JPH08201249A - Odor measuring instrument - Google Patents

Abstract

PURPOSE: To obtain an odor measuring instrument for effectively analyze an odor generated in a container by means of a mass spectrometer, etc. CONSTITUTION: An odor measuring instrument is provided with a container 20, sample stage 7 which is provided in the container 20 and on which a sample 11 is set, temperature controlling means equipped with a ceramic heater 10 which is connected to the stage 7 and generates an odor from the sample 11 by heating the sample 11, sampling pipe 31 which is used for sampling the odor and equipped with a heater 32, and analyzer 30 which analyzes the odor introduced from the pipe 31. Therefore, the odor generated in the container 20 can be analyzed with an external analyzer, because the odor can be introduced to the analyzer 30 without allowing the pipe 31 to adsorb the odor.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for measuring odor generated when heating various substances (hereinafter referred to as samples).

[0002]

2. Description of the Related Art For example, there is an odor measuring device as disclosed in Japanese Patent Application Laid-Open No. 3-235047. The operation of the device disclosed in that publication will be briefly described below. When the sample is placed on the heater in the container and the start button of the control device is pressed, the control device starts the intake fan and starts ventilation, When the data of the temperature controller, the odor sensor, etc. are read into the control device and the test becomes possible, the heating of the heater is started. As a result, it is possible to measure the output of the odor sensor at predetermined time intervals.

[0003]

The odor generated in the container of the odor measuring device can be easily output if the detection unit such as the odor sensor can be installed in the container. In order to use an analyzer such as an analyzer, it is necessary to guide the odor in the container to the analyzer. Then, when the odorous substance having a large molecular weight is guided to the analyzer by using the sampling tube, it may be adsorbed in the sampling tube until it reaches the analyzer.

An object of the present invention is to obtain an odor measuring device for effectively analyzing the odor generated in a container by a mass spectrometer or the like.

[0005]

SUMMARY OF THE INVENTION The present invention is directed to a container, a sample table on which a sample is placed in the container, and a temperature which is connected to the sample table and controls heating to generate odor from the sample to be placed. It is characterized by having a control means, a sampling pipe with a heater for sampling odor from a container, and an analyzer for analyzing odor introduced from the sampling pipe. Further, the container is provided with a supply means capable of introducing a specific gas from the outside and can be hermetically sealed, and the temperature control means uses a heater for heating the sample to measure the temperature of the sample. The heating of the sampling tube with a heater can be turned on and off, and the heating of the sampling tube with a heater can be turned on and off. The apparatus is one or a combination of a mass spectrometer, a gas chromatograph, an infrared spectrophotometer, an ultraviolet spectrophotometer, an X-ray analyzer and an electron beam analyzer.

[0006]

[Function] By heating the sample placed on the sample table and guiding the odor generated in the container to the external analyzer with the sampling tube with the heater, the odor in the container is analyzed without being adsorbed by the sampling tube. It can be guided to the device and the odor generated can be analyzed by an external device.

Further, the container is provided with a supply means capable of introducing a specific gas from the outside and can be hermetically sealed, so that the atmosphere can be adjusted when the sample is heated. It is possible. The temperature control means
The heater for heating the sample is used to perform linear rising heating or constant temperature heating, and the heating method of the sample can be controlled. The heater of the sampling tube with a heater can be turned on and off, and unnecessary heating is not performed when there is no fear of odor adsorption. Further, the analyzer is one of a mass spectrometer, a gas chromatograph, an infrared spectrophotometer, an ultraviolet spectrophotometer, an X-ray analyzer and an electron beam analyzer, or a combination thereof, and these The device can be used to qualify, quantify, and identify odors.

[0008]

The structure of one embodiment of the present invention will be described below.

FIG. 1 is a schematic diagram showing the odor measuring device of the present invention. In the figure, 20 is a sealable container, which is composed of a container body 21 and a lid 22 thereof. An inlet pipe 23 for introducing a specific gas such as dry air is provided inside the side surface of the container body 21. A sample table 7 is provided on the inner wall of the container body 21, a ceramic heater 10 is placed on the sample table 7, and a sample 11, for example, cellulose powder, cotton or filter paper is placed on the ceramic heater 10. Adjacent to the thermocouple 1
2 is placed. The ceramic heater 10 and the thermocouple 12 are connected to the temperature controller 13.

Reference numeral 30 denotes an analyzer in which the odor in the container 20 is introduced through a sampling tube 31, which can identify and quantify the odor substance. As the analyzer 30, a mass spectrometer, a gas chromatograph, an infrared spectrophotometer, an ultraviolet spectrophotometer, an X-ray analyzer, an electron beam analyzer and the like can be used.
The mass spectrometer can separate the odorants by their molecular weights, and can perform the molecular weights of the odorants and their quantification. The gas chromatograph device can separate odorants based on their mobility, and can perform quantification for each odorant. Other spectrophotometers and the like can detect the absorption of infrared wavelengths based on the molecular shape of the odorant, and identify or quantify the odorant.

A sampling tube 31 for this analyzer 30
Is provided with a coiled heater 32 for heating the entire inner wall thereof. Even if the odorant has a relatively high molecular weight, it is possible to prevent the odorant from adsorbing to the inner wall of the sampling tube 31 and to reliably introduce the odor in the container 20 into the analyzer 30. Similarly, although not shown in detail,
The inner wall of the container 20 is also preferably heatable, and the shape of the heater is the same as that of the sampling tube 31 as long as each part can be uniformly heated. And regarding the heating temperature,
Although it depends on the odorant, it is preferably about 60 to 150 ° C., and if it is heated too much, the odorant may be thermally decomposed.

On the inner wall of the container body 21 facing the sample table 7, a fan 24 that can be turned on and off is provided as a stirring means. Furthermore, an odor sensor 14 as a detection means is arranged in the container body 21. The odor sensor 14 detects the presence of odor by, for example, a odor sensor having stannic oxide as a main material.
Although it is not possible to discriminate the detailed odor substance, it is possible to detect the presence or absence of the odor and its strength. Then, from the output of the odor sensor 14 and the analysis result of the analysis device 30, it is possible to relatively examine the relationship between the amount and property of the odor substance and the odor intensity.

The temperature controller 13 to which the ceramic heater 10 and the thermocouple 12 are connected is the thermocouple 12
The heating of the heater 10 is controlled based on the output of 1) and is connected to a control device (not shown) together with the odor sensor 14.

The operation of this odor measuring device will be briefly described. First, the lid 22 is opened, the sample 11 is placed on the ceramic heater 10 of the sample table 7, the lid 22 is closed, and the container 2 is closed.
After setting the inside of 0 to a predetermined atmosphere, the controller outputs a start signal to the temperature controller, the ceramic heater 10 heats the sample 11, and the odor peculiar to the sample 11 is generated. By rotating the fan 24 with the start of heating, the generated odor can be made uniform in the container 20.

The atmosphere in the container 20 can be adjusted by introducing, for example, dry air or nitrogen gas supplied from a cylinder (not shown) through the introduction pipe 23, and in order to adjust environmental conditions such as humidity. Can also be used. It is also possible to supply the atmosphere sequentially from the introduction pipe 23.

The heating method of the sample 11 is controlled by the temperature controller 13 based on the setting in the controller,
The temperature of the sample 11 is detected by the thermocouple 12, and the heating condition by the heater is adjusted. This heating method can perform linear rising heating that raises the temperature at a constant rate, such as 5 ° C. per minute, or low temperature heating that maintains a predetermined temperature, such as 200 ° C. It is possible to set the heating method for a certain period of time. These heating methods and atmospheres are configured so that various settings can be made when investigating the generation process of odor from the sample 11.

Further, the measurement of the analyzer 30 may be started manually, but may be automatically measured by the controller.

Next, a simple structure of the mass spectrometer as an analyzer is shown in FIG. 2, but it basically comprises an ionization section 14, a mass separation section 15, and an ion detection section 16.

The odor drawn by the two-stage oil rotary pump 48 and drawn from the sampling tube 31 is introduced from the capillary 42 through the filter 43 into the apparatus of about 10 ^-6 torr, and first, the ionization section by the EI ion source. 44
Are ionized by the electric field due to the high voltage. The ionized odor is separated by the molecular weight of the component in the odor flow by the magnetic field of 45 of the mass separation section by the quadrupole,
The separated components reach the ion detector 46 by the electron multiplier, and the odor caused by combustion is separated and detected for each molecular weight. Then, for example, when benzene is produced, a peak appears at the position of ionic strength 78 (m / e = 78), at the position of 50 (m / e = 50) for butadiene and at the position of 92 (m / e) for toluene. A peak appears at the position of e = 92).

Filter 43 from this capillary 42
Is provided in order to reduce the pressure in the apparatus from atmospheric pressure to a reduced pressure state by the turbo pump 47, but there is an influence that large molecules in the component are adsorbed by the filter 43. Considering the formation process of soot, it is considered that high molecular weight odors such as xylene, naphthalene, and anthracene are generated. Therefore, when measuring even large molecules, this filter 4
A plate or skimmer having holes (for example, about 1 μm) without 3 is provided with a through hole at the top of a cone, and stacking a plurality of them has the effect of repelling and concentrating light molecules such as nitrogen and oxygen. ) Or the like may be used. Further, the ionization section 44 may be an ion source using a radioactive element other than the EI ion source, and the mass separation section 45.
May be a magnetic source other than the quadrupole, and may use the TOF method.

As an analyzer other than the mass spectrometer, an infrared spectrophotometer having a simple structure is shown in FIG. 3, but basically, the infrared light source 56, the measuring cell 55, and the spectroscope 6 are used.
0, an infrared detector 52.

The air flow sent from the sampling pipe 31 to the measuring cell 55 via the inlet 53 continuing from the sampling pipe 31 is exhausted from the exhaust port 54.
It is exhausted from, and a new air flow is always taken in. On the other hand, the compensation cell 57 communicates with the measurement cell 55, but since the shielding plates 61 and 62 are provided, the compensation cell 57 is provided.
The atmosphere inside the container 20 can be left as it is in the initial state. It is preferable that the shield plates 61 and 62 be removed during the preparation for measurement and mounted in a state where the atmosphere in the container 20 starts the measurement. And these shield plates 6
A small through hole may be provided in each of the parts 1 and 62 so as to follow a slight change in the atmosphere, or may not be provided.

Light from an infrared light source 56 capable of emitting light in the infrared wavelength band is applied to the measuring cell 55 and the compensating cell 57 by the separator 51. The two lights that have passed through the measurement cell 55 and the compensation cell 57 are alternately shielded by the sector part 58, are separated into respective wavelengths by the spectroscope 60, and are condensed on the infrared detection part 52. In the spectroscope 60, although not shown in detail, the light from the sector section 58 passing through the slit for introduction is split by a prism and emitted toward the infrared detecting section 52 for each wavelength through the slit for emission. To be done. A silicon carbide rod, a Nernst lamp, or the like is used for the light source 56, and a thermocouple, a bolometer, or the like is used for the infrared detection unit 52.

Then, the measurement cell 55 and the compensation cell 57
The absorption due to the odor of each wavelength is measured from the intensity difference of the passing light of. Here, the odor in the container 20 is introduced into the measurement cell 55, but the atmosphere in the initial state of the container 20 remains in the compensation cell 57, and the intensity difference of each wavelength of the passing light is odor. It represents the characteristics of the molecular structure of a substance. For example, when benzene is produced, the absorption due to the = CH stretching vibration of the aromatic ring is around 3000 cm ^-1 , and
200 peculiar small wave absorption based on C-H out-of-plane bending vibration
At ⁰ to 1660 cm ⁻¹ , strong absorption due to ring vibration including C═C stretching vibration of aromatic ring is at 1600 to 1450 cm ⁻¹ , and slightly strong absorption due to ═C—H in-plane bending vibration of aromatic ring is 1.
The 250~1000cm ^-1, strong absorption based on = C-H out-of-plane deformation vibration of aromatic rings in 1000~650cm ^-1, infrared absorption spectrum having a large number of specific absorption bands are obtained.

In addition to the mass spectrometer and infrared spectrophotometer as described above, a gas chromatograph, an ultraviolet spectrophotometer, an X-ray analyzer or an electron beam analyzer can be used as an analyzer. , A combination thereof, for example, GC-MS separated by a gas chromatograph and introduced into a mass spectrometer, G separated by a gas chromatograph and introduced into an infrared spectrophotometer.
It may be C-IR, UV-IR or the like that simultaneously performs an infrared spectrophotometer and an ultraviolet spectrophotometer, and by using these instruments, it is possible to qualitatively, quantitatively, and identify odors in a multifaceted manner. is there.

[0026]

INDUSTRIAL APPLICABILITY As described above, according to the present invention, a container, a sample base for mounting a sample in the container, and a sample base connected to the sample base to control heating, generate odor from the mounted sample. Since the temperature control means, the sampling tube with the heater for sampling the odor from the container, and the analyzer for analyzing the odor introduced from the sampling tube are included, the odor in the container is adsorbed to the sampling tube. Can lead to the analyzer without
The generated odor can be analyzed by an external device.

Further, the container is provided with a supply means capable of introducing a specific gas from the outside and can be hermetically sealed, and the atmosphere can be adjusted when the sample is heated. It is possible. The temperature control means
The heater that heats the sample performs linear rising heating that raises the temperature of the sample constant, or the constant temperature heating that keeps the sample at a constant temperature by the heater that heats the sample, and the heating method of the sample can be controlled. . The heater of the sampling tube with a heater can be turned on and off, and unnecessary heating is not performed when there is no fear of odor adsorption. Further, the analyzer is one of a mass spectrometer, a gas chromatograph, an infrared spectrophotometer, an ultraviolet spectrophotometer, an X-ray analyzer and an electron beam analyzer, or a combination thereof, and these It is possible to qualitatively, quantitatively, and identify odors from various aspects by using the device.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram showing an embodiment of the present invention.

FIG. 2 is a block diagram of the mass spectrometer used in FIG.

FIG. 3 is a configuration diagram of an infrared spectrophotometer used in FIG.

[Explanation of symbols]

 7 sample stage 10 ceramic heater 11 sample 20 container 30 analyzer 31 sampling tube 32 heater

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁶ Identification code Internal reference number FI technical display location G01N 27/62 V 30/88 Z

Claims (7)

[Claims] 1. A container, a sample table for mounting a sample provided in the container, temperature control means connected to the sample table to generate odor from the mounted sample by heating control, and odor from the container. An odor measuring device, comprising: a sampling tube with a heater for sampling the odor; and an analyzer for analyzing the odor introduced from the sampling tube. 2. The odor measuring device according to claim 1, wherein the container is provided with a supply means capable of introducing a specific gas from the outside. 3. The odor measuring device according to claim 1, wherein the container can be sealed. 4. The odor measuring device according to claim 1, wherein the temperature control means performs linear ascending heating in which the sample is constantly heated by a heater for heating the sample. 5. The odor measuring device according to claim 1, wherein the temperature control means performs constant temperature heating for maintaining the sample at a constant temperature by a heater for heating the sample. 6. The odor measuring device according to claim 1, wherein the heater of the sampling tube with the heater can be turned on and off. 7. The analyzer comprises a mass spectrometer, a gas chromatograph, an infrared spectrophotometer, an ultraviolet spectrophotometer,
The odor measuring device according to claim 1, which is one of an X-ray analyzing device and an electron beam analyzing device or a combination thereof.