JP2008101930A - Qualitative analyzing method of inorganic fibrous substance and qualitative analyzing system - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a qualitative analyzing method for rapidly, simply and accurately discriminating the presence of an inorganic fibrous substance being a target in a sample, and a qualitative analyzing system. <P>SOLUTION: This qualitative analyzing method ST includes at least an organic fiber ashing process for ashing a sample Ay to obtain an ashed sample A wherein an organic fiber (y) is ashed, a Fourier transform infrared spectroscopic analyzing process st2 for measuring the ashed sample A by a Fourier transform infrared spectroscopic apparatus 2 to obtain Fourier transform infrared spectrum sp of the ashed sample A and an inorganic fiber detection process st3 which enables the detection of predetermined asbestos (a) from the Fourier transform infrared spectrum sp obtained by the Fourier transform infrared spectroscopic analyzing process st2. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a method for qualitative analysis of inorganic fibrous materials, and mainly relates to a method for qualitative analysis of inorganic fibrous materials contained in products such as air and products such as calcium silicate plates, heat insulating materials, slate plates, and spray materials. Is.

  Conventionally, inorganic fibrous materials such as asbestos have excellent properties such as durability, heat resistance, chemical resistance, and electrical insulation, and are inexpensive, so calcium silicate plates, heat insulating materials, slate plates, fireproof coatings and sound absorption It has been widely used in various applications such as spraying materials for heat insulation, wear materials, brake linings, packings and the like.

  Here, especially in the case of asbestos, the effects on the human body are often discussed, and in Japan recently the use of asbestos has been banned. In addition, measures to prevent the asbestos-containing material already used from scattering and measures to prevent the asbestos from scattering when the building is removed are necessary, and a method that can quickly and easily determine the presence or absence of asbestos is required. ing.

Under such circumstances, for example, a method for determining the presence or absence of asbestos by performing color-specific observation using a phase contrast microscope or a polarizing microscope (see, for example, Patent Document 1 and Patent Document 2), X-ray A method for determining the presence or absence of asbestos by specifying the asbestos crystal structure by diffraction has been proposed.
JP-A-7-181268 JP-A-9-127102

  However, in these methods, since the operation of the microscope and the X-ray diffraction apparatus is complicated and skill is required, for example, the method described in the above-mentioned patent document requires about 7 to 8 hours per sample. It has become. In addition, in such a method using a microscope, it is conceivable that the organic fiber contained in the sample is confused with the inorganic fibrous substance to be detected. Furthermore, in the analysis method by X-ray diffraction, for example, when the amount of the sample is very small, it cannot be detected, and for example, an inorganic fibrous substance to be detected and a non-fibrous substance having the same mineral composition are included. When it exists, there exists a possibility of detecting the said non-fibrous substance accidentally.

  The present invention pays attention to such problems, and provides a method and system for quickly, simply and accurately determining the presence or absence of a target inorganic fibrous substance in a sample.

  In order to achieve such an object, the present invention takes the following measures. That is, the method for qualitative analysis of an inorganic fibrous substance according to the present invention includes an organic fiber ashing step for obtaining an ashed sample obtained by ashing a sample by ashing the sample, and Fourier transform infrared for the ashed sample. A Fourier transform infrared spectroscopic analysis step for obtaining a Fourier transform infrared spectroscopic spectrum of the ashed sample measured by a spectroscopic device, and a predetermined inorganic fiber from the Fourier transform infrared spectroscopic spectrum obtained by the Fourier transform infrared spectroscopic analysis step And an inorganic fiber detecting step capable of detecting a particulate substance.

  Further, the qualitative analysis system for inorganic fibrous materials according to the present invention includes an organic fiber ashing device for obtaining an ashed sample obtained by ashing an organic fiber by ashing the sample, and Fourier transform infrared spectroscopy of the ashed sample. It comprises at least a Fourier transform infrared spectroscopic device capable of detecting a predetermined inorganic fibrous substance from a Fourier transform infrared spectroscopic spectrum of the ashed sample obtained by performing the analysis. .

  If it is such, when the organic fiber is contained in the sample, the organic fiber in the sample can be ashed to form an ashed sample, so the organic fiber and the predetermined inorganic fiber It is possible to effectively avoid the problem of erroneously identifying and detecting the particulate matter. Furthermore, it is possible to perform rapid processing by performing Fourier transform infrared spectroscopy, and according to the Fourier transform infrared spectroscopy, inorganic fibrous materials and non-fibrous materials having the same mineral composition, such as chrysotile (White asbestos) and antigolite (non-asbestos) can be accurately discriminated.

  In order to effectively avoid the problem that a predetermined inorganic fibrous material is decomposed or altered by the organic fiber ashing process, by using a low-temperature ashing device, the organic fiber ashing process is heated by, for example, chrysotile. It is desirable to use a low-temperature ashing step in which the sample is incinerated at a temperature of 450 ° C. or lower, which is the temperature at which decomposition begins. Furthermore, in order to effectively suppress the amount of energy required for such ashing, it is more preferable to ash the sample at a temperature of 200 ° C.

  And if the Fourier transform infrared spectroscopic analysis process is a microscopic Fourier transform infrared spectroscopic analysis process using a microscopic Fourier transform infrared spectroscopic device, not only the above-mentioned chrysotile but also other kinds of inorganic fibrous substances are single. Even when it is contained in the sample, it is possible to suitably detect each fiber, and to discriminate each, that is, to suitably perform qualitative analysis.

  In particular, as an application in which the present invention can be effectively used, it is desirable to employ asbestos as a predetermined inorganic fibrous substance.

  In the present invention, it is desirable to effectively use the suspended matter or building material in the atmosphere as a sample for qualitative analysis.

  According to the present invention, when an organic fiber is contained in the sample, the organic fiber in the sample can be incinerated to obtain an ashed sample. Therefore, the organic fiber and the predetermined inorganic fibrous substance can be obtained. Can be effectively avoided. Furthermore, the Fourier transform infrared spectroscopic analysis enables rapid processing, and according to the Fourier transform infrared spectroscopic analysis, the inorganic fibrous material and non-fibrous material having the same mineral blockage can be accurately identified. Can be determined. By doing so, it is possible to perform simple, quick and accurate qualitative analysis of inorganic fibrous materials.

Hereinafter, an embodiment of the present invention will be described with reference to the drawings.

  A qualitative analysis system (hereinafter referred to as an analysis system) S for inorganic fibrous substances according to this embodiment is schematically shown in FIG.

  Such an analysis system S can accurately determine the presence and type of asbestos a, which is an inorganic fibrous substance, from a sample Ay such as a suspended matter or building material in the atmosphere.

  Here, the analysis system S according to the present embodiment includes an organic fiber ashing apparatus 1 that obtains an ashed sample A obtained by ashing the organic fiber y by ashing the sample Ay, and the ashed sample A by Fourier transform infrared. Characterized in that it comprises at least a Fourier transform infrared spectrometer 2 capable of detecting a predetermined asbestos a from the Fourier transform infrared spectroscopic spectrum sp of the ashed sample A obtained by spectroscopic analysis. It is.

  And the qualitative analysis method (hereinafter referred to as the analysis method) ST of the inorganic fibrous substance according to the present invention is an organic fiber ashing step for obtaining an ashed sample A in which the organic fiber y is ashed by ashing the sample Ay. The ashing step st1, the ashing sample A is measured by the Fourier transform infrared spectroscopic device 2 and the Fourier transform infrared spectroscopic analysis step sp2 of the ashing sample A is obtained. It includes at least a detection step st3 which is an inorganic fiber detection step capable of detecting a predetermined asbestos a from the Fourier transform infrared spectroscopic spectrum sp obtained in the step st2. In the present embodiment, the inorganic fibrous substance that can be detected in the embodiment is referred to as “asbestos a” in the following description, but the inorganic fibrous substance according to the present invention is described as such. It is not limited to asbestos a.

  Hereinafter, the analysis system S and the analysis method ST will be described.

  As described above, the analysis system S includes the ashing apparatus 1 capable of ashing the sample Ay, and the ashing sample A ashed by the ashing apparatus 1 with a Fourier transform infrared spectroscopic analysis process (hereinafter referred to as a spectroscopic analysis process). ) A Fourier transform infrared spectroscopic device (hereinafter referred to as an infrared spectroscopic device) 2 capable of detecting a predetermined asbestos a from a Fourier transform infrared spectroscopic spectrum (hereinafter referred to as a spectroscopic spectrum) sp obtained through st2. It is what has.

  As shown in FIG. 1, the ashing apparatus 1 ashes a sample Ay containing an organic fiber y to form an ashed sample A. In other words, the ashing step st1 according to the present invention can be performed. Specifically, the ashing apparatus 1 is included in the sample Ay by performing the low-temperature ashing process according to the present invention in which ashing is performed at 200 ° C., which is a temperature of 450 ° C. or less at which chrysotile cannot be decomposed. The fibrous molecular structure is destroyed by oxidizing or thermally decomposing the organic fiber y. By doing so, the ashed sample A can be in a state where there is no organic fiber y that is mistakenly detected as asbestos a by the analysis step st2 described later. As the ashing device 1, LTA-102 manufactured by Yanako Analytical Industries, Ltd. is adopted.

  The infrared spectroscopic device 2 has an analysis unit 21 that obtains a spectral spectrum sp by analyzing the ashed sample A, and a detection unit 22 that detects asbestos a from the obtained spectral spectrum sp. In other words, the infrared spectroscopic device 2 can perform the analysis step st2 according to the present invention and the detection step st3 which is an inorganic fiber detection step. Specifically, as the infrared spectroscopic device 2, a microscopic Fourier transform infrared spectroscopic device 2 (a device comprising Nicolet 6700 (FT-IR) and Nicolet Centaurus (infrared microscope) manufactured by Thermo Electron Co., Ltd.) is employed. .

  In the analysis step st2, the analysis unit 21 analyzes the ashed sample A to obtain the spectral spectrum sp of each sample Ay as shown in FIG. 2, FIG. 3, FIG. 4, and FIG. In such a spectral spectrum sp, one or more predetermined peaks reflecting the crystal structure of each asbestos a appear.

  In the detection step st3, that is, in the detection step st3, the presence or absence of asbestos a and the position of the peak appearing in the spectral spectrum sp obtained by the analysis step st2 by the analysis unit 21 or the waveform of the spectral spectrum sp including the peak intensity are detected. Asbestos a can be identified.

  Hereinafter, analysis results of detecting asbestos a in the sample Ay by the analysis system S and the analysis method ST will be described with reference to FIGS. 2, 3, 4, and 5. Note that the work time required from the ashing of the sample Ay to the qualitative analysis of asbestos a by the analysis system S is about 20 minutes.

  First, as shown in FIG. 2, in the analysis system S and the analysis method ST, the waveform of the chrysotile (white asbestos) a1 and the anti mineral having the same mineral composition as the chrysotile are obtained due to the difference in the waveform of each spectral spectrum sp. The waveform of the golite b1 can be discriminated.

  Moreover, as shown in FIG. 3, since the microscopic Fourier transform infrared spectroscopic device is adopted as the infrared spectroscopic device 2, it is also an asbestos a in addition to the chrysotile a1, and was used in Japan. Even when samples Ay mixed with crocidolite (Ao Asbestos) a2, amosite (Brown asbestos) a3, anthophyllite a4, tremolite a5 and actinolite a6, which are prohibited to use in Japan, were tested. It can be detected from different waveforms. In other words, qualitative analysis between asbestos a can be suitably performed.

  Then, by using the spectral spectrum sp as shown in FIG. 2 and FIG. 3, as shown in FIG. 4, when an ash-blast furnace heat insulating material as a building material is used as the sample Ay, the chrysotile contained When asbestos string is used for a1 and crocidolite b1, the contained chrysotile a1 can be accurately detected. Further, as shown in FIG. 5, the chrysotile a1 contained in the cement coking material can be accurately detected. In addition, the waveform of the spectral spectrum sp of chrysotile a1, cement and talc is also shown in the same figure, and the waveform of the caulking material is common to the waveform of the chrysotile a1 shown in FIG. 2 in addition to these waveforms. It can be seen that a peak appears.

  And of course, even when these building materials or the building materials are scattered in the air, the asbestos a can be accurately detected and identified even when the suspended matter in the atmosphere is the sample Ay. .

  With the configuration as described above, the analysis method ST according to the present embodiment includes the ashing step st1, the analysis step st2, and the detection step st3, and the qualitative analysis of the asbestos a according to the present invention. Since the system S includes at least the ashing device 1 and the infrared spectroscopic device 2, when the organic fiber y is included in the sample Ay, the organic fiber y in the sample Ay is included. As a result of ashing, the problem that the organic fiber y is erroneously identified and detected as the predetermined asbestos a can be effectively avoided. Further, rapid processing can be performed by performing Fourier transform infrared spectroscopic analysis on the ashed sample A. According to the Fourier transform infrared spectroscopic analysis, chrysotile a1 (white asbestos) and antigolite b1 ( It is possible to accurately discriminate those having the same mineral inhibition (non-asbestos). Specifically, conventionally, it took 7 to 8 hours to analyze one sample Ay, but according to the present embodiment, the time required is about 20 minutes.

  In this embodiment, the ashing step st1 by the ashing device 1 uses the ashing device 1 which is a low-temperature ashing device, whereby a temperature of 450 ° C. or less, which is a temperature at which the chrysotile a1 starts to be thermally decomposed, specifically Is a low-temperature ashing step according to the present invention in which sample Ay is incinerated at a temperature of 200 ° C., so that the amount of energy required for incineration can be effectively suppressed.

  Since the analysis step st2 is the analysis step st2 by the microscopic Fourier transform infrared spectroscopic device 2, not only the above-mentioned chrysotile a1, but also the asbestos a, crocidolite (blue asbestos) a2, amosite (tea asbestos) a3 In addition, even when a building material including anthophyllite a4, tremolite a5 and actinolite a6, and a sample Ay as shown in FIG. 5 are tested, they can be suitably detected from the waveform of the spectral spectrum sp. . In other words, the qualitative analysis of asbestos a can be suitably performed. Of course, by adopting the microscopic Fourier transform infrared spectroscopic device 2, it is possible to suitably perform qualitative analysis of asbestos a even when the sample Ay to be tested is a very small amount.

  Although the embodiment of the present invention has been described above, the specific configuration of each unit is not limited to the above-described embodiment, and various modifications can be made without departing from the spirit of the present invention.

  For example, what is adopted as the sample is not limited to those described in the above embodiment, and can be applied to other various building materials.

  In addition, the specific configuration of each part is not limited to the above embodiment, and various modifications can be made without departing from the spirit of the present invention.

The typical block diagram which concerns on one Embodiment of this invention. The figure which shows the infrared spectroscopy spectrum of the inorganic fibrous substance which concerns on the same embodiment. Same as above. Same as above. Same as above.

Explanation of symbols

1 ... Ashing equipment, low-temperature ashing equipment (ashing equipment)
2 ... Fourier transform infrared spectroscopic analyzer, microscopic Fourier transform infrared spectroscopic analyzer (analyzer)
A ... Ash sample Ay ... Sample y ... Organic fiber a ... Asbestos (inorganic fibrous material)
S ... Qualitative analysis system for inorganic fibrous materials (analysis system)
ST: Qualitative analysis method for inorganic fibrous materials (analysis method)
st1 ... Organic fiber ashing process (ashing process)
st2 ... Fourier transform infrared spectroscopic analysis process (analysis process)
st3 ... Inorganic fiber detection process (detection process)

Claims (11)

An organic fiber ashing step for obtaining an ashed sample obtained by ashing the organic fiber by ashing the sample;
A Fourier transform infrared spectroscopic analysis step of measuring the ashed sample with a Fourier transform infrared spectroscopic device to obtain a Fourier transform infrared spectroscopic spectrum of the ashed sample;
A qualitative property of the inorganic fibrous material, comprising at least an inorganic fiber detecting step capable of detecting a predetermined inorganic fibrous material from the Fourier transform infrared spectrum obtained by the Fourier transform infrared spectroscopy Analysis method. The method for qualitative analysis of an inorganic fibrous material according to claim 1, wherein the organic fiber ashing step is a low-temperature ashing step in which the sample is ashed at a temperature of 450 ° C or lower. The method for qualitative analysis of an inorganic fibrous substance according to claim 1 or 2, wherein the Fourier transform infrared spectroscopic analysis step is a micro Fourier transform infrared spectroscopic analysis step using a microscopic Fourier transform infrared spectroscopic device. The method for qualitative analysis of an inorganic fibrous substance according to claim 1, 2 or 3, wherein the predetermined inorganic fibrous substance is asbestos. The method for qualitative analysis of an inorganic fibrous substance according to claim 1, 2, 3, or 4, wherein the sample is a suspended matter in the atmosphere. The qualitative analysis method for an inorganic fibrous substance according to claim 1, 2, 3 or 4, wherein the sample is a building material. An organic fiber ashing device for obtaining an ashed sample obtained by ashing the organic fiber by ashing the sample;
A Fourier transform infrared spectroscopic device capable of detecting a predetermined inorganic fibrous substance from a Fourier transform infrared spectroscopic spectrum of the ashed sample obtained by performing Fourier transform infrared spectroscopic analysis of the ashed sample. A system for qualitative analysis of inorganic fibrous materials. The qualitative analysis system for an inorganic fibrous substance according to claim 8, wherein the organic fiber ashing device is a low-temperature ashing device capable of ashing the sample at a temperature of 450 ° C or lower. The qualitative analysis system for an inorganic fibrous material according to claim 8, wherein the organic fiber ashing device is a low-temperature ashing device capable of ashing the sample at a temperature of 200 ° C. The qualitative analysis system for inorganic fibrous substances according to claim 7 or 8, wherein the Fourier transform infrared spectrometer is a microscopic Fourier transform infrared spectrometer. The qualitative analysis system for an inorganic fibrous substance according to claim 8, 9 or 10, wherein the predetermined inorganic fibrous substance is asbestos.

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