System for testing VOCs released by material

Abstract

The utility model discloses a system for testing VOCs released by a material, and belongs to the technical field of VOC testing. Comprising a bag type environmental chamber, a chemical ionization source and a mass spectrometer, the bag type environmental chamber is communicated with the chemical ionization source, and the chemical ionization source is communicated with the mass spectrometer; the bag type environment chamber comprises a water bath kettle, a bubbling bottle, an environment air bag, a constant temperature box and an auxiliary air bag, the environment air bag and the auxiliary air bag are arranged in the constant temperature box, and the environment air bag is communicated with the auxiliary air bag; the bubbling bottle is arranged in the water bath kettle, the water bath kettle is communicated with the environment air bag, and the environment air bag is communicated with the chemical ionization source. The environment air bag can be cleaned through cooperation of the auxiliary air bag and the constant-temperature box, a new air bag does not need to be replaced, the experiment cost is reduced, and the implementation efficiency is improved; the problems that the mass spectrum analysis efficiency is low and the time resolution of mass spectrum analysis is influenced due to the fact that environment starting is manually replaced are solved.

Description

Technical Field

[0001] The utility model relates to the technical field of VOC testing, in particular to a material-released VOCs testing system. Background Art

[0002] The statements herein merely provide background art related to the present invention and do not necessarily constitute prior art.

[0003] Pollutants that may be present in indoor (micro)environments mainly include formaldehyde, benzene series, nitric oxide, sulfur dioxide, nitrogen oxides, and various VOCs. Among the various indoor pollutants, VOCs are of the greatest concern because their persistent volatility can have long-term negative impacts on human health.

[0004] The environmental chamber test method is a method for testing and evaluating the release of toxic and hazardous substances under conditions that most closely resemble actual use. It is an internationally recognized method for studying the release of toxic and hazardous substances from materials. By placing samples in a test chamber under the same indoor conditions, the method simulates the release of toxic and hazardous gases from materials in an indoor (micro)environment.

[0005] However, existing environmental chambers use a single airbag system. After simulating the release of volatile organic compounds (VOCs) from sample materials, the airbag must be manually replaced for the next round of simulation experiments. However, during this manual airbag replacement process, the relocation of the gas circuit and related accessories increases sample analysis time, thereby affecting the temporal resolution of mass spectrometry analysis. Utility Model Content

[0006] In view of the shortcomings of the existing technology, the purpose of the embodiment of the present utility model is to provide a material release VOCs testing system to solve the problem of increased sample analysis time caused by manual replacement of air bags.

[0007] In order to achieve the above objectives, the present invention provides the following technical solutions:

[0008] A material release VOCs testing system includes a bag-type environmental chamber, a chemical ionization source, and a mass spectrometer, wherein the bag-type environmental chamber is connected to the chemical ionization source, and the chemical ionization source is connected to the mass spectrometer;

[0009] The bag-type environmental chamber includes a water bath, a bubbling bottle, an environmental air bag, a constant temperature box and an auxiliary air bag. The environmental air bag and the auxiliary air bag are arranged in the constant temperature box; the bubbling bottle is arranged in the water bath, the bubbling bottle is connected to the environmental air bag, and the environmental air bag is connected to the chemical ionization source.

[0010] By adopting the above technical solution, after a simulation experiment is completed, the sample in the environmental air bag is removed and dry air is filled into the environmental air bag until the volume of the gas inside the environmental air bag is equal to the volume inside the constant temperature box; the environmental air bag is opened, and dry air is filled into the auxiliary air bag. Under the squeezing action of the auxiliary air bag, the gas in the environmental air bag is discharged until the volume of the gas inside the auxiliary air bag is equal to the volume inside the constant temperature box, completing one cleaning; based on the above component design and working method, there is no need to manually replace the air bag, which improves the experimental efficiency of the system and reduces the experimental cost.

[0011] In some embodiments, the chemical ionization source includes an ionization chamber, in which a vacuum ultraviolet lamp, a lamp holder electrode, a photoelectron electrode, a transmission electrode and a metal capillary are sequentially arranged from top to bottom, and the metal capillary is connected to the mass spectrometer.

[0012] A reagent ion zone is formed between the lamp holder electrode and the photoelectron electrode, and an ionization zone is formed between the photoelectron electrode and the transmission electrode.

[0013] By adopting the above technical solution, the sample generated by the bag-type environmental chamber is transmitted to the chemical ionization source, and undergoes molecular ion reaction with the reagent ions ionized by vacuum ultraviolet light to achieve chemical ionization.

[0014] In some embodiments, the chemical ionization source further comprises a reagent bottle, wherein the reagent bottle is used to store acetone;

[0015] The reagent bottle is communicated with the ionization chamber.

[0016] By adopting the above technical solution, the gas in the nitrogen headspace purging reagent bottle enters the reagent ion area between the lamp holder electrode and the photoelectron electrode, and is ionized into reagent ions under the irradiation of vacuum ultraviolet light.

[0017] In some embodiments, the bubbling bottle is connected to a first pipe and a second pipe, and the first pipe is provided with a first gas mass flow controller;

[0018] The second pipeline is connected to a third pipeline and a fourth pipeline through a tee. The third pipeline is provided with a second gas mass flow controller. The fourth pipeline is provided with a solenoid valve and is connected to the environmental air bag.

[0019] By adopting the above technical solution, ultrapure water is placed in the bubbling bottle, the ultrapure water is heated by a water bath, and the humidity of the air input into the environmental air bag is regulated by inputting dry air at different flow rates.

[0020] In some embodiments, the environmental air bag is connected to a fourth pipe, and the fourth pipe is provided with a solenoid valve;

[0021] The fourth pipeline is connected to a fifth pipeline and a sixth pipeline through a tee, and the sixth pipeline is connected to the chemical ionization source.

[0022] By adopting the above technical solution, the fifth pipe is used to discharge excess gas, and the sixth pipe is used to flow the sample in the environmental air bag into the chemical ionization source.

[0023] In some embodiments, the auxiliary air bag is connected to a seventh pipeline and an eighth pipeline, the seventh pipeline and the eighth pipeline are respectively provided with a solenoid valve, and the eighth pipeline is provided with a fourth gas mass flow controller.

[0024] By adopting the above technical solution, the gas (pressure) in the auxiliary air bag is released through the seventh pipe, and dry air is filled into the auxiliary air bag through the eighth pipe.

[0025] In some embodiments, the fourth gas mass flow controller is a Sevenstar MassFlow Controller D07-26 model, and the solenoid valve is a Takasago MTV-2-M6GHT-20 model.

[0026] In some embodiments, a ninth pipeline is further included, wherein the ninth pipeline is connected to the chemical ionization source; and the ninth pipeline is provided with a sixth gas mass flow controller.

[0027] By adopting the above technical solution, gas is replenished into the chemical ionization source through the ninth pipeline.

[0028] In some embodiments, the environmental air bag is made of Tedlar film, perfluoroalkoxy resin, polyetheretherketone material or Teflon material.

[0029] By adopting the above technical solution, the manufacturing cost of the environmental air bag is reduced.

[0030] In some embodiments, the mass spectrometer is a time-of-flight mass spectrometer or a quadrupole mass spectrometer.

[0031] One or more technical solutions provided by this utility model have at least the following technical effects or advantages:

[0032] 1. The technical solution provided by the utility model utilizes the cooperation of auxiliary air bags, environmental air bags and constant temperature chambers to realize self-cleaning of environmental air bags. After cleaning several times, the next round of simulation experiments can be carried out without manual replacement of air bags, avoiding the impact of rearrangement of air circuits and related accessories on sample analysis time, improving experimental efficiency and reducing experimental costs.

[0033] 2. The technical solution provided by the utility model utilizes a bubbling bottle and a water bath to generate humidified air with different humidity levels by inputting dry air at different flow rates, thereby regulating the humidity of the air input into the environmental air bag, and thus simulating the release of VOCs from sample materials under different humidity environments in summer and winter.

[0034] 3. The technical solution provided by the utility model places the air bag in a constant temperature box, which not only ensures the stable release of VOCs in the material during the sample detection process, but also can increase the temperature to above 120°C during the air bag cleaning process, effectively removing VOCs remaining in the environmental air bag from the previous round of samples, thereby improving the accuracy of sample detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The drawings in the specification, which constitute a part of the present invention, are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation on the present invention.

[0036] Figure 1 This is a schematic structural diagram of a material VOCs release testing system provided by an embodiment of the present utility model;

[0037] Figure 2 This is a schematic diagram of the switch status of each component in the material release VOCs testing system provided by an embodiment of the present utility model;

[0038] Figure 3 This is an example of a mass spectrum obtained when the Applied Materials VOCs Release Testing System provided in an embodiment of the present invention detects formamide and ammonia released from a foam floor mat;

[0039] Figure 4 An example graph of the trend of formamide and ammonia released from a foam floor mat detected by the Applied Materials VOCs release testing system for 28 consecutive days is provided in an embodiment of the present invention.

[0040] In the figure: 1. Bag-type environmental chamber; 2. Chemical ionization source; 3. Mass spectrometer; 4. Solenoid valve No. 1; 5. Auxiliary air bag; 7. Sample; 8. Environmental air bag; 9. Solenoid valve No. 2; 10. Bubble bottle; 11. Water bath; 12. Solenoid valve No. 3; 13. Solenoid valve No. 4; 14. Reagent bottle; 15. Lamp holder electrode; 16. Vacuum ultraviolet lamp; 17. Metal capillary; 18. Transfer electrode; 19. Photoelectron electrode.

[0041] In order to show the positions of various parts, the distances or sizes between them are exaggerated. The schematic diagram is for reference only. DETAILED DESCRIPTION

[0042] It should be noted that the following detailed descriptions are illustrative and intended to provide further explanation of the present invention. Unless otherwise specified, all technical and scientific terms used in the present invention have the same meanings as those commonly understood by those skilled in the art to which the present invention belongs.

[0043] Explanation of terms:

[0044] Headspace purging: It is a method that uses flowing gas to "purge" the volatile components in the sample7.

[0045] Example 1

[0046] As introduced in the background technology, the existing VOCs testing system requires manual replacement of air bags, resulting in a decrease in experimental efficiency and a reduction in experimental costs. In order to solve the above technical problems, the utility model proposes a material release VOCs testing system, which adds an auxiliary air bag 5 and places the auxiliary air bag 5 and the environmental air bag 8 in a constant temperature box to achieve effective removal of the previous round of experimental samples 7 in the environmental air bag 8.

[0047] Combine Figures 1-4 The material release VOCs test system includes a bag-type environmental chamber 1, a chemical ionization source 2 and a mass spectrometer 3. The bag-type environmental chamber 1 includes a water bath 11, a bubbling bottle 10, an environmental air bag 8, a constant temperature box and an auxiliary air bag 5. The chemical ionization source 2 includes an ionization chamber and a reagent bottle 14. A vacuum ultraviolet lamp 16, a lamp holder electrode 15, a photoelectron electrode 19, a transmission electrode 18 and a metal capillary 17 are installed in the ionization chamber from top to bottom. The metal capillary 17 is connected to the mass spectrometer 3; the vacuum ultraviolet lamp 16 is used to emit ultraviolet light and photoionize sample 7 molecules; the lamp holder electrode 15, the photoelectron electrode 19 and the transmission electrode 18 are used to transmit ions, the metal capillary 17 is used for vacuum differential, and the reagent bottle 14 is used to place acetone.

[0048] Furthermore, the bubbling bottle 10 is placed in a water bath 11, and the environmental air bag 8 and the auxiliary air bag 5 are placed inside the constant temperature box; the bubbling bottle 10 is connected to a first pipe and a second pipe, a first gas mass flow controller is installed on the first pipe, the second pipe is connected to a third pipe and a fourth pipe through a tee, the third pipe is installed with a second gas mass flow controller, and the fourth pipe is installed with a No. 2 solenoid valve 9 and is connected to the air inlet of the environmental air bag 8.

[0049] During the simulated release test, the first pipe and the first gas mass flow controller are used to input dry air into the bubbling bottle 10, and the dry air enters the bubbling bottle 10 to obtain high-humidity air; the third pipe and the second gas mass flow controller are used to input dry air and mix it with the high-humidity air output from the bubbling bottle 10 at the tee to obtain air with a certain humidity and input it into the ambient air bag 8 through the fourth pipe and the solenoid valve until the gas inside the ambient air bag 8 is equal to the volume inside the constant temperature box.

[0050] The environmental air bag 8 has an outlet connected to a fourth pipe. A third solenoid valve 12 and a tee are installed in sequence along the gas outflow direction. The fourth pipe is connected to a fifth and sixth pipes via the tee. The sixth pipe is connected to the ionization chamber and is equipped with a third mass flow controller. The outlet of the sixth pipe is located between the lamp holder electrode 15 and the photoelectron electrode 19. The humidified gas in the environmental air bag 8 flows into the chemical ionization source 2 through the fourth and sixth pipes, and excess gas is discharged through the fourth and fifth pipes.

[0051] The ionization chamber is connected to a ninth and tenth pipeline. A sixth gas mass flow controller is mounted on the ninth pipeline, with its gas inlet located below the transmission electrode 18. A fifth gas mass flow controller is mounted on the tenth pipeline, with its gas outlet connected to a sealed chamber. Reagent bottle 14 is placed in the sealed chamber. The other side of the sealed chamber is connected to a gas channel, with its gas outlet located between the lamp holder electrode 15 and the photoelectron electrode 19. Nitrogen gas is purged from the reagent bottle 14 through the tenth pipeline and the fifth gas mass flow controller, causing it to enter the reagent ion region between the lamp holder electrode 15 and the photoelectron electrode 19, where it is ionized into reagent ions under the irradiation of vacuum ultraviolet light.

[0052] When the experimenter deems it necessary to supplement the gas, the supplementary gas enters the area between the transmission electrode 18 and the metal capillary 17 through the ninth pipeline and the sixth gas mass flow controller.

[0053] The mass spectrometer 3 is a time-of-flight mass spectrometer or a quadrupole mass spectrometer. In this embodiment, a time-of-flight mass spectrometer is used, and the model of the time-of-flight mass spectrometer is the "YF-TOF-1500 Time-of-Flight Mass Spectrometer" of Guangdong Yingfeng Technology Co., Ltd.; the outer diameter of the metal capillary 17 is 1 / 16 inch, the inner diameter is 0.75 mm, and the length is 40 mm. The model of the gas mass flow controller is the Sevenstar Mass Flow Controller D07-26 model, the model of the solenoid valve is the Takasago MTV-2-M6GHT-20 model, and the model of the constant temperature box is the Taisite101-1AB model.

[0054] Furthermore, the air outlet of the auxiliary air bag 5 is connected to the seventh pipe, the air inlet of the auxiliary air bag 5 is connected to the eighth pipe, the fourth solenoid valve 13 is installed on the seventh pipe, and the fourth gas mass flow controller and the No. 1 solenoid valve 4 are installed in sequence on the eighth pipe along the gas flow direction.

[0055] In this embodiment, the first pipe, the second pipe, the third pipe, the fourth pipe, the fifth pipe, the sixth pipe, the seventh pipe, the eighth pipe, the ninth pipe and the tenth pipe are all made of polytetrafluoroethylene.

[0056] When the bag-type environmental chamber 1 is cleaned, the material release VOCs testing system described in this embodiment works as follows:

[0057] Remove sample 7 from ambient air bag 8. Adjust the incubator's temperature to 120°C. Open solenoid valves 13 and 9, and pump dry air into the ambient air bag 8 at a rate of 2 L / min via the second mass flow controller. After 5 minutes, the volume of air inside the ambient air bag 8 will equal the volume inside the incubator. Close solenoid valves 13 and 9, respectively. Open solenoid valves 12 and 4, and pump dry air into the auxiliary air bag 5 at a rate of 2 L / min via the fourth mass flow controller. As the volume of the auxiliary air bag 5 expands, the air in the ambient air bag 8 is squeezed out of its outlet until the volume of air inside the auxiliary air bag 5 equals the volume inside the incubator. The air inside the ambient air bag 8 is completely exhausted, completing the purge. Repeat this process 3-5 times before proceeding to the next sample 7.

[0058] During the simulated release test, the VOCs release test system of the material described in this embodiment works as follows:

[0059] After the water bath 11 heats the ultrapure water to 50°C, dry air is input into the bubbling bottle 10 at 0.2L / min through the first air mass flow controller to obtain high-humidity air, and is mixed with the dry air input at 0.3L / min controlled by the first air mass flow controller at the tee to obtain 50% humidity air and input into the environmental air bag 8.

[0060] Sample 7 was placed in ambient air bag 8 of a thermostat, and the thermostat was set to 25°C. Solenoid valve No. 4 (13) and solenoid valve No. 2 (9) at the air inlet of ambient air bag 8 were opened. Air with a predetermined humidity was introduced into ambient air bag 8 at a flow rate of 0.5 L / min until the volume of air inside ambient air bag 8 equaled the volume of the thermostat's internal chamber (10 L). Solenoid valve No. 3 (12) at the air outlet was opened, and solenoid valve No. 4 (13) was closed. The outflowing gas was controlled by a third mass flow controller and entered chemical ionization source 2 at a flow rate of 0.4 L / min. Excess gas was discharged through a three-way valve.

[0061] After the test is completed, close all solenoid valves and MFC.

[0062] Here, Sample 7 refers to floor mats or other items containing VOCs.

[0063] Figure 3 This is the mass spectrum obtained when using the VOCs release test system described in this example to detect formamide and ammonia released from a foam floor mat. The detection time for a single sample 7 was 30 seconds. The acetone dimer hydrogenation peak [RH]+ (m / z = 117) is the primary reagent ion peak, while [RH]+ (m / z = 59) is the acetone monomer hydrogenation peak. [NH3+RH]+ (m / z = 76) is the adduct peak of acetone monomer and ammonia, while [NH3+RH]+ (m / z = 134) is the adduct peak of acetone dimer and ammonia. [CH3NO+RH]+ (m / z = 104) is the adduct peak of acetone monomer and formamide.

[0064] Figure 4 This is a trend chart of formamide and ammonia released from foam floor mats using the VOCs release testing system of the material described in this embodiment for 28 consecutive days. It can be seen that the concentrations of formamide and ammonia released from the foam floor mats gradually decrease with increasing environmental exposure time.

[0065] Although the above describes the specific implementation methods of the present invention in conjunction with the accompanying drawings, it does not limit the scope of protection of the present invention. Technical personnel in the relevant field should understand that on the basis of the technical solution of the present invention, various modifications or variations that can be made by technical personnel in this field without creative work are still within the scope of protection of the present invention.

Claims

1. A material release VOCs testing system, characterized in that: It comprises a bag-type environmental chamber, a chemical ionization source and a mass spectrometer, wherein the bag-type environmental chamber is connected to the chemical ionization source, and the chemical ionization source is connected to the mass spectrometer; The bag-type environmental chamber includes a water bath, a bubbling bottle, an environmental air bag, a constant temperature box and an auxiliary air bag. The environmental air bag and the auxiliary air bag are arranged in the constant temperature box; the bubbling bottle is arranged in the water bath, the bubbling bottle is connected to the environmental air bag, and the environmental air bag is connected to the chemical ionization source.

2. The material release VOCs testing system according to claim 1, characterized in that: The chemical ionization source includes an ionization chamber, in which a vacuum ultraviolet lamp, a lamp holder electrode, a photoelectron electrode, a transmission electrode and a metal capillary are sequentially arranged from top to bottom, and the metal capillary is connected to the mass spectrometer; A reagent ion zone is formed between the lamp holder electrode and the photoelectron electrode, and an ionization zone is formed between the photoelectron electrode and the transmission electrode.

3. The material release VOCs testing system according to claim 2, characterized in that: The chemical ionization source further comprises a reagent bottle, wherein the reagent bottle is used to store acetone; The reagent bottle is communicated with the ionization chamber.

4. The material release VOCs testing system according to claim 1, characterized in that: The bubbling bottle is connected to a first pipeline and a second pipeline, and the first pipeline is provided with a first gas mass flow controller; The second pipeline is connected to a third pipeline and a fourth pipeline through a tee. The third pipeline is provided with a second gas mass flow controller. The fourth pipeline is provided with a solenoid valve and is connected to the environmental air bag.

5. The material release VOCs testing system according to claim 1, characterized in that: The environmental air bag is connected to a fourth pipeline, and the fourth pipeline is provided with a solenoid valve; The fourth pipeline is connected to a fifth pipeline and a sixth pipeline through a tee, and the sixth pipeline is connected to the chemical ionization source.

6. The material release VOCs testing system according to claim 1, characterized in that: The auxiliary air bag is connected to a seventh pipeline and an eighth pipeline. The seventh pipeline and the eighth pipeline are respectively provided with a solenoid valve, and the eighth pipeline is provided with a fourth gas mass flow controller.

7. The material release VOCs testing system according to claim 6, characterized in that: The model of the fourth gas mass flow controller is Sevenstar Mass Flow Controller D07-26, and the model of the solenoid valve is Takasago MTV-2-M6GHT-20.

8. The material release VOCs testing system according to claim 7, characterized in that: It also includes a ninth pipeline, which is connected to the chemical ionization source; the ninth pipeline is provided with a sixth gas mass flow controller.

9. The material release VOCs testing system according to claim 1, characterized in that: The environmental air bag is made of Tedlar film, perfluoroalkoxy resin, polyetheretherketone material or Teflon material.

10. The material release VOCs testing system according to claim 1, characterized in that: The mass spectrometer is a time-of-flight mass spectrometer or a quadrupole mass spectrometer.

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