JP2006184066A - Spectroscopic analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a new spectroscopic analyzer in which a fluorescent X-ray spectroscopic analysis system, capable of acquiring information on constituent elements and a Raman spectroscopic analysis system, capable of acquiring information on atomic coupling are skillfully combined with each other. <P>SOLUTION: The spectroscopic analyzer is capable of simultaneous measurements on elementary analysis in a sample and information on molecular binding at the same location of the sample and is provided with both a Raman spectroscopic analyzer (a) provided with a Raman probe for making a laser beam enter a sample surface in a coaxial direction with an observation camera, having an optical axis in a vertical direction and extracting Raman scattering light of the sample in the coaxial direction with the camera and a fluorescent X-ray spectroscopic analyzer (b) for making X-rays incident on the location of the intersection between an optical axis of the Raman spectroscopic analyzer and the sample surface from an oblique direction and received X-rays, reflected at the location of the intersection at an X-ray detector arranged in an oblique direction. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to an analytical apparatus capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample, and more particularly to a spectral analysis apparatus combining a Raman spectroscopic analysis apparatus and a fluorescent X-ray spectroscopic analysis apparatus.

  In recent years, device manufacturers have been forced to respond to the European Environmental Standards WEEE & RoHS Directive. In particular, in order to analyze chromium, which is a toxic substance, and bromine in organic substances, measurements using fluorescent X-ray, FTIR, Raman, XPS, MS, etc. are performed. The possibility of being incorporated into is being studied.

JP 2001-13095 A.

JP-T-2002-514747.

  Conventionally, an X-ray fluorescence spectrometer has been widely used for analysis of chromium and bromine. However, when chromium is analyzed by an X-ray fluorescence spectrometer, the total amount of chromium can be analyzed, but there is a problem that the valence of trivalent chromium and hexavalent chromium cannot be determined. Further, when bromine is analyzed by an X-ray fluorescence spectrometer, the total amount of bromine can be analyzed, but there is a problem that it is impossible to determine what organic structure bromine has.

  On the other hand, as shown in FIG. 1, the Raman spectroscopic analyzer can determine the trivalent and hexavalent valences of chromium from the spectrum. In addition, for bromine, the bromine-derived signal is not affected by the base material. It has the advantage that it can be detected and information about the molecular structure can be obtained. In environmental problems, the determination of hexavalent chromium, which is extremely toxic to the human body, is important. However, if the total amount of chromium is determined with a fluorescent X-ray spectrometer and the hexavalent chromium is determined with a Raman spectrometer. Complementary data can be obtained.

  If non-destructive evaluation of materials is performed in a short time by using an X-ray fluorescence spectrometer and a Raman spectrometer in a complementary manner, it can be an effective measurement tool for the European Environment Standards WEEE & RoHS Directive. .

  In view of the above-described points, the object of the present invention is to provide a new spectroscopic device that is devised in combination with a fluorescent X-ray spectroscopic analyzer that obtains information on constituent elements and a Raman spectroscopic analyzer that obtains information about atomic bonds. An analyzer is provided.

In order to achieve this object, a spectroscopic analyzer according to the present invention provides:
A spectroscopic analyzer capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample,
(A) a Raman spectroscopic analysis apparatus provided with a Raman probe that allows laser light to be incident in a coaxial direction with an observation camera having an optical axis in a direction perpendicular to the sample surface, and to extract Raman scattered light from the sample in the coaxial direction with the camera;
(B) An X-ray detector in which X-rays are incident from an oblique direction on the intersection point between the optical axis of the Raman spectroscopic analyzer and the sample surface, and the X-rays reflected at the intersection point are placed in the oblique direction. X-ray fluorescence spectrometer for receiving light,
It is characterized by having.

  The observation camera and the Raman probe can be replaced with each other.

  The optical axis of the X-ray fluorescence spectrometer is inclined at an angle of 45 ° with respect to the sample surface.

In addition, a spectroscopic analyzer capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample,
(A) an X-ray fluorescence spectrometer that makes X-rays incident on the sample surface in the vertical direction and receives the reflected X-rays with an X-ray detector placed in an oblique direction;
(B) The laser beam from the lateral direction through a half mirror placed on the X-ray incident optical axis at an intersection position between the X-ray incident optical axis and the sample surface of the X-ray fluorescence spectrometer And a Raman spectroscopic analysis apparatus comprising a Raman probe that takes out the Raman scattered light of the sample generated at the intersection position from the X-ray incident optical axis via the half mirror,
It is characterized by having.

  The half mirror is made of a material that transmits X-rays and reflects visible light.

  The half mirror is made of a thin aluminum plate, a thin beryllium plate, or a dichroic mirror.

  In addition, instead of the Raman probe, a compatible observation camera is installed.

According to the spectroscopic analyzer of the present invention,
A spectroscopic analyzer capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample,
(A) a Raman spectroscopic analyzer provided with a Raman probe that allows laser light to be incident in a coaxial direction with an observation camera having an optical axis in a direction perpendicular to the sample surface, and to extract Raman scattered light from the sample in the coaxial direction with the camera;
(B) An X-ray detector in which X-rays are incident from an oblique direction with respect to the intersection position between the optical axis of the Raman spectroscopic analyzer and the sample surface, and the X-ray reflected at the intersection position is placed in the oblique direction. X-ray fluorescence spectrometer for receiving light,
So that
It is possible to provide a new spectroscopic analysis device that has been devised in a combination of a fluorescent X-ray spectroscopic analysis device that can obtain information on constituent elements and a Raman spectroscopic analysis device that can obtain information on the bonding of atoms.

In addition, a spectroscopic analyzer capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample,
(A) an X-ray fluorescence spectrometer that makes X-rays incident on the sample surface in the vertical direction and receives the reflected X-rays with an X-ray detector placed in an oblique direction;
(B) The laser beam from the lateral direction through a half mirror placed on the X-ray incident optical axis at an intersection position between the X-ray incident optical axis and the sample surface of the X-ray fluorescence spectrometer And a Raman spectroscopic analysis apparatus comprising a Raman probe that takes out the Raman scattered light of the sample generated at the intersection position from the X-ray incident optical axis via the half mirror,
So that
It is possible to provide a new spectroscopic analysis device that has been devised in a combination of a fluorescent X-ray spectroscopic analysis device that can obtain information on constituent elements and a Raman spectroscopic analysis device that can obtain information on the bonding of atoms.

  Embodiments of the present invention will be described below with reference to the drawings.

  FIG. 2 shows an embodiment of a spectroscopic analyzer according to the present invention. FIG. 2 shows the main configuration of the spectroscopic analyzer according to the present invention.

  In FIG. 2A, 1 is a sample. The measurement surface of sample 1 is facing downward. The X-ray fluorescence spectrometer is an X-ray detector in which X-rays are incident from an X-ray generator 2 located approximately 45 ° obliquely downward, and X-rays reflected on the sample surface are disposed approximately 45 ° obliquely downward. The light is received by the device 3. Thereby, a fluorescent X-ray spectrum can be acquired.

  On the other hand, the Raman probe 4 causes laser light to enter vertically upward with respect to the sample surface, and extracts Raman scattered light from the sample in the coaxial downward direction. At this time, since the position on the sample surface where the laser beam hits and the position on the sample surface where the X-ray hits are the same position, the same part of the sample is analyzed simultaneously with fluorescent X-rays and Raman. Will be. Since the fluorescent X-ray and Raman information at the same location can be obtained at the same time, information with much higher reliability can be obtained as compared with the case where the fluorescent X-ray and Raman are measured separately.

  As shown in FIG. 2B, the Raman probe 4 is configured to be used in place of a CCD camera fiberscope 5 with an observation function. The Raman probe 4 and the CCD camera fiber with an observation function are used. Since the flange (not shown) for attaching the scope 5 is completely shared, no cost is required. When Raman analysis is not performed, if the CCD camera fiberscope 5 with an observation function is installed, the sample surface can be observed with an image. The Raman probe 4 and the CCD camera fiberscope 5 with an observation function use the same optical axis and are compatible with each other.

  FIG. 3 shows an embodiment of a spectroscopic analyzer according to the present invention. FIG. 3 shows a main configuration of the spectroscopic analyzer according to the present invention. The same components as those in FIG. 2 will be described with the same numbers.

  In FIG. 3A, 1 is a sample. The measurement surface of the sample 1 is facing upward. The X-ray fluorescence spectrometer receives X-rays from an X-ray generator 2 positioned vertically upward, and receives X-rays reflected from the sample surface by an X-ray detector 3 placed obliquely upward. Thereby, a fluorescent X-ray spectrum can be acquired.

  On the other hand, the Raman probe 3 is reflected by a half mirror 6 placed at an inclination of approximately 45 ° on the incident optical axis of X-rays, and laser light is incident from the lateral direction to irradiate the sample surface. The sample Raman scattered light generated on the sample surface is taken out from the X-ray incident optical axis in the lateral direction via the half mirror 6.

  The half mirror 6 is made of a material that transmits X-rays and reflects visible light. For this purpose, for example, a thin aluminum plate, a thin beryllium plate, or a dichroic mirror can be used. As a result, even if the X-ray is transmitted while the half mirror is fixed on the optical axis of the X-ray, the X-ray analysis is not affected.

  At this time, since the position on the sample surface where the laser beam hits and the position on the sample surface where the X-ray hits are the same position, the same part of the sample is analyzed simultaneously with fluorescent X-rays and Raman. Will be. Since the fluorescent X-ray and Raman information at the same location can be obtained at the same time, information with much higher reliability can be obtained as compared with the case where the fluorescent X-ray and Raman are measured separately.

  As shown in FIG. 3B, the Raman probe 4 is configured to be used in place of the CCD camera fiberscope 5 with an observation function. The Raman probe 4 and the CCD camera fiber with an observation function are used. Since the flange (not shown) for attaching the scope 5 is completely shared, no cost is required. When Raman analysis is not performed, if the CCD camera fiberscope 5 with an observation function is installed, the sample surface can be observed with an image. The Raman probe 4 and the CCD camera fiberscope 5 with an observation function use the same optical axis and are compatible with each other.

  Can be widely used for environmental analysis.

It is an example of the Raman spectrum of chromium. It is a figure which shows one Example of the spectroscopic analyzer concerning this invention. It is a figure which shows another Example of the spectroscopic analyzer concerning this invention.

Explanation of symbols

1: Sample, 2: X-ray generator, 3: X-ray detector, 4: Raman probe, 5: CCD camera fiberscope with observation function, 6: Half mirror

Claims (7)

A spectroscopic analyzer capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample,
(A) a Raman spectroscopic analysis apparatus provided with a Raman probe that allows laser light to be incident in a coaxial direction with an observation camera having an optical axis in a direction perpendicular to the sample surface, and to extract Raman scattered light from the sample in the coaxial direction with the camera;
(B) An X-ray detector in which X-rays are incident from an oblique direction on the intersection point between the optical axis of the Raman spectroscopic analyzer and the sample surface, and the X-rays reflected at the intersection point are placed in the oblique direction. X-ray fluorescence spectrometer for receiving light,
A spectroscopic analyzer characterized by comprising: The spectroscopic analysis apparatus according to claim 1, wherein the observation camera and the Raman probe can be replaced with each other. 2. The spectroscopic analyzer according to claim 1, wherein an optical axis of the fluorescent X-ray spectroscopic analyzer is inclined at an angle of 45 [deg.] With respect to the sample surface. A spectroscopic analyzer capable of simultaneously measuring elemental analysis and molecular bond information in a sample at the same location of the sample,
(A) an X-ray fluorescence spectrometer that makes X-rays incident on the sample surface in the vertical direction and receives the reflected X-rays with an X-ray detector placed in an oblique direction;
(B) The laser beam from the lateral direction through a half mirror placed on the X-ray incident optical axis at an intersection position between the X-ray incident optical axis and the sample surface of the X-ray fluorescence spectrometer And a Raman spectroscopic analysis apparatus comprising a Raman probe that takes out the Raman scattered light of the sample generated at the intersection position from the X-ray incident optical axis via the half mirror,
A spectroscopic analyzer characterized by comprising: The spectroscopic analyzer according to claim 4, wherein the half mirror is made of a material that transmits X-rays and reflects visible light. 6. The spectroscopic analyzer according to claim 5, wherein the half mirror is made of a thin aluminum plate, a thin beryllium plate, or a dichroic mirror. 5. The spectroscopic analysis apparatus according to claim 4, wherein a compatible observation camera is installed instead of the Raman probe.

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