JP2006091000A - Method for measuring amount of pollutant diffusion - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To simply measure a diffusion amount of pollutant where diffusions from an end and a backside do not occur, without using any seal box. <P>SOLUTION: Two catching tubes are connected by a connector, and a test body 1 is completely enclosed by an aluminum foil or a copper foil, and then a portion with a prescribed dimension of above metallic foil existing on the surface side of the test body is cut out in order to make only the surface side exposed, thereby making up the test body which is contained in the upstream catching tube used as the primary catching tube 7 being also used for volatilizing, and the downstream catching tube which is used as the secondary catching tube 8, is filled up with a catching agent 10, and a carrier gas is applied at a prescribed temperature, at a prescribed flow rate and at a prescribed timing, and a volatile organic compound which is diffused from the test body, is catched by the primary catching tube 7 and the secondary catching tube 8, and then the two catching tubes 7, 8 are respectively set to a thermal desorption section of a thermal desorption type gas chromatograph mass spectrometer (GC/MS), and the total diffusion amount of the volatile organic compound is computed. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for measuring pollutant emissions of volatile organic compounds.

  In recent years, with increasing health consciousness, “sick house syndrome” caused by chemical substances emitted from building materials and construction materials has become a social problem, and in chemical and liquid crystal manufacturing clean rooms, etc., it can cause yield reduction due to the adhesion of chemical substances emitted. Accordingly, it is important to measure the concentration of a very small amount of chemical substance existing in the air.

  Examples of indoor air pollution sources include supervolatile organic compounds (VVOC), volatile organic compounds (VOC), and semivolatile organic compounds (SVOC) generated from building materials and construction materials.

  As a method for measuring the concentration of the volatile organic compounds from building materials, the “small chamber method” was established in JIS A 1901 in January 2003. In this small chamber method, among the volatile organic compounds, super volatile organic compounds (VVOC) and volatile organic compounds (VOC) are specified, but phthalates and phosphates having higher boiling points are specified. The semi-volatile organic compound (SVOC) represented by is not defined.

  However, the semivolatile organic compound (SVOC) is contained in various building materials and household products as a plasticizer and flame retardant, and is a hazardous substance that is also included in the guidelines of the Ministry of Health, Labor and Welfare. Development of a method capable of accurately measuring volatile organic compounds (VVOC) and semi-volatile organic compounds (SVOC) together with volatile organic compounds (VOC) is desired.

  However, the measurement of the emission amount of the semivolatile organic compound (SVOC) is that the SVOC component has a very low concentration in the air and requires a large amount of trapping. However, there was a problem that it could not be measured accurately.

  Therefore, in the following Non-Patent Document 1, as shown in FIG. 4A, a microchamber 51 in which a test body 50 is set is installed in a thermostat 52 for a radiation test, and a semivolatile organic compound ( In order to dissipate the SVOC) and then desorb the semivolatile organic compound (SVOC) adhering to the inner wall of the microchamber 51, as shown in FIG. Is installed in the chamber heating device 53, heated at 220 ° C. for 45 minutes, collected with an inert gas and collected by a collecting tube 54 (TenaxTA), and then collected by a gas chromatograph mass spectrometer (GC / MS). There has been proposed a method (conventional method 1) for calculating the amount of emission by performing qualitative / quantitative analysis of minutes.

  In the case of this method, when the semivolatile organic compound (SVOC) is heated and desorbed, the line up to the microchamber 51 and the collection tube 54 needs to be heated uniformly, so that a large chamber heating device 53 is required.

Therefore, as a simpler evaluation method (conventional method 2), the following Non-Patent Document 2 proposes a method using a collection tube (Tenax tube) made of quartz glass directly instead of a chamber. Specifically, as shown in FIG. 5, two collection tubes 56 and 57 are connected by a connector, and a test body 58 is accommodated in the upstream collection tube 56 to serve as a primary collection tube for volatilization. The downstream collection tube 57 is filled with a collection agent 59 to form a secondary collection tube, air at a temperature of 40 ° C. is supplied at a flow rate of 1 ml / min, and the volatile organic compound released from the specimen is removed. After being collected by the primary collection tube 56 and the secondary collection tube 57, the two collection tubes 56 and 57 are respectively heated and desorbed by a thermal desorption type gas chromatograph mass spectrometer 61 (GC / MS) 60. And a method for calculating the total emission amount of volatile organic compounds has been proposed.
Building Materials Testing Center, “Standardization of Evaluation Methods for VOC Emissions from Building Materials”, March 2004, p.193-202 Shuichi Ishiwari, two others, “Volatilization behavior of high-boiling adsorbable organic substances at room temperature in clean room components”, Japan Air Cleaners Association 22nd Air Cleaner and Contamination Control Research Conference Lecture, April 2004 13-14 days, p.54-57

  In the case of the conventional method 2, the two collecting tubes 56 and 57 that collect volatile organic compounds can be directly attached to the heat desorption part 60 of the gas chromatograph mass spectrometer 61 (GC / MS). No need for a large high-temperature bath like 1 and has the advantage of being able to efficiently measure semivolatile organic compounds (SVOC) along with supervolatile organic compounds (VVOC) and volatile organic compounds (VOC) .

  However, according to JIS A 1901, it is described that the specimen for measuring the gas emission amount seals the fore edge and the back surface portion of the test piece so that the chemical substance is emitted only from the surface. Therefore, in the same rule, it is described that the seal box 62 shown in FIG. 6 is used. The seal box 62 is an instrument including a seal box main body 63, frame plates 64A to 64C interposed between the front and back surfaces of the test body to maintain airtightness, and a back cover 65.

  The seal box 62 has high functionality that eliminates the diffusion of volatile substances from the back surface of the test specimen and can be reused by cleaning and dry baking. It is too large to serve and cannot be inserted into the collection tube. Moreover, when producing a seal box of a size that can be inserted into the collection tube, there is a problem that a highly accurate work is required.

  Accordingly, a main object of the present invention is to measure the amount of pollutant diffused without using a seal box and in a state where it is simple and eliminates the radiation from the fore edge and the back surface.

  In order to solve the above-mentioned problem, as the present invention according to claim 1, after connecting two collecting tubes with a connector and completely surrounding the specimen with aluminum foil or copper foil in the upstream collecting tube, Cut the metal foil on the surface side of the test specimen to a predetermined size and store the test specimen prepared by exposing only the surface side to the primary collection pipe for volatilization and collect it in the downstream collection pipe The secondary collection tube is filled with the agent, the carrier gas at a predetermined temperature is supplied at a predetermined flow rate and for a predetermined time, and the volatile organic compound released from the test body is the primary collection tube and the secondary collection tube. The two collection tubes are set in the heat desorption section of a thermal desorption type gas chromatograph mass spectrometer (GC / MS), and the total emission amount of volatile organic compounds is calculated. A method for measuring the amount of pollutant emission is provided.

  As described above in detail, according to the present invention, it is possible to measure the pollutant emission amount without using a seal box and in a state in which the emission from the fore edge and the back surface is eliminated.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

[Preparation of specimen]
As shown in FIG. 1 (A), a test body 1 such as a building material or a construction material is cut to a predetermined size, and the test body 1 is made of a metal foil 2 such as an aluminum foil or a copper foil that is larger than this. The test piece 1 is completely surrounded by folding the metal foil 2 on the upper surface. At this time, it is desirable that the side of the test body 1 without the folded portion of the metal foil 2 be the surface. In the example of FIG. 1, when the test body 1 is placed on the metal foil 2, it is desirable that the contact surface side with respect to the metal foil 2 be the surface.

  When the specimen 1 is completely surrounded by the metal foil 2, as shown in FIG. 1 (B), the metal foil 2 is cut to a predetermined size with a cutter on the surface side of the specimen, and the surface side is exposed. . As the metal foil 2, a general aluminum foil as a kitchen utensil can be suitably used. There are various thicknesses of aluminum foil depending on the application, but it is preferable to use a thickness of about 15 to 100 μm for heat treatment.

[Measurement equipment for pollutant emissions]
As shown in FIG. 2, in order from the air supply side, a clean air supply unit 3, an activated carbon tank 4, a humidity control unit 5, a static mixer 6, a primary collection pipe 7 for volatilization, a secondary collection pipe 8, An integrated flow meter 9 is provided continuously.

  The air (28 ± 1 ° C.) sent as the carrier gas from the clean air supply unit 3 passes through the activated carbon tank 4 to remove fine dust and the like, and then the humidity adjustment unit 5 makes 50 ± 5%. After being adjusted to the RH humidity state, the air is uniformly mixed by passing through the static mixer 6 and supplied to the primary collection tube 7 for volatilization.

  The primary collection tube 7 is a tubular body made of quartz glass called a Tenax tube, and the test body 1 is inserted into the tube. This primary collection tube 7 is used for the purpose of dissipating gas from the accommodated test body 1 and collecting semi-volatile organic compounds (SVOC) adhering to the inner wall surface of the tube. As shown in FIG. 3, the primary collection tube 7 (Tenax tube) can be set as it is in the heat desorption section 11 of the thermal desorption type gas chromatograph mass spectrometer 12 (GC / MS). Semi-volatile organic compounds (SVOC) adhering to the inner wall of the collecting tube 7 (Tenax tube) can be qualitatively and quantitatively determined. Since the primary collection tube 7 (Tenax tube) has an inner diameter of 12 mm, the test body 1 is produced in a size that can be inserted.

  Similarly, the secondary collection tube 8 is a tubular body made of quartz glass called a Tenax tube and is filled with a collection agent 10. The scavenger 10 is a heat-resistant resin having a 2,6-diphenyl-p-phenylene oxide structure called “TenaxTA”, or a mixture called “TenaxGR” in which “TenaxTA” is impregnated with 23% graphite carbon. A scavenger or the like can be used. The collection tubes filled with these “TenaxTA” and “TenaxGR” are easily available. In the secondary collection tube 8, the supervolatile organic compound (VVOC) and the volatile organic compound (VOC) are collected by the collection agent 10 among the volatile organic compounds released from the specimen. This secondary collection tube 8 (Tenax tube) can also be set as it is in the heat desorption section 11 of the thermal desorption type gas chromatograph mass spectrometer 12 (GC / MS), as shown in FIG. The volatile organic compound (VVOC) and the volatile organic compound (VOC) adsorbed on the collection agent 10 of the next collection tube 8 (Tenax tube) can be qualitatively and quantitatively determined.

  In the above measuring apparatus, in a state where the test body 1 is inserted into the primary collection tube 7, a carrier gas of a predetermined temperature is supplied at a predetermined flow rate and a predetermined time, and the volatile organic compound released from the test body 1 is supplied. After being collected by the primary collection tube 7 and the secondary collection tube 8, as described above, these two collection tubes 7 and 8 are respectively connected to the thermal desorption type gas chromatograph as shown in FIG. It is set in the heat desorption part 11 of the mass spectrometer 12 (GC / MS), and the total emission amount of the volatile organic compound is analyzed.

(1) Preparation of the test specimen Cut from the center of the vinyl floor sheet roll to a size of 11.5mm x 52mm, completely enclosed with aluminum foil, and then cut off the aluminum foil on the surface with dimensions of 10mm x 50mm. An exposed specimen was prepared. For comparison, a specimen not covered with aluminum foil was also prepared.

(2) Measurement conditions Using the measuring apparatus shown in FIG. 2, the amount of volatile organic compounds emitted was measured under the conditions shown in Table 1 below.

(3) Analytical conditions After circulating the carrier gas for a predetermined time, the primary collection tube 7 and the secondary collection tube 8 were subjected to thermal desorption gas chromatograph mass spectrometry (GC / MS) as shown in Tables 2 and 3 below. Analyzed by condition.

(4) Analysis results Table 4 below shows the analysis results of the specimens coated with aluminum and those without coating. The blank is an analytical value that is inevitably generated in a state where the collection tube is not set.

It is a figure which shows the preparation points of the test body 1 which concerns on this invention. It is a figure which shows the measuring apparatus of pollutant emission amount. It is a figure which shows the analysis point of the volatile organic compound by the primary collection tube 7 and the secondary collection tube 8. FIG. It is a figure which shows the measuring method of the pollutant emission amount of the conventional method 1. FIG. It is a figure which shows the measuring method of the pollutant emission amount of the conventional method 2. FIG. 3A is an exploded perspective view showing a seal box, and FIG.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1 ... Test body, 2 ... Metal foil, 3 ... Clean air supply unit, 4 ... Activated carbon tank, 5 ... Humidity control unit, 6 ... Static mixer, 7 ... Primary collection pipe, 8 ... Secondary collection pipe, 9 ... Integral flow meter, 10 ... collecting agent, 11 ... heat desorption part, 12 ... thermal desorption type gas chromatograph mass spectrometer

Claims (1)

Connect the two collection tubes with a connector, and completely surround the test specimen with aluminum foil or copper foil in the upstream collection pipe. Then, cut the metal foil on the test specimen surface side to the specified size. A test tube made by exposing only the sample to a volatilized primary collection tube, filling the downstream collection tube with a collection agent to form a secondary collection tube, and a carrier at a predetermined temperature. Gas is supplied at a predetermined flow rate and for a predetermined time, and volatile organic compounds released from the specimen are collected by the primary collection tube and the secondary collection tube, and then the two collection tubes are heated. A method for measuring the amount of pollutant emission, which is set in a heat desorption part of a desorption type gas chromatograph mass spectrometer (GC / MS) and calculates the total emission amount of volatile organic compounds.

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