JP2015137961A - head space gas collecting container - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a head space gas collecting container and a quick collecting method for analyzing a solid material inside a sealed container and VOC (volatile organic compound) generated from a liquid material.SOLUTION: A sealed container collects VOC (volatile organic compound) generated from a solid material or a liquid material. A sealed container main body a has a cylindrical shape with an opening e, and the center of the opening e has a flange type bearing and a cylindrical propeller shaft shaped rotation axis f which penetrates the flange type bearing. The end part of the propeller shaft shaped rotation axis has at least two or more blades c on the side of the sealed container main body. The sealed container is a head space gas collection container having a VOC collecting body containing a cassette b connected to the blade part.

Description

  The present invention relates to a headspace gas collection container for analyzing VOC (volatile organic compound) generated from a solid or liquid in a sealed container, and a collection method using the same.

  When collecting and analyzing VOCs generated from solids or liquids in a sealed container, the head is vapor phase equilibrated by setting an arbitrary temperature and time in order to expel VOCs from the solids and liquids in the sealed container. GC (gas chromatograph), GC / MS (gas chromatograph / mass spectrometer), etc., by collecting the space part with a gas tight syringe and by collecting the trapped body in a sealed container head space part. There is a method of analyzing by introducing into an analyzer.

  In general, flavor and off-flavor components generated from foods and beverages often contribute to the odor of components that have low detection sensitivity (low odor threshold) and are collected from these samples. Even if VOC is directly analyzed by GC or GC / MS, only a part of the odor component generated from the sample is collected, and it does not reflect the sensual and felt odor, but achieves its original purpose. I can't.

  As a conventional method, as a method for collecting and analyzing VOCs generated from solids and liquids, the solids are put in a vial and sealed, and the vial is heated and equilibrated with the headspace gas in the container as a gas. After collecting with a tight syringe, it analyzes by GC / MS (nonpatent literature 1). Moreover, after collecting head space gas in a collector with a gas concentration syringe, a method of analyzing by P & T (purge and trap) -GC / MS (Patent Document 1) is shown.

JP 2008-275367 A

“3-1-2-1-2 Headspace-GC-MS”, 2005 Japan Patent Office Standard Technology Collection Mass Spectrometry, pages 224-225

  However, the above-described collection method described in Non-Patent Document 1 is intended to analyze the collection of headspace gas that has been heat-balanced, and when food or beverage samples that are often subjected to sensory evaluation at room temperature are used as samples. Therefore, it seems that it is difficult to detect a component present in a trace amount by this collection method that does not heat the headspace gas.

  In addition, the collection method described in Patent Document 1 is intended to collect the headspace gas in which the sample is in gas phase equilibrium, and the sample is a food or beverage often subjected to sensory evaluation at room temperature. In such a case, it takes about 3 to 24 hours for the headspace gas to reach a vapor phase equilibrium at room temperature, and it seems that rapid analysis is difficult.

  The present invention has been made to solve the above-mentioned problems, and the invention according to claim 1 is a sealed container that collects VOC (volatile organic compound) generated from a solid or liquid material. The sealed container body has a cylindrical shape having an opening, and has a flange-type bearing and a cylindrical propeller shaft-shaped rotation shaft passing through the flange-type bearing at the center of the opening, The propeller shaft-shaped end of the rotating shaft has at least two or more blades on the sealed container main body side, and further has a VOC collection inclusion cassette connected to the blade portion. A gas collection container.

  The invention according to claim 2 is characterized in that the blade is rotated in order to uniformly diffuse VOC generated from solid or liquid material in the sealed container. It is a collection container.

  According to a third aspect of the present invention, a motor is connected to the other end of the propeller shaft-shaped rotating shaft having the blade, and the blade is rotated at a constant output. The headspace gas collection container according to any one of the above.

  According to a fourth aspect of the present invention, the VOC collector has a structure in which polydimethylsiloxane is applied to the outside of a glass stirrer that encloses a magnet, or a cylindrical shape having a monolithic structure of a silica skeleton. The head space gas collecting container according to claim 1.

  The invention according to claim 5 uses the headspace gas collection container according to any one of claims 1 to 4 to collect VOC generated from solid matter or liquid matter in the container. The headspace gas collection method characterized by the above.

  The headspace gas collection container of the present invention makes it possible to reliably and easily collect and analyze VOCs generated from solids or liquids placed in a sealed container.

It is the schematic of the container for head space gas collection of this invention. It is the front view and sectional drawing of the bb part of the head space gas collection container of this invention. It is TIC (total ion chromatogram) of GC / MS which showed the Example and the comparative example.

  An embodiment of the present invention will be described in detail with reference to FIGS.

FIG. 1 is a schematic view of a headspace gas collecting container according to the present invention.
The container body (a) has a cylindrical shape with a thick wall from the opening (e) to a predetermined depth, and has a propeller shaft-shaped rotating shaft (f) passing through the center of the opening (e). It is fixed by a flange type bearing (d). Further, the container body (a) has three blades (c) that can be combined with the propeller shaft-shaped rotation shaft (f), and the propeller shaft-shaped rotation shaft on one opening (e) side. (F) has a shape that can be connected to a motor, and has a cassette (b) with a hook that can contain a collector at the tip of the blade (c).

FIG. 2 is a front view and a cross-sectional view of b to f of the present invention.
The cassette (b) body has a mesh shape, the upper part has a hook, the bottom part has an openable / closable stopper that can store the collector, and the collector can be easily set by connecting to the tip of the rotating blade. Is a possible structure. The tip of the blade (c) has a hook, the end has a structure that can be connected to the rotating shaft with a female screw, and the blade has a structure of three. The flange-type bearing (d) has a structure in which a bearing is combined with the center hole of the opening (e) so that the flange (d) can be fixed to the opening (d). The propeller shaft-shaped rotating shaft (f) has a structure in which the blade (c) is fixed to one propeller shaft portion, and the other propeller shaft portion has a shaft that is rotated by a motor.
As a result, the collected body was stored in the cassette (b), the sample was simultaneously placed in the container body (a), the opening (e) was closed, and then connected to the propeller shaft-shaped rotating shaft (f) by a motor. By rotating the blade (c) at a constant output, VOC generated from the sample can be collected in the collector so that quantitative evaluation can be performed.

  The main body (a) of the headspace gas collection container of the present invention is an improved glass storage container for food, and the material of the headspace gas collection container main body (a) is most preferably made of glass. The container bottom shape is preferably a cylindrical shape that can be stably placed on a laboratory table. Furthermore, it is desirable that the container opening has a structure that can completely block the inside and outside of the container, that is, has high airtightness.

  The cassette (b) of the headspace gas collection container of the present invention has a hook attached to the tip, the main body has a mesh-like cylindrical shape, and the bottom has a lid that can store the collection body. desirable. The material of the cassette is preferably made of stainless steel or Teflon (registered trademark).

  The blade (c) of the head space gas collection container of the present invention is preferably at least two blades, and has a cylindrical shape that can be connected to a propeller shaft-shaped rotating shaft and has a female screw portion. The material is preferably made of stainless steel or Teflon (registered trademark).

  The flange-type bearing of the headspace gas collection container of the present invention has a structure that is fixed with a nut, a screw, or the like that sandwiches the opening (e), and there is a gap between the bearing and the opening (e). It is desirable that the bearing contact surface has no gap with the propeller shaft.

  The opening (e) of the headspace gas collection container of the present invention has a structure that can be fitted to the container body (a), and a structure in which a flange-type bearing can be fixed at the center of the opening (e). Is most preferably made of glass.

  The propeller shaft-shaped rotating shaft (f) of the head space gas collection container of the present invention has a shaft at both ends, a structure in which one side can be connected to a blade and the other side to a motor. Most preferred is Teflon (registered trademark).

  Hereinafter, the method for extracting VOC and hardly volatile components from solids using the headspace gas collection container of the present invention will be described in more detail with specific examples. The scope is not limited to these examples.

<Example>
Using the headspace gas collection container of the present invention, VOCs from bad breath prevention tablets were collected according to the following procedure.
A PDMS (polydimethylsiloxane) type collector is fixed in a cassette in a 900 ml headspace gas collection container in advance, and then a sample tablet (for 50 tablets) and an internal standard reagent (methyl myristate 0 0.1 μg) and the container was sealed. Here, the PDMS type collector has a structure or silica skeleton in which polydimethylsiloxane (PDMS) is coated on the outside of a glass stirrer that encloses a magnet for the purpose of adsorbing VOC in a sealed container. A cylindrical shape having a monolith structure.

  A motor shaft is incorporated into a propeller shaft-shaped rotating shaft that is outside the opening, connected to a motor with an output of 10 W, operated for 15 minutes at room temperature, and the air flow in the headspace gas collection container is stirred to generate from the sample. VOCs were collected in a PDMS type collector.

  Take out the PDMS type collector from which VOC was collected from the headspace gas collection container, set the PDMS type collector in the dedicated glass tube in the purge and trap unit (TDU) made by GERSTEL, and then remove it by heating. The analysis was performed by GC / MS (GC7890 / 5975MSD) manufactured by Agilent Technologies.

<Comparative example>
Using the glass container for food preservation, VOC from the bad breath prevention tablet was collected according to the following procedure.
A PDMS (polydimethylsiloxane) type collector is fixed in advance in the headspace of a 900 ml food storage glass container, and a sample tablet (for 50 tablets) and an internal standard reagent (methyl myristate 0.1 μg) The glass container for food preservation was sealed.

VOC generated from the sample was collected in a PDMS type collector for 24 hours at room temperature.
Take out the PDMS type collector that has collected VOC from the glass container for food preservation, set the PDMS type collector in the dedicated glass tube in the purge and trap unit (TDU) made by GERSTEL, then perform heat desorption, Analysis was performed with GC / MS (GC7890 / 5975MSD) manufactured by Agilent Technologies.

<Analysis results>
As shown in FIG. 3, in the results of the comparison between the example and the comparative example, the peak area value of limonene, menthol, terpineol, which are characteristic components of the sample, and the internal standard substance added in the same amount (0.1 μg) to the sample. Were almost equivalent.
From this, it is judged that VOC generated from solid matter or liquid matter is reliably and easily collected by using the headspace gas collection container of the present invention, and the reliability of quantitative evaluation is ensured and Collection time can be greatly reduced.

a ... container body b ... cassette c ... blade d ... flange-type bearing e ... opening f ... rotating shaft of propeller shaft shape

Claims (5)

  A sealed container for collecting VOC (volatile organic compound) generated from a solid or liquid substance, wherein the sealed container body has a cylindrical shape having an opening, and a flange-type bearing and the A cylindrical propeller shaft-shaped rotary shaft penetrating the flange-type bearing, and an end of the propeller shaft-shaped rotary shaft has at least two blades on the sealed container body side; Furthermore, the container for head space gas collection which has a VOC collection body inclusion cassette connected to the said blade part.   2. The headspace gas collection container according to claim 1, wherein the blade is rotated in order to uniformly diffuse VOC generated from a solid substance or a liquid substance in the sealed container.   3. The headspace gas trap according to claim 1, wherein a motor is connected to the other end of the propeller shaft-shaped rotary shaft having the blade to rotate the blade at a constant output. Collection container.   The said VOC collector is the column shape which has the structure which apply | coated polydimethylsiloxane to the outer side of the glass stirring element which includes a magnet, or the monolith structure of the silica frame | skeleton. A container for collecting headspace gas as described.   5. A headspace gas collection device using the headspace gas collection vessel according to claim 1 to collect VOCs generated from solids and liquids in the vessel. Method.

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