Method for detecting volatile organic compounds in solid component

Abstract

The invention relates to a method for detecting volatile organic compounds in a solid component, which comprises the following steps of: 1, aging micro-cabin equipment at 200 DEG C for more than 8 hours, and collecting a blank of the micro-cabin equipment; the adsorption tube is aged at 300 DEG C for 1 hour, and on-machine detection confirms that the blank of micro-cabin equipment and the blank of the adsorption tube are smaller than the detection limit of the method and meet the use requirements; step 2, transferring the sample into micro-cabin equipment by using metal tweezers, confirming that the sample can completely lie flat on the quartz stand, adding an internal standard solution (anthracene-D10) on the surface of the sample block to avoid touching a ventilated hollow pipe, tightly covering a cover of the micro-cabin equipment, and inserting an adsorption pipe; step 3, placing the adsorption tube on a thermal desorption instrument tube disc, carrying out TD-GCMS analysis according to setting, and carrying out standard sample (n-decane) detection before and after sample testing for subsequent quantitative calculation; and 4, carrying out qualitative analysis according to the peak appearance time and characteristic ions of the compound, wherein the qualitative analysis is generally carried out on the first twenty sample peaks of the peak area.

Description

Technical Field

[0001] This invention relates to the field of detection, and more specifically to a method for detecting volatile organic compounds in solid components. Background Technology

[0002] In the semiconductor industry, volatile organic compounds (VOCs) are one of the key factors affecting the performance and surface cleanliness of semiconductor devices. There are limited methods for rapidly, effectively, and reasonably evaluating the VOCs in solid-state semiconductor components. It is necessary to consider both the sufficiency of VOC volatilization from the solid-state component and the high recovery rate of the collection process to avoid biasing the VOC results of the tested solid-state component. Summary of the Invention

[0003] To address the problems existing in the prior art, the present invention provides a method for detecting volatile organic compounds in solid components, thereby solving at least one of the aforementioned technical problems.

[0004] The technical solution of the present invention is: a method for detecting volatile organic compounds in solid components, characterized by comprising the following steps:

[0005] Step 1: The micro-chamber device is aged at 200℃ for more than 8 hours, and the blank of the micro-chamber device is collected; the adsorption tube is aged at 300℃ for 1 hour, and the blank of the micro-chamber device and the adsorption tube are tested on the machine to confirm that the blank of the micro-chamber device and the blank of the adsorption tube are less than the method detection limit and meet the usage requirements.

[0006] Step 2: Use metal tweezers to transfer the sample into the microchamber device, ensuring that the sample can lie completely flat on the quartz stand. Add internal standard solution (anthracene-D10) to the surface of the sample block, avoiding contact with the venting hollow tube. Tighten the cover of the microchamber device and insert the adsorption tube.

[0007] Step 3: Place the adsorption tube on the thermal desorption instrument tray and perform TD-GCMS analysis according to the settings. Standard sample (n-decane) detection is required before and after sample testing for subsequent quantitative calculations.

[0008] Step four: Perform qualitative analysis based on the peak time and characteristic ions of the compound. Typically, qualitative analysis is performed on the top twenty sample peaks in terms of peak area.

[0009] Step 5: Quantitative analysis. Semi-quantitative analysis of the target compound is performed using n-decane as an external standard. The GC spectrum is automatically integrated using instrument software to obtain the peak area for calculation. Manual integration can be performed as needed. The VOC content of the sample is obtained by dividing the peak area ratio of the standard sample to the sample surface area by the sample surface area, in ng / cm³. 2 .

[0010] This invention achieves high VOC recovery rates and good sample repeatability by adjusting the carrier gas flow rate, temperature, and sampling time of the microcabin device. The same equipment is suitable for VOC collection from solid components of different materials. Data from the test tables show that the microcabin device can efficiently collect VOCs from solid components, and TD-GCMS can accurately analyze the compound types and contents of VOCs. This invention provides a clear view of the VOC content in solid components and achieves high recovery rates and good sample repeatability for trace VOCs.

[0011] Further preferably, the interior of the microcabin device is provided with a quartz stand, the surface of which is used to place samples, and the central axis of the quartz stand coincides with the central axis of the microcabin device.

[0012] Ensure the quartz stand is centered so that the sample does not come into contact with its surroundings when placed.

[0013] Further preferred, the microcabin device is set with a carrier gas flow rate of 300-500 mL / min, a temperature of 150-200℃, and a collection time of 20-30 min.

[0014] In a further preferred embodiment, the top of the micro-chamber device is provided with a micro-chamber device cover, and an adsorption tube is inserted into the center of the micro-chamber device cover. After the micro-chamber device completes heating according to the settings, the adsorption tube is removed, and both ends of the adsorption tube are tightly covered with a plastic cap.

[0015] This ensured a stable environment inside the micro-cabin equipment.

[0016] In a further preferred embodiment, one end of the hollow tube is connected to the carrier gas, and the other end of the hollow tube is inside the micro-cabin.

[0017] This invention optimizes the length of the hollow tube, thus enabling better operation. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the overall structure of the micro-cabin device.

[0019] Figure 2 These are the results of an embodiment of the present invention;

[0020] Figure 3 These are the organic components resulting from the embodiments of the present invention. Detailed Implementation

[0021] The present invention will be further described below with reference to the embodiments.

[0022] The detection of volatile organic compounds in this embodiment includes the following steps:

[0023] Aging micro-chamber equipment and adsorption tubes

[0024] The microcabin device was aged at 200℃ for more than 8 hours, and a blank sample was collected from the microcabin device; the adsorption tube was aged at 300℃ for 1 hour. On-machine testing confirmed that the blank samples from both the microcabin device and the adsorption tube were below the method detection limit, meeting the usage requirements.

[0025] VOC collection in samples

[0026] Using metal tweezers, transfer the sample into the microcabin device, ensuring it lies completely flat on the quartz stand 1. Add internal standard solution (anthracene-D10) to the sample surface, avoiding contact with the venting hollow tube 3. Tightly close the microcabin device lid and insert the adsorption tube 4. Set the microcabin device conditions: carrier gas flow rate 300-500 mL / min, temperature 150-200 ℃, and collection time 20-30 min. After heating according to the settings, remove the adsorption tube and tightly seal both ends with plastic caps. A schematic diagram of VOC collection using the microcabin device is shown below. Figure 1 As shown:

[0027] VOC detection in samples

[0028] Place the adsorption tube on the thermal desorption instrument tray and perform TD-GCMS analysis according to the settings. Standard sample (n-decane) analysis is required before and after sample testing for subsequent quantitative calculations.

[0029] 4. Qualitative Analysis

[0030] Qualitative analysis is performed based on the elution time and characteristic ions of the compounds. Typically, the top 20 sample peaks in terms of peak area are used for qualitative analysis.

[0031] 5. Quantitative analysis

[0032] This method uses n-decane as an external standard for semi-quantitative analysis of the target compound. The GC spectrum is automatically integrated using instrument software to obtain the peak area for calculation; manual integration can be performed as needed. The VOC content of the sample is obtained by dividing the peak area ratio of the standard sample to the sample surface area by the sample surface area, in ng / cm³. 2 The results of the examples are included. Figure 2 and Figure 3 .

[0033] This invention relates to a method for detecting volatile organic compounds (VOCs) in solid components. The test data shows that the micro-chamber device can efficiently collect VOCs from solid components, and TD-GCMS can accurately analyze the compound types and contents of VOCs. It should be noted that the embodiments are for illustrative purposes only and are not intended to limit the invention. Without departing from the spirit and essential characteristics of this invention, those skilled in the art can make various modifications to the invention in form and detail, including but not limited to adjustments to the structure of the micro-chamber device and the operating parameters of the TD-GCMS. These modified technical solutions still fall within the protection scope of this invention, the specific scope of protection being defined by the claims.

[0034] The upper and lower limit embodiments of the present invention have been specifically described above, but the present invention is not limited to the embodiments described. 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 volatile organic compounds in solid components, characterized in that, Includes the following steps: Step 1: The micro-chamber device is aged at 200℃ for more than 8 hours, and the blank of the micro-chamber device is collected; the adsorption tube is aged at 300℃ for 1 hour, and the blank of the micro-chamber device and the adsorption tube are tested on the machine to confirm that the blank of the micro-chamber device and the blank of the adsorption tube are less than the method detection limit and meet the usage requirements. Step 2: Use metal tweezers to transfer the sample into the microchamber device, ensuring that the sample can lie completely flat on the quartz stand. Add internal standard solution (anthracene-D10) to the surface of the sample block, avoiding contact with the venting hollow tube. Tighten the cover of the microchamber device and insert the adsorption tube. Step 3: Place the adsorption tube on the thermal desorption instrument tray and perform TD-GCMS analysis according to the settings. Standard sample (n-decane) detection is required before and after sample testing for subsequent quantitative calculations. Step four: Perform qualitative analysis based on the peak time and characteristic ions of the compound. Typically, qualitative analysis is performed on the top twenty sample peaks in terms of peak area. Step 5: Quantitative analysis. Semi-quantitative analysis of the target compound is performed using n-decane as an external standard. The GC spectrum is automatically integrated using instrument software to obtain the peak area for calculation. Manual integration can be performed as needed. The VOC content of the sample is obtained by dividing the peak area ratio of the standard sample to the sample surface area by the sample surface area, in ng / cm³. 2 .

2. The method for detecting volatile organic compounds in a solid component according to claim 1, characterized in that: The micro-cabin device has a quartz stand inside, the surface of which is used to place samples, and the central axis of the quartz stand coincides with the central axis of the micro-cabin device.

3. The method for detecting volatile organic compounds in a solid component according to claim 2, characterized in that: The microcabin device is set to a carrier gas flow rate of 300-500 mL / min, a temperature of 150-200 ℃, and a collection time of 20-30 min.

4. The method for detecting volatile organic compounds in a solid component according to claim 2, characterized in that: The top of the micro-chamber device is equipped with a micro-chamber device cover, and an adsorption tube is inserted into the center of the micro-chamber device cover. After the micro-chamber device completes heating according to the settings, the adsorption tube is removed and the two ends of the adsorption tube are tightly covered with a plastic cap.

5. The method for detecting volatile organic compounds in a solid component according to claim 2, characterized in that: One end of the hollow tube is connected to the carrier gas, and the other end of the hollow tube is inside the micro-cabin.

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