JPS58143254A - Substance identifying device - Google Patents

Abstract

PURPOSE:To increase the quantity of information, to easily identify a substance, to elevate the exactitude for identification, and to efficiently execute an analyzing work, by incorporating an analyzing means into an X-ray diffracting device. CONSTITUTION:A driving pulse of a goniometer controlling device 5 is sent to a data processing device 12 and is counted, and an angle position on a goniometer of a sample 3, an X-ray tube 2 and an X-ray detector 6 are detected. A meansuring circuit 7 sends diffracted X-ray intensity data obtained from an output pulse of the detector 6, to the device 12. The device 12 calculates a lattice plane gap from the tube 2 in case when the diffracted X-ray is at a peak, and the angle position of the detector 6, and obtains the data regarding a Debye- Scherrer ring for the sample 3. Also, a condensing optical system 10 condenses light from the sample 3 and makes it incident to a spectrophotometer 11. A spectral reflecting characteristic of the sample 3 is calculated by a ratio of a spectral photometric value of reflected light of the sample 3, to a photometric value in the corresponding wavelength of a standard white plate stored in advance, and a fluorescent characteristic of the sample 3 is obtained by the photometer 11. By these data, a classification of a sample substance is identified.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for identifying a given sample material, particularly a crystalline sample material.

X-ray diffraction is often used to identify crystalline samples. However, although it is relatively easy to determine whether a given sample is the expected substance using X-ray diffraction, it is not easy to determine what the sample substance is, and the predictive value of identification is low. not good.

When identifying substances in a laboratory, there is no time constraint, and a variety of equipment is available and a variety of analysis methods can be used to ensure reliable identification. When identifying a sample, there are time constraints and equipment is also limited, so it is desirable to be able to perform analysis in a short period of time with a single device.

The present invention increases the amount of information, facilitates substance identification, and improves the accuracy of identification by incorporating other analytical means into the X-ray diffraction apparatus, where identification is difficult due to lack of information using X-ray diffraction alone. The aim is to provide an expensive substance identification device. The present invention will be explained below with reference to Examples.

The drawing shows an embodiment of the invention. 1 is a goniometer of an X-ray diffraction apparatus, 2 is an X-ray tube, 3 is a sample set at the center of the goniometer 1, 4 is a power supply for the X-ray tube, and 6 is an X-ray detector.

Reference numeral 5 denotes a goniometer control device, which rotates the X-ray detector 6 around the sample 3 in the case of a powder or polycrystalline sample, so that the incident angle of the X-rays relative to the sample 3 can be changed as appropriate.
The sample 3 and the X-ray source 2 can be rotated around the goniometer 1. These rotations themselves are performed by pulse motors, and the goniometer control device 5 transfers the pulse signals that drove these pulse motors to the data processing device 12.
send to The data processing device 12 counts those pulses and calculates the pulses for the sample 3. X-ray tube2. The angular position of the X-ray detector 6 on the goniometer is detected. 7 receives the output pulse of the X-ray detector 6 through the x, 1 measurement circuit and measures the diffracted X-ray intensity. This intensity data is also
2, the data processing device 12 detects the peak of the diffracted X-rays, calculates the lattice spacing or black reflection angle from the angular positions of the X-ray tube 2 and the X-ray detector 60 at that time, and calculates several By detecting the diffraction X-ray peak of , data regarding the Debye-Scherrer ring for the sample is obtained. 8 is a light source, 9 is an irradiation optical system that focuses the light from the light source and projects it onto the sample 3, 10 is a focusing optical system, 11 is a spectrophotometer, and the focusing optical system 10 collects the light coming from the sample 3. Spectrophotometer 1
1 is insufficient. The light coming from the sample 3 is not limited to only the reflected light of the light from the light source 8, but also includes fluorescent light excited by the irradiation of the light from the light source 8, Raman scattered light, and even fluorescent light excited by the irradiation of X-rays. etc. are also included. The data processing device 12 stores the spectral characteristics of the light source 8 in advance. To do this, a standard white plate is placed at the position of the sample 3, and the reflected light from the light source 8 is measured using a spectrophotometer, and the results are input into a data processing device. Spectral reflection characteristics of arbitrary sample 3 are sample 30
The spectrophotometer 11 can obtain the fluorescence characteristics of the sample by changing the light source to the spectrophotometric value of the reflected light and the photometric value at the corresponding wavelength of a standard white plate previously stored. Furthermore, by irradiating the sample with X-rays without energizing the light source 8, it is also possible to measure fluorescence when the sample is excited with X-rays. Data from these measurements are input to and stored in the data processing device 12.

In the above-mentioned apparatus, any program can be used to identify the type of sample substance from the data about one sample accumulated in the data processing device 12 and the data about various substances stored in advance. For example, search for a substance that gives a diffraction line that is the same as or very similar to the diffraction line that also gives a strong peak in the diffraction The process of searching for a substance that gives a diffraction line that matches the diffraction line of is repeated. Normally, this narrows down the candidates to several candidate substances, but it is difficult to decide on a single substance name based only on X-ray diffraction data. Here, the color characteristics of the sample, ie, the spectral reflectance and fluorescence characteristics, are referenced to confirm the identity of the sample substance.

The device of the present invention has the above-mentioned configuration, and can obtain X-ray diffraction data and spectroscopic data with one device, making it easy to identify the sample substance and improving the predictive value. Fluorescence spectrum data in the form of lines provides extremely powerful information for identifying samples containing rare earth elements, for example, and the equipment consists mainly of an X-ray diffraction device, with a goniometer also serving as a sample stage during spectroscopic measurements. , X-ray sources can also be used as excitation lines for fluorescence analysis, so they are multifunctional.
Compared to installing separate devices for each function, equipment costs for analysis can be significantly reduced, and since the device is multi-functional, only a single sample is needed, and sample preparation or Since there is no time consumption such as transferring from one device to another, and two types of analysis methods can be carried out simultaneously and in parallel, the effect of streamlining the analysis work can also be obtained.

[Brief explanation of the drawing]

The drawing is a block diagram showing the configuration of an apparatus according to an embodiment of the present invention. DESCRIPTION OF SYMBOLS 1... Goniometer, 2... X-ray tube, 3... Sample, 5... Goniometer control device, 6... X-ray detector, 7... X-ray measurement circuit, 8... Light source, 9... Irradiation optical system, 10... Condensing optical system, 11... Spectrophotometer, 12... Data processing device.

Claims (1)

[Claims] The sample substance is identified using an X-ray diffraction device, a spectrometer that spectrophotometrically measures the sample set in the device, data obtained from the X-ray diffraction device and spectrometer 1 device, and data related to various substances contained therein. A substance identification device consisting of a data processing device.