Sample pretreatment system for anhydrous acid detection

Abstract

The utility model relates to a sample pretreatment system for anhydrous acid detection. The sample pretreatment system for anhydrous acid detection comprises a mounting box as well as a V1 multi-way valve, a V5 multi-way valve, a first quantitative loop and an air inlet pipe which are positioned in the mounting box, and further comprises a V3 multi-way valve, a V4 multi-way valve, a V6 multi-way valve, a V7 multi-way valve, a peristaltic pump, a second quantitative loop, a third quantitative loop, a waste liquid injection pump, a carrier liquid injection pump and a diluent injection pump which are positioned on the outer side of the mounting box, a plurality of valve ports of the V1 multi-way valve are communicated with the anhydrous acid liquid inlet pipe, and the gas inlet pipe is communicated with the valve port of the V1 multi-way valve and one valve port of the V5 multi-way valve through the three-way valve; and one valve port of the V5 multi-way valve is communicated with a waste liquid pipe. According to the utility model, through the split design of the mounting box and the fixed box, the space layout is optimized, the multi-way valve through which the anhydrous acid does not flow cannot be damaged when the anhydrous acid with strong corrosivity leaks, only the multi-way valve in the mounting box needs to be replaced, the maintenance cost is low, and the use safety is high.

Description

Technical Field

[0001] This utility model belongs to the field of anhydrous acid detection technology, specifically relating to a sample pretreatment system for anhydrous acid detection. Background Technology

[0002] The manufacturing processes in industries such as chips and LCD panels are increasingly demanding precision and high performance, requiring high-purity hydrofluoric acid. Currently, the production process for high-purity hydrofluoric acid involves chemically pretreating anhydrous acid, then distilling it in a distillation column. The resulting anhydrous acid is cooled and absorbed by ultrapure water in an absorption tower. Further purification is achieved by controlling spray density and gas-liquid ratio. This is followed by ultrafiltration to a depth of less than 0.2 μm, and finally, the product—high-purity hydrofluoric acid—is packaged in a closed, clean environment. The entire preparation process requires multiple samplings of the anhydrous acid to better adjust process parameters. The anhydrous acid sampling equipment must maintain a high level of cleanliness, and the sampling waste gas must be treated for safety and ease of operation.

[0003] Hydrofluoric acid is an aqueous solution of hydrogen fluoride gas. It is a clear, colorless, fuming, corrosive liquid with a pungent, irritating odor. It is extremely corrosive, severely damaging metals, glass, and silicon-containing materials. Inhalation of its vapor or skin contact can cause burns that are difficult to heal. Currently, most high-purity anhydrous acid sampling equipment uses industrial-grade hydrofluoric acid sampling methods, often employing open sampling, which lacks sufficient safety and easily leads to accidents.

[0004] Chinese invention patent application CN118518425A discloses an anhydrous acid sampling and injection system and method. This system uses a syringe pump for precise control, achieving accurate dilution of anhydrous acid within the pipeline and solving the dilution problem for corrosive and volatile samples. However, all valves in this system are housed in a single enclosure. If a leak occurs in the multi-way valve through which hydrofluoric acid flows, it will contaminate other multi-way valves within the enclosure that do not flow with hydrofluoric acid, causing damage to other valves, increasing maintenance costs and time, and causing significant inconvenience to users. Utility Model Content

[0005] To address the aforementioned technical problems, this invention provides a sample pretreatment system for anhydrous acid detection.

[0006] The technical solution of the sample pretreatment system for anhydrous acid detection according to this utility model is as follows:

[0007] A sample pretreatment system for anhydrous acid detection includes an installation box and a V1 multi-way valve, a V5 multi-way valve, a first metering loop, and an air inlet pipe located inside the installation box. It also includes a V3 multi-way valve, a V4 multi-way valve, a V6 multi-way valve, a V7 multi-way valve, a peristaltic pump, a second metering loop, a third metering loop, a waste liquid injection pump, a carrier liquid injection pump, and a diluent injection pump located outside the installation box.

[0008] Several valve ports of the V1 multi-way valve are connected to the anhydrous acid inlet pipe, and the air inlet pipe is connected to the valve port of the V1 multi-way valve and one valve port of the V5 multi-way valve through a three-way valve.

[0009] One valve port of the V5 multi-way valve is connected to the waste liquid pipe, and the other valve port is connected to one valve port of the V6 multi-way valve. The two valve ports are respectively connected to the two ends of the first metering ring.

[0010] One valve port of the V6 multi-port valve is connected to the waste liquid pipe, one valve port is connected to the liquid carrier pipe, and the two valve ports are respectively connected to the two ends of the second metering ring.

[0011] Several valve ports of the V3 multi-port valve are connected to the standard solution pipeline, and one valve port is connected to the cleaning solution pipeline.

[0012] One valve port of the V4 multi-way valve is connected to the valve port of the V3 multi-way valve, one valve port is connected to the liquid carrying tube, and the two valve ports are respectively connected to the two ends of the third metering ring.

[0013] The three valve ports of the V7 multi-way valve are respectively connected to one valve port of the V6 multi-way valve, one valve port of the V4 multi-way valve, and the inlet of the peristaltic pump through pipelines.

[0014] The waste liquid injection pump is connected to the waste liquid pipe and one valve port of the V4 multi-way valve via a three-way valve; the carrier liquid injection pump is connected to the carrier liquid pipe and one valve port of the V5 multi-way valve via a three-way valve.

[0015] The diluent injection pump is connected to the diluent pipe and one port of the V5 multi-way valve via a three-way valve.

[0016] Furthermore, the installation box includes a box body, which is a rectangular structure with an open front end. A door is hinged to the open end of the box body, and an observation window is provided on the door.

[0017] Furthermore, the sample pretreatment system also includes a fixed box, in which the V3 multi-way valve, V4 multi-way valve, V6 multi-way valve, V7 multi-way valve, peristaltic pump, second metering ring, third metering ring, waste liquid injection pump, carrier liquid injection pump, and diluent injection pump are installed.

[0018] Furthermore, the V1 multi-port valve is a nine-channel valve, with each of the nine valve ports connected to one of the nine anhydrous acid inlet pipes.

[0019] Furthermore, the V3 multi-way valve is a twelve-channel valve, the V4 multi-way valve is a two-position six-way valve, the V5 multi-way valve is a two-position seven-way valve, the V6 multi-way valve is a two-position six-way valve, and the V7 multi-way valve is a two-position three-way valve.

[0020] Furthermore, an air pump is installed on the air intake pipe.

[0021] This invention provides a sample pretreatment system for anhydrous acid detection, which has the following advantages compared to existing technologies:

[0022] This utility model's sample pretreatment system for anhydrous acid detection achieves automatic sampling, dilution, injection, and cleaning of standard solutions and anhydrous acids through the coordinated switching of multi-port valves and the linkage of syringe pumps and peristaltic pumps, reducing manual intervention and operational errors. By configuring peristaltic pumps and multiple syringe pumps (for carrier liquid, diluent, and waste liquid), precise control of liquid delivery volume is ensured, improving the consistency of dilution ratios and injection, and enhancing the accuracy of test results. The separate design of the mounting box and the fixing box optimizes space layout; leakage of highly corrosive anhydrous acid will not damage the multi-port valves through which the anhydrous acid does not flow, requiring only replacement of the multi-port valves within the mounting box, resulting in low maintenance costs and high operational safety. The independent waste liquid pipeline and waste liquid syringe pump design, combined with the automatic cleaning function in the standard solution / sample flow, effectively avoids cross-contamination and ensures system cleanliness. Attached Figure Description

[0023] Figure 1 This is a flowchart of the sample pretreatment system for anhydrous acid detection according to this utility model;

[0024] Figure 2 This is a flowchart of the standard solution sampling process in the anhydrous acid detection sample pretreatment system of this utility model;

[0025] Figure 3 This is a flowchart of the standard solution injection process in the anhydrous acid detection sample pretreatment system of this utility model;

[0026] Figure 4 This is a flowchart of the anhydrous acid sampling process in the sample pretreatment system for anhydrous acid detection of this utility model;

[0027] Figure 5 This is a flowchart of the anhydrous acid dilution process in the sample pretreatment system for anhydrous acid detection according to this utility model;

[0028] Figure 6 This is a flowchart of the anhydrous acid injection process in the sample pretreatment system for anhydrous acid detection according to this utility model; Detailed Implementation

[0029] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments:

[0030] Specific embodiments of the sample pretreatment system for anhydrous acid detection of this utility model are as follows: Figure 1 As shown, the system includes an installation box and a mounting box. The installation box is a rectangular box with an open front end. The door is hinged and has a transparent acrylic observation window embedded in the center for easy monitoring of the internal operating status. The installation box contains a V1 multi-way valve, a V5 multi-way valve, and a first metering ring. The mounting box contains a V3 multi-way valve, a V4 multi-way valve, a V6 multi-way valve, a V7 multi-way valve, a peristaltic pump, a second metering ring, a third metering ring, a waste liquid injection pump, a carrier liquid injection pump, and a diluent injection pump. The nine ports of the V1 multi-way valve are connected to nine anhydrous acid inlet pipes. The V3 multi-way valve is a twelve-channel valve, the V4 multi-way valve is a two-position six-way valve, the V5 multi-way valve is a two-position seven-way valve, the V6 multi-way valve is a two-position six-way valve, and the V7 multi-way valve is a two-position three-way valve.

[0031] The V1 multi-port valve has nine ports connected to nine anhydrous acid inlet lines for multi-channel sample switching. The V5 multi-port valve has port 4 connected to an inlet line via a three-way valve, which houses an air pump. Port 5 is connected to a waste line. Ports 3 and 6 are connected to the two ends of the first metering loop. Port 2 is connected to a carrier injection pump via a three-way valve, and port 1 is connected to a diluent injection pump. The V6 multi-port valve has port 6 connected to a waste line, port 3 connected to a carrier line, ports 2 and 5 connected to the two ends of the second metering loop, port 4 connected to one port of the V5 multi-port valve, and port 1 connected to the V7 multi-port valve via a pipeline.

[0032] The V3 multi-port valve has multiple ports connected to standard solution tubing of different concentrations, with port 11 connected to the cleaning solution tubing. The V4 multi-port valve has port 3 connected to the V3 multi-port valve, port 1 connected to the loading solution tubing, ports 2 and 5 connected to the two ends of the third metering loop, and port 4 connected to the waste injection pump and waste tubing via a three-way valve. The V7 three-way valve has one port connected to port 1 of the V6 multi-port valve, one port connected to port 6 of the V4 multi-port valve, and one port connected to the inlet of the peristaltic pump. The outlet of the peristaltic pump is connected to the ICP-MS detection instrument.

[0033] The sample pretreatment system for anhydrous acid detection of this utility model includes a standard solution sampling and injection process and a sample sampling and injection process. The standard solution sampling and injection process includes the following steps: standard solution sampling, standard solution injection, and standard solution washing.

[0034] Standard solution sampling: such as Figure 2 As shown, switch the V3 multi-way valve to connect the standard solution pipeline with the V4 multi-way valve. Switch the V4 multi-way valve to connect valve ports 3, 2, the third metering loop, 5, and 4. The standard solution enters the third metering loop, and any excess standard solution is discharged through the waste liquid pipeline, thus completing the standard solution sampling.

[0035] Standard solution injection: such as Figure 3 As shown, switch the V4 multi-way valve to connect valve ports 1, 2, the third metering loop, 5, and 6. Then switch the V7 multi-way valve to connect valve port 4 of the V4 multi-way valve to the inlet of the peristaltic pump. The liquid-carrying pipeline feeds into valve port 1 of the V4 multi-way valve, pushing the standard solution in the third metering loop into the peristaltic pump. The peristaltic pump delivers the standard solution to the ICP-MS detection instrument.

[0036] The following steps are required for the sampling and injection of anhydrous acid: anhydrous acid sampling, anhydrous acid dilution, and anhydrous acid injection.

[0037] Anhydrous acid sampling: such as Figure 4 As shown, switch the V5 multi-way valve to connect valve ports 4, 3, the first metering ring, 6, and 5. The anhydrous acid inlet pipe feeds into the V5 multi-way valve, filling the first metering ring. Excess anhydrous acid is discharged through the waste acid pipeline, completing the anhydrous acid sampling.

[0038] Anhydrous acid dilution: such as Figure 5 As shown, switch the V5 multi-way valve to connect valve ports 2, 3, the first metering loop, 6, and 1. Then switch the V6 multi-way valve to connect valve ports 4, 5, the second metering loop, 2, and 3. The diluent injection pump injects the diluent into valve port 1 of the V5 multi-way valve. The diluent flows along valve port 1 and outflow port, enters valve port 4 of the V6 multi-way valve, and then enters the second metering loop. The carrier injection pump injects the carrier liquid into valve port 2 of the V5 multi-way valve, transferring the anhydrous acid from the first metering loop to the second metering loop, where it mixes with the diluent. The diluted anhydrous acid is then stored in the second metering loop.

[0039] Anhydrous acid injection: such as Figure 6 As shown, switch the V6 multi-way valve to connect valve ports 6, 5, the second metering loop, 2, and 1; then switch the V7 multi-way valve to connect valve port 1 of the V6 multi-way valve to the peristaltic pump. The carrier fluid is introduced into the V6 multi-way valve through the carrier line, delivering the anhydrous acid from the second metering loop to the peristaltic pump. The peristaltic pump then supplies the anhydrous acid to the ICP-MS analyzer.

[0040] This utility model's sample pretreatment system for anhydrous acid detection achieves automatic sampling, dilution, injection, and cleaning of standard solutions and anhydrous acids through the coordinated switching of multi-port valves and the linkage of syringe pumps and peristaltic pumps, reducing manual intervention and operational errors. By configuring peristaltic pumps and multiple syringe pumps (for carrier liquid, diluent, and waste liquid), precise control of liquid delivery volume is ensured, improving the consistency of dilution ratios and injection, and enhancing the accuracy of test results. The separate design of the mounting box and the fixing box optimizes space layout; leakage of highly corrosive anhydrous acid will not damage the multi-port valves through which the anhydrous acid does not flow, requiring only replacement of the multi-port valves within the mounting box, resulting in low maintenance costs and high operational safety. The independent waste liquid pipeline and waste liquid syringe pump design, combined with the automatic cleaning function in the standard solution / sample flow, effectively avoids cross-contamination and ensures system cleanliness.

[0041] The above are merely preferred embodiments of the present utility model and are not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model shall be included within the protection scope of the present utility model.

Claims

1. A sample pretreatment system for anhydrous acid detection, characterized in that, It includes an installation box and V1 multi-way valve, V5 multi-way valve, first metering ring, and air inlet pipe located inside the installation box, as well as V3 multi-way valve, V4 multi-way valve, V6 multi-way valve, V7 multi-way valve, peristaltic pump, second metering ring, third metering ring, waste liquid injection pump, carrier liquid injection pump, and diluent injection pump located outside the installation box. Several valve ports of the V1 multi-way valve are connected to the anhydrous acid inlet pipe, and the air inlet pipe is connected to the valve port of the V1 multi-way valve and one valve port of the V5 multi-way valve through a three-way valve. One valve port of the V5 multi-way valve is connected to the waste liquid pipe, and the other valve port is connected to one valve port of the V6 multi-way valve. The two valve ports are respectively connected to the two ends of the first metering ring. One valve port of the V6 multi-port valve is connected to the waste liquid pipe, one valve port is connected to the liquid carrier pipe, and the two valve ports are respectively connected to the two ends of the second metering ring. Several valve ports of the V3 multi-way valve are connected to the standard solution pipeline, and one valve port is connected to the cleaning solution pipeline; one valve port of the V4 multi-way valve is connected to the valve port of the V3 multi-way valve, one valve port is connected to the liquid carrier pipeline, and two valve ports are respectively connected to the two ends of the third metering ring. The three valve ports of the V7 multi-way valve are respectively connected to one valve port of the V6 multi-way valve, one valve port of the V4 multi-way valve, and the inlet of the peristaltic pump through pipelines. The waste liquid injection pump is connected to the waste liquid pipe and one valve port of the V4 multi-way valve via a three-way valve. The liquid carrier injection pump is connected to the liquid carrier tube and one port of the V5 multi-way valve via a three-way valve; the diluent injection pump is connected to the diluent tube and one port of the V5 multi-way valve via a three-way valve.

2. The sample pretreatment system for anhydrous acid detection according to claim 1, characterized in that, The installation box includes a box body, which is a rectangular structure with an open front end. A door is hinged to the open end of the box body, and an observation window is provided on the door.

3. The sample pretreatment system for anhydrous acid detection according to claim 2, characterized in that, The sample pretreatment system also includes a fixed box, in which the V3 multi-way valve, V4 multi-way valve, V6 multi-way valve, V7 multi-way valve, peristaltic pump, second metering ring, third metering ring, waste liquid injection pump, carrier liquid injection pump, and diluent injection pump are installed.

4. The sample pretreatment system for anhydrous acid detection according to claim 1, characterized in that, The nine ports of the V1 multi-port valve are respectively connected to nine anhydrous acid inlet pipes.

5. The sample pretreatment system for waterless acid detection according to claim 1, wherein, The V3 multi-way valve is a twelve-channel valve, the V4 multi-way valve is a two-position six-way valve, the V5 multi-way valve is a two-position seven-way valve, the V6 multi-way valve is a two-position six-way valve, and the V7 multi-way valve is a two-position three-way valve.

6. The sample pretreatment system for waterless acid detection according to claim 1, wherein, An air pump is installed on the air intake pipe.

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