pumped by the syringe pump, carrier fluid enters the solution storage ring through the third port of the six-way valve, the syringe pump reversely pushes the carrier fluid in the solution storage ring out through the third port of the six-way valve, the carrier fluid enters the solution mixing chamber through the solution mixing valve and is mixed and diluted with the standard solution mother liquor, the stroke of the syringe pump is controlled, the sample feeding amounts of the standard solution mother liquor and the carrier fluid are controlled, stepless concentration dilution within 1000 times is achieved, then the standard solutions with different concentrations are diluted into any part of the standard solutions, the standard solutions with different concentrations are configured according to requirements, and diluted samples are pumped by the syringe pump and enter the solution storage ring through the third port of the six-way valve, and (3) reversely pushing the injection pump, pumping out the water sample in the liquid storage ring through a sixth port of the six-way valve, injecting the water sample into the ion chromatograph for analysis through a normally closed port of the liquid inlet valve, discharging redundant calibration liquid through a normally open port of the liquid inlet valve, and repeating the process for fixed times to finish calibration.

Preferably, when the sample injection pipeline needs to be cleaned, the carrier fluid is pumped into the liquid storage ring through the injection pump, and the ion chromatography sample injection pipe is cleaned through the sixth port of the six-way valve.

Preferably, when needs are washd the muddy liquid room, draw the carrier fluid through the syringe pump and get into the liquid storage ring, wash the muddy liquid room through No. three mouth of six-way valve, wash the completion back, the extraction air gets into the liquid storage ring, squeezes into the muddy liquid room with the air through No. one mouth of six-way valve, mixes indoor waste liquid of liquid and through muddy liquid valve discharge waste liquid, the waste liquid is through independent waste discharge port, directly the wasting discharge, no longer the back suction pollutes liquid storage ring and introduction pipeline.

Compared with the prior art, the invention has the beneficial effects that:

1. the high-concentration mother solution of the standard solution can be stored for a long time.

2. The remote control high-concentration standard solution mother liquor is automatically diluted into a calibration concentration standard solution, so that the automatic calibration function is realized. The manual calibration is liberated, generally 6 hours are needed for one-time manual calibration, and one-time calibration is needed every month.

3. The mixed liquid chamber independently discharges waste liquid, and the sample introduction pipeline is not polluted by pumping back.

4. The device can be independently formed into a device, and can also be integrated in large-scale equipment to continuously supply liquid for ion chromatography.

5. The ion chromatography detector of the laboratory instrument can be applied to the on-line measurement occasion through the device.

Drawings

FIG. 1 is a schematic structural diagram of an online measurement calibration sample injector for online ion chromatography automatic cleaning according to the present invention.

In the figure: 1. an injection pump; 2. a six-way valve; 3. a liquid inlet valve; 4. high concentration mother liquor of the standard solution; 5. a liquid mixing valve; 6. a liquid mixing chamber; 7. an exhaust valve; 8. a liquid storage ring; 9. a first port; 10. a second port; 11. a third port; 12. a fourth port; 13. a fifth port; 14. a sixth port; 15. a precision filter.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1, in an embodiment of the present invention, an online measurement calibration sample injector for online ion chromatography automatic cleaning includes an injection pump 1, a six-way valve 2, a liquid inlet valve 3, a high-concentration standard solution mother solution 4, a liquid mixing valve 5, a liquid mixing chamber 6, and an exhaust valve 7, the injection pump 1 is connected to the six-way valve 2 through a liquid storage ring 8, the injection pump 1 is communicated with a carrier solution, the six-way valve 2 includes a first port 9, a second port 10, a third port 11, a fourth port 12, a fifth port 13, and a sixth port 14, the first port 9 is communicated with the liquid mixing chamber 6, the first port 9 is communicated with the upper port of the liquid mixing chamber 6 through the exhaust valve 7, the other end of the exhaust valve 7 is communicated with air, the liquid mixing valve 5 is communicated with the liquid mixing chamber 6, the liquid mixing valve 5 is further connected to the third port 11, one end of the liquid mixing valve 5 far from the liquid mixing chamber 6 is connected to a waste liquid collecting device, fourth No. 12 connection introduction end, fifth No. 13 passes through the tube coupling with high concentration standard solution mother liquor 4, No. sixth No. 14 and feed liquor valve 3, the one end and the waste liquid collection device of feed liquor valve 3 are connected, and precision filter 15 is connected to the other end to in injecting ion chromatogram after precision filter 15. The online measurement calibration sample injector adopting the online ion chromatography automatic cleaning of the invention not only can realize online sampling and online calibration, but also can realize automatic cleaning, remotely control the high-concentration standard solution mother liquor to be automatically diluted into the calibration concentration standard solution, and realize the automatic calibration function. The device can be used for independently forming equipment, can be integrated in large-scale equipment, continuously supplies liquid for ion chromatography, and can be used for applying the ion chromatography detector of a laboratory instrument to an on-line measurement occasion.

When low concentration on-line measurement is carried out, the on-line sample enters the liquid storage ring 8 through the fourth port 12 of the six-way valve 2, the injection pump 1 reversely pushes the water sample in the liquid storage ring 8 out through the sixth port 14 of the six-way valve 2, the water sample is injected into the ion chromatograph for analysis through the normally closed port of the liquid inlet valve 3, and redundant samples are discharged through the normally open port of the liquid inlet valve 3.

When high concentration on-line measurement is carried out, if the concentration of a measured water sample is too high, an automatic dilution process is started, the on-line sample is extracted through the injection pump 1, the on-line sample enters the liquid storage ring 8 through the fourth port 12 of the six-way valve 2, the injection pump 1 reversely pushes, the water sample in the liquid storage ring 8 is pumped out through the third port 11 of the six-way valve 2, the water sample enters the liquid mixing chamber 6 through the liquid mixing valve 5 and is then extracted through the injection pump 1, the carrier fluid enters the liquid storage ring 8 through the third port 11 of the six-way valve 2, the injection pump 1 reversely pushes the carrier fluid in the liquid storage ring 8 out through the third port 11 of the six-way valve 2, wherein the carrier fluid is ultrapure water, the ultrapure water enters the liquid mixing chamber 6 through the liquid mixing valve 5 and is mixed and diluted with the on-line sample, the stroke of the injection pump 1 is controlled, the sample feeding amounts of the on-line sample and the carrier fluid are controlled, the stepless concentration dilution within 1000 times is achieved, the diluted sample is pumped through the third port 11 of the six-way valve 2 and enters the liquid storage ring 8 through the injection pump 1, the injection pump 1 reversely pushes, water samples in the liquid storage ring 8 are pumped out through the sixth port 14 of the six-way valve 2, the water samples are injected into the ion chromatograph for analysis through the normally closed port of the liquid inlet valve, and redundant samples are discharged through the normally open port of the liquid inlet valve.

When calibration is needed, high-concentration standard solution mother liquor 4 is extracted through an injection pump 1, the standard solution mother liquor enters a solution storage ring 8 through a fifth port 13 of a six-way valve 2, the injection pump 1 reversely pushes, the standard solution mother liquor in the solution storage ring 8 is pumped out through a third port 11 of the six-way valve 2, enters a solution mixing chamber 6 through a solution mixing valve 5, is extracted through the injection pump 1, carrier fluid enters the solution storage ring 8 through the third port 11 of the six-way valve 2, the injection pump 1 reversely pushes the carrier fluid in the solution storage ring 8 out through the third port 11 of the six-way valve 2, enters the solution mixing chamber 6 through the solution mixing valve 5, is mixed and diluted with the standard solution mother liquor, the stroke of the injection pump 1 is controlled, the sample feeding amounts of the standard solution mother liquor and the carrier fluid are controlled to achieve stepless concentration dilution within 1000 times, and then the standard solutions with different concentrations are diluted into any one of high, medium and low concentration standard solutions according to be configured, the diluted sample is extracted by the injection pump 1 and enters the liquid storage ring 8 through the third port 11 of the six-way valve 2, the injection pump 1 reversely pushes the water sample in the liquid storage ring 8 out through the sixth port 14 of the six-way valve 2, the water sample is injected into the ion chromatograph for analysis through the normally closed port of the liquid inlet valve, redundant calibration liquid is discharged through the normally open port of the liquid inlet valve, and the calibration is completed by repeating the times specified in the process.

When the sampling pipeline needs to be cleaned, the injection pump 1 is used for pumping the carrier fluid into the liquid storage ring 8, and the ion chromatography sampling pipe is cleaned through the sixth port 14 of the six-way valve 2.

When needs are washd mixing liquid chamber 6, get into liquid storage ring 8 through 1 extraction carrier fluid of syringe pump, wash mixing liquid chamber 6 through No. three port 11 of six-way valve 2, wash the completion back, the extraction air gets into liquid storage ring 8, squeeze into mixing liquid chamber 6 with the air through No. one first port 9 of six-way valve 2, the waste liquid in mixing liquid chamber 6 is through mixing liquid valve 5 discharge waste liquid, the waste liquid is through independent waste discharge port, direct wasting discharge, no longer the pumpback pollutes liquid storage ring and introduction pipeline.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.