On-line washing, neutralizing and regenerating device for ion chromatograph

Abstract

The utility model discloses an on-line washing, neutralizing and regenerating device for an ion chromatograph, which comprises an ultrapure water washing bottle, a sample bottle, a regenerated liquid bottle, a washing water pump, a sample liquid pump, a regenerated liquid pump, a washing water filter, a sample liquid filter, a regenerated liquid filter, a switching valve I and a cation exchange column, the switching valve I is provided with a flushing water sample inlet hole, a sample inlet hole, a regenerated liquid sample inlet hole and a sample outlet hole, and the sample outlet hole is connected with the cation exchange column; the ultrapure water flushing bottle is connected with a flushing water pump, the flushing water pump is connected with a flushing water filter, and the flushing water filter is connected to the flushing water sample injection hole; the sample bottle is connected with the sample liquid pump, the sample liquid pump is connected with the sample liquid filter, and the sample liquid filter is connected to the sample injection hole; the regenerated liquid bottle is connected with the regenerated liquid pump, the regenerated liquid pump is connected with the regenerated liquid filter, and the regenerated liquid filter is connected to the regenerated liquid sample injection hole. According to the utility model, integration and automation of flushing, neutralization and regeneration can be realized.

Description

TECHNICAL FIELD

[0001] The utility model relates to a kind of flushing neutralization and regeneration device, especially a kind of ion chromatograph online flushing neutralization regeneration device, analytical chemistry technical field. BACKGROUND

[0002] As a kind of high sensitivity, high selectivity analysis technique, ion chromatograph can simultaneously determine multiple anions, so it is often used for trace anion analysis. However, when determining anions in strong alkaline samples, the concentration of its hydroxyl group and other matrices is much higher than that in ion chromatography eluent. Direct measurement by ion chromatography will result in shortened component retention time, irregular baseline and incomplete separation, increased background conductivity, and inaccurate measurement of the content of each component to be measured. Even dilution measurement will also cause poor reproducibility of measurement results, higher detection limit than control limit, and other problems due to poor peak shape and early peak appearance, resulting in poor accuracy of measurement results. Therefore, the sample must be neutralized.

[0003] Manual sample processing methods, including chemical neutralization and resin neutralization, are rarely used due to time-consuming and poor accuracy. Automated online processing methods, which have the advantages of high automation, speed, and accuracy, are the preferred method for ion chromatography sample analysis and processing. They mainly include online neutralization devices based on peristaltic pumps or syringe pumps using neutralizers, dialysis, and solid-phase extraction columns. Instrument manufacturers have developed "Yinglan" automatic online processing devices based on dialysis principles and "Puru" automatic online processing devices based on solid-phase extraction columns. These automated online sample processing devices have solved the interference of sample matrix on ion chromatography anion analysis, and have significantly improved accuracy and precision. Among them, "Yinglan" and "Puru" processing devices developed by instrument manufacturers have complex structures and high operation and maintenance costs due to their consideration of multiple types of sample processing. Online neutralization devices based on peristaltic pumps or syringe pumps using neutralizers, dialysis, and solid-phase extraction columns have low cost, strong specificity for strong alkaline sample processing, and good effect, but the structure is slightly complex, and they do not consider regeneration after use. When the neutralization medium fails, it can only be replaced or regenerated offline, and the degree of automation still needs to be improved. UTILITY MODEL CONTENT

[0004] (I) Technical problem solved

[0005] To overcome the shortcomings of the prior art, the utility model provides an ion chromatograph online flushing neutralization regeneration device.

[0006] (II) Technical solution

[0007] To solve the above problems, this utility model provides the following technical solution: an online rinsing, neutralization and regeneration device for an ion chromatograph, characterized in that it includes an ultrapure water rinsing bottle, a sample bottle, a regeneration solution bottle, a rinsing water pump, a sample solution pump, a regeneration solution pump, a rinsing water filter, a sample solution filter, a regeneration solution filter, a switching valve I, and a cation exchange column. The switching valve I is provided with a rinsing water inlet, a sample inlet, a regeneration solution inlet, and an outlet. The outlet is connected to the cation exchange column. The switching valve I is used to connect the rinsing water pump, the sample solution pump, and the regeneration solution pump to the cation exchange column.

[0008] The ultrapure water rinsing bottle is connected to the rinsing water pump, the rinsing water pump is connected to the rinsing water filter, the rinsing water filter is connected to the rinsing water inlet, and the ultrapure water rinsing bottle is used for the online rinsing mode of the device.

[0009] The sample vial is connected to the sample liquid pump, the sample liquid pump is connected to the sample liquid filter, the sample liquid filter is connected to the sample inlet, and the sample vial is used for the online sample neutralization mode of the device.

[0010] The regenerated liquid bottle is connected to the regenerated liquid pump, the regenerated liquid pump is connected to the regenerated liquid filter, the regenerated liquid filter is connected to the regenerated liquid inlet, and the regenerated liquid bottle is used for the device in regeneration mode.

[0011] Preferably, the online flushing, neutralization and regeneration device for the ion chromatograph further includes a switching valve II and an ion chromatograph. The switching valve II is provided with a cation exchange column water inlet, a waste liquid outlet and a sample outlet. The cation exchange column is connected to the cation exchange column water inlet, and the sample outlet is connected to the ion chromatograph.

[0012] Preferably, the switching valve I and switching valve II are configured as six-channel switching valves.

[0013] Preferably, the rinsing water pump, sample liquid pump, and regeneration liquid pump are all configured as peristaltic pumps.

[0014] Preferably, the rinsing water filter, sample solution filter, and regeneration solution filter are all configured as pipeline filters.

[0015] Preferably, a wastewater tank is provided at the waste liquid outlet.

[0016] Preferably, the cation exchange columns are configured as three, and the three cation exchange columns are connected in series.

[0017] Preferably, all the connections are made through PE pipes.

[0018] (III) Beneficial Effects

[0019] Compared with the prior art, this utility model provides an online rinsing, neutralization and regeneration device for ion chromatographs, which has the following beneficial effects:

[0020] 1. This utility model overcomes the shortcomings of existing online neutralization treatment devices, such as complex structure, high operation and maintenance costs, and lack of online regeneration. It can process strongly alkaline samples online, neutralize the hydroxide matrix in the sample, remove interfering matrix, ensure the accuracy and precision of anion analysis by ion chromatography, and improve analytical sensitivity.

[0021] 2. To avoid sample contamination, this invention adds an online rinsing function, which performs rinsing before and after sample processing by switching valves, reducing the interference of system residues on the sample.

[0022] 3. After the cation neutralization column fails, it can be regenerated online through a switching valve. The structure is further simplified by using a six-channel switching valve, realizing the integration and automation of flushing, neutralization and regeneration. Attached image description:

[0023] Figure 1 This is a schematic diagram of the structure of this utility model;

[0024] In the diagram: 1. Ultrapure water rinse bottle, 2. Sample bottle, 3. Regeneration solution bottle, 4. Rinse water pump, 5. Sample solution pump, 6. Regeneration solution pump, 7. Rinse water filter, 8. Sample solution filter, 9. Regeneration solution filter, 10. Switching valve I, 11. Cation exchange column, 12. Switching valve II, 13. Ion chromatograph, 14. Wastewater tank, 15. Rinse water inlet, 16. Sample inlet, 17. Regeneration solution inlet, 18. Sample outlet, 19. Cation exchange column effluent inlet, 20. Waste liquid outlet, 21. Sample outlet. Detailed implementation method:

[0025] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0026] This utility model provides a new technical solution:

[0027] An online rinsing, neutralization, and regeneration device for an ion chromatograph includes an ultrapure water rinsing bottle 1, a sample bottle 2, a regeneration solution bottle 3, a rinsing water pump 4, a sample solution pump 5, a regeneration solution pump 6, a rinsing water filter 7, a sample solution filter 8, a regeneration solution filter 9, a switching valve I10, and a cation exchange column 11. The switching valve I10 is provided with a rinsing water inlet 15, a sample inlet 16, a regeneration solution inlet 17, and an outlet 18. The outlet 18 is connected to the cation exchange column 11. The switching valve I10 is used to connect the rinsing water pump 4, the sample solution pump 5, and the regeneration solution pump 6 to the cation exchange column 11.

[0028] The ultrapure water rinsing bottle 1 is connected to the rinsing water pump 4, the rinsing water pump 4 is connected to the rinsing water filter 7, the rinsing water filter 7 is connected to the rinsing water inlet 15, and the ultrapure water rinsing bottle 1 is used for the online rinsing mode of the device.

[0029] The sample vial 2 is connected to the sample liquid pump 5, the sample liquid pump 5 is connected to the sample liquid filter 8, the sample liquid filter 8 is connected to the sample inlet port 16, and the sample vial 2 is used for the online sample neutralization mode of the device.

[0030] The regenerated liquid bottle 3 is connected to the regenerated liquid pump 6, the regenerated liquid pump 6 is connected to the regenerated liquid filter 9, the regenerated liquid filter 9 is connected to the regenerated liquid inlet port 17, and the regenerated liquid bottle 3 is used for the device in regeneration mode.

[0031] In this embodiment, the online flushing, neutralization and regeneration device of the ion chromatograph 13 further includes a switching valve II12 and the ion chromatograph 13. The switching valve II12 is provided with a cation exchange column water inlet 19, a waste liquid outlet 20 and a sample outlet 21. The cation exchange column 11 is connected to the cation exchange column water inlet 19, and the sample outlet 21 is connected to the ion chromatograph 13.

[0032] In this embodiment, the switching valve I10 and switching valve II12 are configured as six-channel switching valves.

[0033] In this embodiment, the rinsing water pump 4, the sample liquid pump 5, and the regeneration liquid pump 6 are all configured as peristaltic pumps.

[0034] In this embodiment, the rinsing water filter 7, the sample liquid filter 8, and the regeneration liquid filter 9 are all configured as pipeline filters.

[0035] In this embodiment, a wastewater tank 14 is provided at the waste liquid outlet 20.

[0036] In this embodiment, three cation exchange columns 11 are provided, and the three cation exchange columns 11 are connected in series.

[0037] In this embodiment, all the connections are made through PE pipes.

[0038] Working principle: This utility model has three operating modes: Online flushing mode: The ultrapure water in the ultrapure water flushing bottle 1 is quantitatively drawn out by the flushing water pump 4 through the PE tube, filtered by the flushing water filter 7, and enters the flushing water inlet 15 of the switching valve I 10, which is connected to the outlet 18 of the switching valve I 10. After passing through the cation exchange column 11, it enters the outlet water inlet 19 of the cation exchange column of the switching valve II 12, which is connected to the waste liquid outlet 20 of the switching valve II 14. The flushing water is discharged into the waste water tank 14, realizing the flushing of the entire pipeline.

[0039] Online sample neutralization mode: such as Figure 1 As shown, the water sample in sample bottle 2 is quantitatively drawn out by sample liquid pump 5 through PE tube, filtered by sample liquid filter 8, and enters sample inlet port 16 of switching valve I 10, which is connected to outlet port 18 of switching valve I 10. After passing through cation exchange column 11, it enters outlet port 19 of cation exchange column of switching valve II 12, which is connected to waste liquid outlet port 20 of switching valve II 12. The water sample and the ultrapure water remaining in the pipeline are discharged into waste water tank 14. After running for 120 seconds (time adjustable), the outlet of switching valve II 12 automatically switches from waste liquid outlet port 20 to sample outlet port 21, so that the neutralized sample enters ion chromatograph 13 for detection and analysis.

[0040] Regeneration Mode: When the cation exchange resin fails, first thoroughly flush the entire system using the rinsing mode, then start the regeneration mode. The regeneration solution bottle (3) is metered out by the regeneration solution pump (6) through a PE tube, filtered by the regeneration solution filter (9), and enters the regeneration solution inlet (17) of switching valve I (10), which is connected to the outlet (18) of switching valve I. After passing through the cation exchange column (11), it enters the cation exchange column outlet (19) of switching valve II (12), which is connected to the waste liquid outlet (20) of switching valve II, discharging the regeneration waste liquid into the wastewater tank (14). After regeneration, the rinsing mode is restarted to flush the entire system until the rinsing water pH is neutral, indicating that regeneration is complete and the system is ready for use.

[0041] In practice, the regenerated cation exchange resin needs to be loaded into column 11 (cation exchange column). To ensure the sample is not contaminated, the online flushing mode must be activated before each analysis to thoroughly flush the system. Sample neutralization can only begin after flushing is complete. Since ultrapure water may remain in the cation exchange column and tubing during flushing, it can dilute the sample upon entry, leading to inaccurate ion chromatography results. Therefore, after sample entry, the system must be completely replaced with ultrapure water before entering the ion chromatograph (13). Before this, all ultrapure water should be discharged into the waste container (14) to ensure the accuracy of sample measurements. When the resin in column 11 fails, the flushing mode must be activated to thoroughly flush the system to prevent the residual sample in the cation exchange column from reacting with the regeneration solution. The regeneration mode can only be activated after the system is thoroughly flushed. After resin regeneration is complete, the flushing mode must also be activated to thoroughly flush out any remaining regeneration solution before resetting the resin.

[0042] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An online rinsing, neutralization, and regeneration device for an ion chromatograph, characterized in that, The system includes an ultrapure water rinsing bottle (1), a sample bottle (2), a regenerated liquid bottle (3), a rinsing water pump (4), a sample liquid pump (5), a regenerated liquid pump (6), a rinsing water filter (7), a sample liquid filter (8), a regenerated liquid filter (9), a switching valve I (10), and a cation exchange column (11). The switching valve I (10) is provided with a rinsing water inlet (15), a sample inlet (16), a regenerated liquid inlet (17), and an outlet (18). The outlet (18) is connected to the cation exchange column (11). The switching valve I (10) is used to connect the rinsing water pump (4), the sample liquid pump (5), and the regenerated liquid pump (6) to the cation exchange column (11). The ultrapure water rinsing bottle (1) is connected to the rinsing water pump (4), the rinsing water pump (4) is connected to the rinsing water filter (7), the rinsing water filter (7) is connected to the rinsing water inlet (15), and the ultrapure water rinsing bottle (1) is used for the online rinsing mode of the device. The sample bottle (2) is connected to the sample liquid pump (5), the sample liquid pump (5) is connected to the sample liquid filter (8), the sample liquid filter (8) is connected to the sample inlet (16), and the sample bottle (2) is used for the device to perform online sample neutralization mode; The regenerated liquid bottle (3) is connected to the regenerated liquid pump (6), the regenerated liquid pump (6) is connected to the regenerated liquid filter (9), the regenerated liquid filter (9) is connected to the regenerated liquid inlet (17), and the regenerated liquid bottle (3) is used for the device in regeneration mode.

2. The online flushing, neutralization, and regeneration device for an ion chromatograph according to claim 1, characterized in that, The online flushing, neutralization and regeneration device for the ion chromatograph (13) also includes a switching valve II (12) and the ion chromatograph (13). The switching valve II (12) is provided with a cation exchange column water inlet (19), a waste liquid outlet (20) and a sample outlet (21). The cation exchange column (11) is connected to the cation exchange column water inlet (19), and the sample outlet (21) is connected to the ion chromatograph (13).

3. The online flushing, neutralization, and regeneration device for an ion chromatograph according to claim 1, characterized in that, The switching valve I (10) and switching valve II (12) are configured as six-channel switching valves.

4. The online flushing, neutralization, and regeneration device for an ion chromatograph according to claim 1, characterized in that, The rinsing water pump (4), sample liquid pump (5) and regeneration liquid pump (6) are all peristaltic pumps.

5. The online flushing, neutralization, and regeneration device for an ion chromatograph according to claim 1, characterized in that, The rinsing water filter (7), sample liquid filter (8), and regeneration liquid filter (9) are all configured as pipeline filters.

6. The online flushing, neutralization, and regeneration device for an ion chromatograph according to claim 2, characterized in that, A wastewater tank (14) is installed at the waste liquid outlet (20).

7. The online flushing, neutralization, and regeneration device for an ion chromatograph according to claim 1, characterized in that, The cation exchange column (11) is configured as three, and the three cation exchange columns (11) are connected in series.

8. The online flushing, neutralization, and regeneration device for an ion chromatograph according to any one of claims 1-7, characterized in that, All connections are made through PE pipes.

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