JP6507757B2 - Foreign substance analyzer - Google Patents

Description

The present invention relates to a foreign matter analysis apparatus capable of analyzing the foreign matter contained in the sample.

  Conventionally, it is required to analyze foreign matter contained in a sample. Therefore, Fourier transform infrared spectrophotometer (FTIR) is used when analyzing organic substances (particularly, films, plastics, rubbers, etc.) contained in a sample.

In a Michelson two-beam interferometer used as such an FTIR, infrared light emitted from an infrared light source is split by a beam splitter into two directions of a fixed mirror and a movable mirror, and reflected by the fixed mirror and returned. The structure is such that the infrared light and the infrared light reflected back by the moving mirror are combined by a beam splitter and sent to one optical path. At this time, if the moving mirror is moved back and forth in the incident light axis direction, the difference in optical path length of the two split light beams changes, so that the light intensity of the combined light changes according to the position of the moving mirror. It becomes light (interferogram).
Then, such interference light is irradiated to the surface of the sample, the wavelength of the light reflected from the surface of the sample is acquired by an infrared detector, and the library is examined to quantify the organic substances in the sample (for example, , Patent Document 1).

  On the other hand, when analyzing inorganic substances (for example, Ca, Zn, Si, Al, Mg, S, P, Fe, Cl, Cu, etc.) contained in the sample, a fluorescent X-ray analyzer (EDX) or an atomic absorption photometer (AA) and inductively coupled plasma atomic emission spectrometry (ICP) are used.

  For example, in EDX, the surface of a sample is caused to emit light by arc discharge or spark discharge, the emitted light is introduced into a spectroscope, a spectrum having a wavelength specific to each element is extracted and detected, and the intensity of the spectrum obtained The component concentration is calculated.

  In recent years, with the diversification of samples, it has become important to analyze organic and inorganic substances for samples containing organic and inorganic substances, and the analyst analyzes such samples by FTIR. It analyzes with EDX together.

JP 2002-148116 A

However, when using FTIR and EDX to analyze a sample, the analysis results may differ depending on the analyst because it is left to the analyst's knowledge, and analysis is difficult for an inexperienced analyst There was a thing.
Therefore, an object of the present invention is to provide a foreign matter analysis apparatus capable of analyzing foreign matter contained in a sample accurately and easily.

The foreign substance analysis apparatus of the present invention made to solve the above problems comprises an infrared spectrophotometer for detecting an organic element as a foreign substance contained in a sample and a computer apparatus connected to a fluorescent X-ray analyzer. a foreign matter analyzer for analyzing the sample, wherein the infrared spectrum acquiring section for acquiring infrared spectrum information of said measured sample by an infrared spectrophotometer, the of the sample as measured by X-ray fluorescence spectrometer The sample according to a fluorescent X-ray spectrum acquiring unit for acquiring fluorescent X-ray spectral information, and a ratio of an intensity of Compton scattered radiation to an intensity of Rayleigh scattered radiation in the fluorescent X-ray spectral information being 1.0 or more particular a determination section for determining whether or not the organic elements included, if it is determined to contain a specific organic elements in the determination unit, based on the fluorescent X-ray spectral information in And, based on the infrared spectrum information and the main component information, detect N types of elements having high content based on the creation unit for creating main component information indicating at least one type of element having a high content in the sample. And a detection unit.

  Here, the “set threshold” is an arbitrary numerical value predetermined by a designer or the like, and is, for example, “1.0” or the like.

As described above, according to the foreign matter analysis apparatus of the present invention, it can be easily determined whether the sample contains an organic element as a foreign matter .

In the above invention, the method further includes a quantitation unit that quantifies the elements contained in the sample using the N types of elements detected by the detection unit as the main component of the sample based on the fluorescent X-ray spectrum information. It is also good.

The “ N type” is an arbitrary numerical value predetermined by the designer or the like, and is, for example, “3 types” or “10 types”.

In the above invention, when the determination unit determines that the organic element containing C, H, O is contained, the preparation unit uses the CH ₂ O balance based on the fluorescent X-ray spectrum information. The main component information indicating at least one kind of high element is created, and the determination unit determines that the organic element including C, H, and O is not contained, the creation unit generates the fluorescent X-ray spectrum Based on the information, principal component information indicating at least one kind of high content element may be created without using CH ₂ O balance .

According to the foreign matter analysis apparatus of the present invention described above, the analysis is substantially automated, whereby a more accurate mixed foreign matter analysis can be realized in a short time.

In the above invention, an appearance information acquiring unit for acquiring appearance information of the observed sample, and a memory for storing a dedicated library indicating a relation between the infrared spectrum information and the element information associated with the appearance information are included. The detection unit may detect the N types of elements based on the acquired appearance information and a dedicated library.
Here, the appearance information may be color, shape and / or gloss .

In the above invention, the memory may store a general library indicating element information in the infrared spectrum information , and the detection unit may select whether to use the dedicated library or the general library. Good.

BRIEF DESCRIPTION OF THE DRAWINGS The block diagram which shows the foreign material analysis apparatus which concerns on this invention. The flowchart explaining the foreign material analysis method by the apparatus of this invention. The flowchart explaining the foreign material analysis method by the apparatus of this invention.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. The present invention is not limited to the embodiments described below, and includes various aspects without departing from the spirit of the present invention.

FIG. 1 is a view showing the configuration of a foreign matter analysis apparatus according to the present invention.
The foreign substance analysis device 1 includes an FTIR 10, an EDX 20, and a computer 30.

The FTIR 10 includes an infrared light source unit 11 for emitting infrared light, an infrared light detection unit 12 having an infrared detector 12a and a mirror 12b for detecting an interferogram (infrared light), and a sample S And a sample placement unit 13.
The infrared light source unit 11 includes an infrared light source 11a that emits infrared light, a main interferometer main portion 11b that creates an interferogram, a mirror 11c, and the like. The infrared light emitted from the infrared light source 11a is irradiated to the beam splitter of the main interferometer main portion 11b.

In the main interferometer main part 11b, a movable mirror unit provided with a movable mirror, a beam splitter, and a fixed mirror unit provided with a fixed mirror are arranged.
According to such a main interferometer main portion 11b, the infrared light emitted from the infrared light source 11a is irradiated to the beam splitter and divided in two directions of the moving mirror and the fixed mirror. Then, the infrared light reflected by the moving mirror and the infrared light reflected by the fixed mirror return to the beam splitter, and these infrared lights are combined by the beam splitter and sent to the mirror 11 c. At this time, since the movable mirror reciprocates back and forth in the incident optical axis direction M, the difference in optical path length of the two split light beams changes periodically, and the light traveling from the beam splitter to the mirror 11c is temporally Becomes an interferogram whose amplitude fluctuates.

  When the sample S is placed at a predetermined position (measurement position), the light collected by the mirror 11 c is irradiated to the measurement point of the sample S, and the sample placement unit 13 reflects or transmits the light at the measurement point of the sample S The light is condensed by the mirror 12 b to the infrared detector 12 a, and the infrared spectrum information obtained by the infrared detector 12 a is output to the computer 30.

  The EDX 20 includes a spectroscope stand 20a. The spectroscope stand 20a includes a counter electrode 20b disposed upward and a spectroscope 20c into which emitted light is introduced. An opening 20d is formed on the top surface of the spectroscope stand 20a at a position facing the counter electrode 20b.

  According to such an EDX 20, the measurement point of the sample S is abutted so as to close the opening 20d of the spectroscope stand 20a, discharge is performed between the measurement point and the counter electrode 20b, and the emitted light is a spectroscope It is introduced into 20 c and a spectrum having a wavelength specific to each element is extracted and detected. Then, the fluorescent X-ray spectrum information obtained by the spectroscope 20 c is output to the computer 30.

The computer 30 includes a CPU (control unit) 31 and a memory 32, and a display device 33 and an input device 34 are connected.
The functions to be processed by the CPU 31 will be described in blocks: an infrared spectrum acquisition unit 31a acquiring infrared spectrum information from the infrared detector 12a, and a fluorescence X-ray spectrum acquisition unit 31b acquiring fluorescence X-ray spectrum information from the spectroscope 20c. , An appearance information acquisition unit 31c that acquires appearance information from the input device 34, a determination unit 31d that determines whether an organic element is contained in the sample S, and main component information based on fluorescence X-ray spectrum information A creating unit (semi-quantifying unit) 31e to be created, a detecting unit 31f for detecting N kinds of elements based on infrared spectrum information, principal component information, appearance information, and a dedicated library, and a sample based on fluorescence X-ray spectrum information Based on infrared spectrum information, principal component information, and a general library, a quantification unit 31g that qualitatively and quantifies elements contained in S With the auxiliary quantification section 31h for analyzing Te.

In addition, a dedicated library and a general library are stored in advance in the memory 32 (storage step). The dedicated library indicates the relationship between appearance information (color, shape, presence of gloss ) and elemental information in infrared spectrum information. Moreover, a general library shows element information in infrared spectrum information, and a commercial item can be used.

  The determination unit 31 d compares the ratio of the intensity of the Compton scattered radiation and the intensity of the Rayleigh scattered radiation in the fluorescent X-ray spectrum information with the “1.0 (preset threshold)” to obtain the organic element in the sample S. Control is performed to determine whether or not it is included. Specifically, when it is determined that the ratio is "1.0" or more, it is determined that the sample S contains an organic element, and when it is determined that the ratio is less than "1.0", It is determined that the sample S contains no organic element.

The creation unit (semi-quantification unit) 31e performs control to create principal component information based on the fluorescent X-ray spectrum information.
For example, when the determination unit 31d determines that the sample S contains an organic element, the CH ₂ O balance is used to detect an element whose content is 0.1% by weight or more. When the number of kinds is six or more, the first to fifth highest elements are detected, and the five kinds of elements are used as main component information. If an element whose content is not less than 0.1% by weight can not be detected, an element having the first to third highest content is detected, and these three elements are used as main component information.
On the other hand, when the determination unit 31d determines that the sample S does not contain an organic element, the balance is not used and an element having a content of 0.1% by weight or more is detected. In the case of the above, an element whose content is the first to fifth highest is detected, and these five types of elements are used as main component information. If an element whose content is not less than 0.1% by weight can not be detected, an element having the first to third highest content is detected, and these three elements are used as main component information.

The detection unit 31 f performs control to detect N types of elements based on infrared spectrum information, main component information, appearance information, and a dedicated library.
For example, the search wave number range is limited for each element based on the principal component information, and the 10 types of elements having high contents are detected and displayed on the display device 33 using the appearance information and the dedicated library. Determine the three elements of high content from

The quantifying unit 31g performs control to characterize and quantify the elements contained in the sample S based on the fluorescent X-ray spectrum information.
For example, whether the analyst confirms the 10 types of elements displayed in the detection unit 31f, and makes the 10 types of elements the main component of the sample S, or makes the 3 types of elements the main component of the sample S Input signal is input to the input device 34. Thereby, the quantifying unit 31g determines three elements as the main component of the sample S based on the input signal and determines the elements contained in the sample S, or ten elements as the main component of the sample S. The elements contained in the sample S are quantified.

The auxiliary quantifying unit 31h detects M types of elements based on the infrared spectrum information, the main component information, and the general library, and controls to finally quantify the elements contained in the sample S.
For example, when the analyst inputs an input signal indicating the desired number M of detection element types to the input device 34, the auxiliary quantification unit 31h converts the input signal, the infrared spectrum information, the main component information, and the general library into Based on the detection of M types of elements, the elements contained in the sample S are quantified from fluorescent X-ray spectrum information and infrared spectrum information using M types of elements.

Here, a foreign substance analysis method (foreign substance analysis apparatus ) for analyzing the sample S by the foreign substance analysis apparatus 1 according to the present invention will be described with reference to the flowcharts of FIGS. 2 and 3.
First, in the process of step s101, the infrared spectrum acquisition unit 31a acquires infrared spectrum information from the infrared detector 12a, and the fluorescence X-ray spectrum acquisition unit 31b acquires fluorescence X-ray spectrum information from the spectrometer 20c. .
Next, in the process of step s102, the appearance information acquisition unit 31c displays an input screen or the like on which the appearance information (color , shape, presence or absence of gloss ) is input on the display device 33, and the appearance input by the analyst etc. Get information.

Next, in the process of step s103, the determination unit 31d determines whether the ratio between the intensity of the Compton scattered radiation and the intensity of the Rayleigh scattered radiation in the fluorescent X-ray spectrum information is “1.0” or more. Do. If it is determined that the ratio is “1.0” or more, in the process of step s104, the creation unit 31e creates principal component information based on the fluorescent X-ray spectrum information.
Next, in the process of step s105, the detection unit 31f detects 10 types of elements having high contents based on the infrared spectrum information, the main component information, and the dedicated library, and displays them on the display device 33. Determine the three elements with high contents among them.

When three types of elements having high contents can be determined in the processing of step s105, in the processing of step s106, the quantification unit 31g selects 10 types or 3 types of elements based on the fluorescent X-ray spectrum information. The elements contained in the sample S are quantified as the main component of the sample S.
Next, in the process of step s107, the infrared spectrum analysis result obtained in the process of step s105 and the fluorescent X-ray spectrum analysis result obtained in the process of step s106 are displayed on the display device 33.

Next, in the process of step s108, the analyst determines whether to analyze using the general library. When the use of the general library is selected, or when the three elements having high contents can not be determined in the process of step s105 (when the hit is not successful), the auxiliary quantification unit 31h in the process of step s109 , M types of elements are detected based on infrared spectrum information, principal component information, and a general library.
Next, in the process of step s110, the auxiliary quantification unit 31h detects elements of which the content is 0.1 wt% or more, with M types of elements as the main component of the sample S based on the fluorescent X-ray spectrum information. However, when there are six or more types, the first to fifth highest elements are detected, and the five types of elements are used as main component information. If an element whose content is not less than 0.1% by weight can not be detected, an element having the first to third highest content is detected, and these three elements are used as main component information.

Next, in the process of step s111, the auxiliary quantification unit 31h quantifies the elements contained in the sample S based on the infrared spectrum information, the main component information, and the general library.
Next, in the process of step s112, the display unit 33 displays the fluorescent X-ray spectrum analysis result obtained in the process of step s110 and the infrared spectrum analysis result obtained in the process of step s111.

On the other hand, when it is determined in the process of step s103 that the ratio is less than “1.0”, in the process of step s113, the creating unit 31e creates principal component information based on the fluorescent X-ray spectrum information.
Next, in the process of step s114, the detection unit 31f detects 10 types of elements with high contents based on the infrared spectrum information, the main component information, and the dedicated library, and displays them on the display device 33. Determine the three elements with high contents among them.

When three types of elements having high contents can be determined in the processing of step s114, in the processing of step s115, the quantification unit 31g selects 10 types or 3 types of elements based on the fluorescent X-ray spectrum information. The elements contained in the sample S are quantified as the main component of the sample S.
Next, in the process of step s116, the infrared spectrum analysis result obtained in the process of step s114 and the fluorescent X-ray spectrum analysis result obtained in the process of step s115 are displayed on the display device 33.

  Next, in the process of step s117, the analyst determines whether or not to analyze using a general library. When the use of the general library is selected, or when the three types of elements having high contents can not be determined in the process of step s114, in the process of step s118, the auxiliary quantification unit 31h determines infrared spectrum information and principal component information And M types of elements are detected on the basis of and the general library.

  Next, in the process of step s119, the display unit 33 displays the fluorescent X-ray spectrum analysis result obtained in the process of step s113 and the infrared spectrum analysis result obtained in the process of step s117.

  When it is determined that the general library is not used in the process of step s108 or the process of step s117, or when the process of step s112 or s119 is completed, the present flowchart is ended.

As described above, according to the foreign substance analysis apparatus of the present invention, if infrared spectrum information and fluorescent X-ray spectral information are acquired, the subsequent analysis is almost automated, so that mixed foreign substance analysis can be performed more accurately in a short time. Can be realized.

  The present invention can be suitably used for a foreign matter analysis apparatus etc. capable of analyzing foreign matter contained in a sample.

1 foreign matter analysis equipment 10 FTIR (infrared spectrophotometer)
20 EDX (Fluorescent X-ray Analyzer)
31a Infrared spectrum acquisition unit (infrared spectrum acquisition step)
31b X-ray fluorescence spectrum acquisition unit (X-ray fluorescence spectrum acquisition step)
31d Judgment unit (judgment step)
S sample

Claims (6)

A foreign substance analysis apparatus comprising: an infrared spectrophotometer for detecting an organic element as a foreign substance contained in a sample; and a computer device connected to a fluorescent X-ray analyzer, wherein the foreign substance analysis apparatus for analyzing the sample,
An infrared spectrum acquiring section for acquiring infrared spectrum information of the sample that the measured in an infrared spectrophotometer,
And a fluorescent X-ray spectrum acquisition unit that acquires the fluorescence X-ray spectral information of said sample is measured by a fluorescent X-ray analyzer,
In the either the ratio of the intensity of the intensity of the Compton scattered radiation in the fluorescent X-ray spectral information and Rayleigh scattered radiation is 1.0 or more, determined determines whether contain specific organic element in the sample Department,
When it is determined by the determination unit that the specific organic element is contained, a creation unit that creates principal component information indicating at least one type of element having a high content in the sample based on the fluorescent X-ray spectrum information When,
A detection unit that detects N types of elements having a high content based on the infrared spectrum information and the main component information;
A foreign substance analysis device characterized in that The apparatus according to claim 1, further comprising: a quantitative unit that uses the N types of elements detected by the detection unit as a main component of the sample based on the fluorescent X-ray spectrum information, and quantifies the elements contained in the sample. Foreign substance analyzer. When it is determined by the determination unit that the organic element containing C, H, and O is contained, the creation unit uses the CH ₂ O balance based on the fluorescence X-ray spectrum information, and at least one having a high content. Create principal component information indicating the types of elements,
When the determination unit determines that the organic element containing C, H, and O is not contained, the creation unit does not use the CH ₂ O balance based on the fluorescent X-ray spectrum information, and the content of The foreign substance analysis device according to any one of claims 1 and 2, wherein principal component information indicating at least one kind of high element is created . An appearance information acquisition unit that acquires appearance information of the observed sample ;
And a memory for storing a dedicated library indicating the relationship between the infrared spectrum information and the element information associated with the appearance information .
The foreign matter analysis apparatus according to claim 3, wherein the detection unit detects the N types of elements based on the acquired appearance information and a dedicated library. 5. The foreign matter analysis apparatus according to claim 4 , wherein the appearance information is color, shape and / or gloss . The memory stores a general library indicating element information in the infrared spectrum information ;
The foreign matter analysis apparatus according to any one of claims 4 and 5, wherein the detection unit selects whether to use the dedicated library or the general library.

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