JPS62110132A - Method for preparing specimen - Google Patents

Abstract

PURPOSE:To prevent the mixing of a contaminant, by inserting a test piece having the same composition as a specimen plate in a holding container and hermetically closing said holding container before rotating or oscillating the same. CONSTITUTION:Specimen plates 6-10 are arranged in a holding container 1 so to be contacted with the bottom surface or side surface thereof and a specimen piece coarsely ground preliminarily is put in the container 1. Thereafter, a specimen plate 11 to be arranged to an upper surface is allowed to cover the holding container 1 and, further, an upper lid 12 is allowed to cover from above to be fixed to the holding container 16 by screws 13-16. By rotating or oscillating thus constituted holding container 1 by a ball mill, the mixing of a contaminant can be prevented.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a sample preparation method for finely pulverizing a highly hard substance such as ceramics.

[Conventional technology]

When analyzing ceramics, etc., it is necessary to pulverize them in order to efficiently perform acid dissolution. For this reason, conventionally, the material was wrapped in paraffin paper and coarsely pulverized by pounding it with an iron bowl, and then finely pulverized using a rod mill made of tungsten carbide (WC) or the like.

[Problem that the invention seeks to solve]

According to the conventional method, WC and Co contained in the rod mill inevitably mix into the sample. For this reason, for example, when measuring the amount of C in SiC ceramics, the amount of mixed WCOC directly affects the measured value. In addition, for example, when conducting chemical analysis of A403 ceramics,
Minor components S lo, , Fe203, Ca
Measure O, etc. using the spectrophotometric method or atomic absorption method.

The purity (content) of At20° is determined by subtracting these contents from 100, but in this case, WC+Co is mixed in during the pulverization.

The initial sample weight value itself contains errors, which affect the accuracy of the measured value. Among these, it is not easy to analyze WC in particular, and it is also difficult to correct the measured values of each component from the analyzed values.

[Failure to solve the problem]

In the sample preparation method of the present invention, a sample plate for the purpose of pulverization is brought into close contact with the inner wall of a previously prepared container made of plastic or the like to construct a container.

Furthermore, the method is characterized in that a coarse piece of the same sample is placed inside the container, and the container itself, such as a plastic container, is rotated and/or shaken to produce a finely pulverized sample.

[Effect]

In the sample preparation method described above, pulverization basically proceeds through the collision of the sample plate to be pulverized with the coarse pieces of the same sample, so contaminants (equivalent to the aforementioned WC and CO) are ) There is no risk of contamination. More particularly, when a plastic container is used as a holder for a sample plate to be ground, plastic components mixed into the ground sample do not become contaminants because they can be easily removed by heat treatment or the like.

〔Example〕

FIG. 1 is a block diagram of an embodiment of a crushing container used in the sample preparation method of the present invention. 1 in the figure is.

This is a container for holding the sample plate, and is a box-shaped container with an open top. Screw holes 2 to 5 are provided at the four corners of the upper surface of the holding container. Further, numerals 6 to 11 are sample plates composed of flat plates of samples to be crushed, which are the bottom and side surfaces of the holding container, respectively.

It is machined to approximate the dimensions of the top cover. Reference numeral 12 denotes an upper lid for holding down the sample plate 11 installed on the upper surface;
There are holes 2 in the four corners of 2 facing the screw holes 2 to 5 of the holding container 1.
' to 5' are open. Further, 13 to 16 are screws for fixing the holding container 1 and the upper lid 12.

When preparing a sample using the crushing container configured as described above, follow the steps below.

(2) Sample plates 6 to 10 are arranged in contact with the bottom and side surfaces of the holding container 1.

■ Place a coarsely crushed sample piece in advance into the holding container 1.

■Then, cover the sample plate 11 to be placed on the top surface.

Furthermore, the upper lid 12 is placed over it and fixed to the holding container 1 with screws 13 to 16.

(2) Rotating and/or shaking the holding container 1 thus constructed using a ball mill, planetary mill, or the like.

〔Effect of the invention〕

According to the sample preparation method performed as described above, the crushing process is performed using a sample plate and a sample piece. Since it is a so-called co-printing method, there is no risk of contamination by contaminants. If contaminants from the holding container are suspected, if the holding container is made of plastic such as tetrafluoroethylene, the contaminants can be treated by heat treatment or the like.

[Brief explanation of drawings]

FIG. 1 is a block diagram of an embodiment of a crushing container used in the sample preparation method of the present invention. 1... Holding container, 2-5... Screw hole, 2'-5'.
··hole. 6-11... Sample plate, 12... Top lid, 13-16.
··screw.

Claims (1)

[Claims] A sample plate made to approximate the inner dimensions of a flat plate constituting a box-shaped sample holding container is fixed to the inner wall of the holding container, and a sample piece having the same composition as the sample plate is placed inside the holding container. A sample preparation method characterized by rotating and/or shaking the holding container after the holding container is sealed.