Gaseous molecular pollutant detection method

Abstract

The invention relates to a gaseous molecular pollutant detection method which comprises the following steps: step 1, building a tool: a gas holder or to-be-detected gas is respectively connected with a left side pipeline and a right side pipeline through a four-way valve, the right side pipeline is an organic end, the right side pipeline is connected with an organic end sampling pump through an adsorption pipe, the left side pipeline is an inorganic end, and the right side pipeline is connected with an organic end sampling pump through an adsorption pipe; the left side pipeline is connected with the absorption bottle and the inorganic end sampling pump; step 2, setting sampling parameters: setting the sampling flow of an organic end to be 0.15 L / min and the sampling time to be 24 hours, and setting the sampling flow of an inorganic end to be 2L / min and the sampling time to be 24 hours; step 3, blank sampling: opening a sealing film of the absorption bottle, sealing after waiting for 30 seconds, placing the absorption bottle on site, opening brass caps at two ends of the absorption tube, screwing the absorption tube after waiting for 30 seconds, and placing the absorption tube on site; and step 4, testing process: clicking START / STOP to start gas production, automatically stopping 24 hours later, recording the inorganic end sampling pump and the sampling flow on the inorganic end sampling pump, and participating in subsequent calculation.

Description

Technical Field

[0001] This invention relates to the field of detection, specifically to a method for detecting gaseous molecular pollutants. Background Technology

[0002] In semiconductor manufacturing, gaseous molecular contaminants (AMCs) are trace amounts of harmful gases invisible to the naked eye in clean environments. The core issue is that even low concentrations can cause irreversible damage in precision manufacturing and scientific research settings, and traditional control methods struggle to achieve comprehensive and high-precision treatment across all categories. There are limited methods for rapidly, effectively, and reasonably evaluating AMCs in clean environments. It is necessary to consider both the sampling equipment and the AMC content of the sampled gas to avoid biasing the AMC results of the tested environment. Summary of the Invention

[0003] In view of the problems existing in the prior art, the present invention provides a method for detecting gaseous molecular pollutants, which has solved at least one of the above-mentioned technical problems.

[0004] The technical solution of the present invention is: a method for detecting gaseous molecular pollutants, characterized by comprising the following steps:

[0005] Step 1, Set up the fixture: Connect the gas holder or the gas to be tested to the left and right pipelines respectively through a four-way valve. The right pipeline is the organic end, and the right pipeline is connected to the organic end sampling pump through an adsorption tube. The left pipeline is the inorganic end, and the left pipeline is connected to the absorption bottle and the inorganic end sampling pump.

[0006] Step 2, set sampling parameters: set the organic end sampling flow rate to 0.15L / min and the sampling time to 24h, and the inorganic end sampling flow rate to 2L / min and the sampling time to 24h.

[0007] Step 3, sampling blank: Unseal the absorption bottle, wait 30 seconds and then reseal it, place it on site; open the brass caps at both ends of the adsorption tube, wait 30 seconds and then screw them back on, place it on site;

[0008] Step 4, Testing Process: Click START / STOP to start gas sampling. It will automatically stop after 24 hours. Record the sampling flow rate of the inorganic end sampling pump and the sampling flow rate on the inorganic end sampling pump for subsequent calculations.

[0009] Step 5, Post-test: After gas sampling, remove the adsorption tube, tighten the brass caps at both ends, wrap it with aluminum foil, pack it in a PE bag, place it in the original packaging box, and send it out within 24 hours after sampling; remove the adsorption bottle, wrap both bottle openings with sealing film, pack it in a PE bag, place it in the original sampling box, and send it out within 24 hours after sampling;

[0010] Step 6, Result Calculation: Using the normalization method, calculate the sample itself and the sampling blank data. Subtract the sampling blank data from the sample and quantify it using the normalization method. Calculate the organic content with the volume of gas that passes through to obtain the organic content in the component, in ppbv.

[0011] The calibration method is used to calculate the sample itself and the sampling blank data. The sampling blank data is subtracted from the sample and quantified by substituting it into the standard curve. The inorganic content is calculated by combining the inorganic content with the volume of gas passing through it, and the inorganic content in the component can be obtained in ppbv.

[0012] This invention allows for simultaneous organic and inorganic gas sampling along with the sample, resulting in low background values ​​and reducing the impact of background values ​​on test results. The same equipment can be used to collect AMC data from gas holders of different sizes by changing port components, or the front end can be removed for direct environmental sampling.

[0013] Further preferably, both the left and right pipes are made of stainless steel, which provides sufficient strength.

[0014] Further preferably, when the gas holder or the gas to be tested is under positive pressure, the lower port of the four-way valve is used for pressure relief; when the gas holder or the gas to be tested is under negative pressure, the lower port of the four-way valve is blocked by a plug.

[0015] The same configuration is used for operation depending on the different gas sources.

[0016] In a further preferred embodiment, an anti-backflow bottle is provided between the left-side pipeline and the absorption bottle. The anti-backflow bottle is connected to an adapter via a flexible hose, and the anti-backflow bottle is connected to the left-side pipeline via the adapter. The anti-backflow bottle is also connected to the absorption bottle via a flexible hose.

[0017] This prevents backflow of gas due to pressure difference during the experiment, thus optimizing detection efficiency.

[0018] Further preferably, the right-side pipeline is connected to the adsorption tube via a connector, and the adsorption tube is connected to the organic end sampling pump via a flexible tube. The commercially available Tenax GR adsorption tube is selected.

[0019] Further preferably, the liquid in the absorption bottle is water, and the volume of the liquid in the absorption bottle is no more than two-thirds of the total volume of the absorption bottle.

[0020] ‌ Attached Figure Description

[0021] Figure 1 This is a flowchart illustrating the invention process;

[0022] Figure 2 This is a structural schematic diagram of the organic end of the present invention during use;

[0023] Figure 3 This is a structural schematic diagram of the inorganic end of the present invention during use;

[0024] Figure 4 These are the sampling parameters of the organic end of this invention;

[0025] Figure 5 These are the sampling parameters of the inorganic end of this invention.

[0026] Figure labels: 1 is a four-way valve; 2 is an adsorption tube; 3 is an organic end sampling pump; 4 is an absorption bottle; 5 is an inorganic end sampling pump; 6 is an anti-backflow bottle. Detailed Implementation

[0027] The present invention will be further described below with reference to the embodiments.

[0028] The detection method for gaseous molecular pollutants includes the following steps:

[0029] Step 1, Participate Figures 1-3 Set up the fixture: The gas holder or the gas to be tested is connected to the left and right pipelines respectively through the four-way valve 1. The right pipeline is the organic end, and the right pipeline is connected to the organic end sampling pump 3 through the adsorption tube 2. The left pipeline is the inorganic end, and the left pipeline is connected to the absorption bottle 4 and the inorganic end sampling pump 5.

[0030] Step 2, see Figure 4 and Figure 5 Set the sampling parameters: set the organic end sampling flow rate to 0.15L / min and the sampling time to 24h, and the inorganic end sampling flow rate to 2L / min and the sampling time to 24h.

[0031] Step 3, sampling blank: Unseal the absorption bottle, wait 30 seconds and then reseal it, place it on site; open the brass caps at both ends of the adsorption tube, wait 30 seconds and then screw them back on, place it on site;

[0032] Step 4, Testing Process: Click START / STOP to start gas sampling. It will automatically stop after 24 hours. Record the sampling flow rate of the inorganic end sampling pump and the sampling flow rate on the inorganic end sampling pump for subsequent calculations.

[0033] Step 5, Post-test: After gas sampling, remove the adsorption tube, tighten the brass caps at both ends, wrap it with aluminum foil, pack it in a PE bag, place it in the original packaging box, and send it out within 24 hours after sampling; remove the adsorption bottle, wrap both bottle openings with sealing film, pack it in a PE bag, place it in the original sampling box, and send it out within 24 hours after sampling;

[0034] Step 6, Result Calculation: Using the normalization method, calculate the sample itself and the sampling blank data. Subtract the sampling blank data from the sample and quantify it using the normalization method. Calculate the organic content with the volume of gas that passes through to obtain the organic content in the component, in ppbv.

[0035] The calibration method is used to calculate the sample itself and the sampling blank data. The sampling blank data is subtracted from the sample and quantified by substituting it into the standard curve. The inorganic content is calculated by combining the inorganic content with the volume of gas passing through it, and the inorganic content in the component can be obtained in ppbv.

[0036] This invention allows for simultaneous organic and inorganic gas sampling along with the sample, resulting in low background values ​​and reducing the impact of background values ​​on test results. The same equipment can be used to collect AMC data from gas holders of different sizes by changing port components, or the front end can be removed for direct environmental sampling.

[0037] Further optimization involves using stainless steel piping on both the left and right sides to provide sufficient strength.

[0038] Further optimization involves using the lower port of the four-way valve to release pressure when the gas holder or the gas to be tested is under positive pressure, and blocking the lower port of the four-way valve with a plug when the gas holder or the gas to be tested is under negative pressure.

[0039] The same configuration is used for operation depending on the different gas sources.

[0040] In a further preferred embodiment, an anti-backflow bottle 6 is provided between the left-side pipeline and the absorption bottle. The anti-backflow bottle is connected to an adapter via a hose, and the anti-backflow bottle is connected to the left-side pipeline via the adapter and to the absorption bottle via a hose.

[0041] This prevents backflow of gas due to pressure difference during the experiment, thus optimizing detection efficiency.

[0042] Further optimization involves connecting the right-side tubing to the adsorption tube via a connector, and the adsorption tube is connected to the organic sampling pump via a flexible hose. Commercially available Tenax GR adsorption tubes are selected.

[0043] Further optimization involves using water as the liquid in the absorption bottle, and ensuring that the volume of the liquid in the absorption bottle does not exceed two-thirds of the total volume of the absorption bottle.

[0044] Example results:

[0045] Testing items 012544-2 (ppbv) 012544-3 (ppbv) 012544-4 (ppbv) 012544-5 (ppbv) Total acid / / <RL <RL SO42- / / <RL <RL Filtration monitoring of total acid / / <RL <RL Total alkali / / <RL <RL NH4+ / / <RL <RL Total organic matter (IPA-C30) 0.39 1.08 / / Recalcitrant substances <RL <RL / / Filter to monitor total organic matter (C9-C30) 0.12 0.81 / /

[0046] The table displays the detection data for AMC. As shown in the example, the device can effectively collect AMC in the gas holder / test gas, and when used in conjunction with TD-GCMS / IC, it can effectively analyze the type and content of AMC.

[0047] The upper and lower limit embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. Those skilled in the art can make many equivalent modifications or substitutions without departing from the spirit of the present invention, and these equivalent modifications or substitutions are all included within the scope defined by the claims of this application.

Claims

1. A method for detecting gaseous molecular pollutants, characterized in that, Includes the following steps: Step 1, Set up the fixture: Connect the gas holder or the gas to be tested to the left and right pipelines respectively through a four-way valve. The right pipeline is the organic end, and the right pipeline is connected to the organic end sampling pump through an adsorption tube. The left pipeline is the inorganic end, and the left pipeline is connected to the absorption bottle and the inorganic end sampling pump. Step 2, set sampling parameters: set the organic end sampling flow rate to 0.15L / min and the sampling time to 24h, and the inorganic end sampling flow rate to 2L / min and the sampling time to 24h. Step 3, sampling blank: Unseal the absorption bottle, wait 30 seconds and then reseal it, place it on site; open the brass caps at both ends of the adsorption tube, wait 30 seconds and then screw them back on, place it on site; Step 4, Testing Process: Click START / STOP to start gas sampling. It will automatically stop after 24 hours. Record the sampling flow rate of the inorganic end sampling pump and the sampling flow rate on the inorganic end sampling pump for subsequent calculations. Step 5, Post-test: After gas sampling, remove the adsorption tube, tighten the brass caps at both ends, wrap it with aluminum foil, pack it in a PE bag, place it in the original packaging box, and send it out within 24 hours after sampling; remove the adsorption bottle, wrap both bottle openings with sealing film, pack it in a PE bag, place it in the original sampling box, and send it out within 24 hours after sampling; Step 6, Result Calculation: Using the normalization method, calculate the sample itself and the sampling blank data. Subtract the sampling blank data from the sample and quantify it using the normalization method. Calculate the organic content with the volume of gas that passes through to obtain the organic content in the component, in ppbv. The calibration method is used to calculate the sample itself and the sampling blank data. The sampling blank data is subtracted from the sample and quantified by substituting it into the standard curve. The inorganic content is calculated by combining the inorganic content with the volume of gas passing through it, and the inorganic content in the component can be obtained in ppbv.

2. The method for detecting gaseous molecular pollutants according to claim 1, characterized in that: Both the left and right side pipes are made of stainless steel.

3. The method for detecting gaseous molecular pollutants according to claim 1, characterized in that: When the gas holder or the gas to be tested is under positive pressure, the lower port of the four-way valve is used to release pressure; when the gas holder or the gas to be tested is under negative pressure, the lower port of the four-way valve is blocked by a plug.

4. The method for detecting gaseous molecular pollutants according to claim 1, characterized in that: An anti-backflow bottle is provided between the left-side pipeline and the absorption bottle. The anti-backflow bottle is connected to an adapter via a hose, and the anti-backflow bottle is connected to the left-side pipeline via the adapter. The anti-backflow bottle is also connected to the absorption bottle via a hose.

5. The method for detecting gaseous molecular pollutants according to claim 1, characterized in that: The right-side pipeline is connected to the adsorption tube via a connector, and the adsorption tube is connected to the organic end sampling pump via a flexible tube.

6. The method for detecting gaseous molecular pollutants according to claim 1, characterized in that: The liquid in the absorption bottle is water, and the volume of the liquid in the absorption bottle is no more than two-thirds of the total volume of the absorption bottle.

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