JPH11118686A - Creation method for refractory test body for fluorescent x-ray analysis - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a creation method in which a glass-bead test body for fluorescent X-ray analysis is created safely and easily by a method wherein an oxidized and molten substance which is obtained by indirectly heating a mixture of a ceramic refractory and a lithium borate-based flux is induction-heated and a uniform molten liquid is formed so as to be changed into glass beads. SOLUTION: A ceramic refractory sample which is oxidized and treated at a high temperature is broken into pieces until it is passed wholly through a sieve of 100 μm. The sample in a prescribed amount is sampled so as to be mixed well with lithium metaborate (a lithium borate-based flux) whose weight is about 10 times and which is dried and treated, and it is spread all over uniformly in a flat-bottom evaporating dish which is composed of a platinum alloy containing gold. Then, a vertical electric furnace is heated preliminarily. The flat-bottom evaporating dish is put into the furnace, and a temperature is set at about 1100 deg.C. The sample is heated for about 30 minutes, it is oxidized and melted, and a molten substance in a turbid state is obtained. After that, the molten substance is moved to a deep pan whose material is identical to that of the flat-bottom dish, it is put into an induction heating-type vertical electric furnace so as to be heated at about 1200 deg.C, and it is melted completely. A uniform molten liquid is obtained, and it is then cooled so as to be changed into glass beads.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention
The present invention relates to a method for measuring by X-ray analysis, and particularly to a method for preparing a glass bead specimen suitable for X-ray fluorescence analysis regardless of the composition in analyzing the composition of a ceramic refractory.

[0002]

2. Description of the Related Art Conventionally, a wet chemical analysis method (for example, JIS R 2212 "Chemical analysis method of refractory brick and refractory mortar") has been adopted as a standard analytical method for analyzing the composition of ceramic refractories. I have. However, in this chemical analysis method, it is converted into a water-soluble substance by a method such as adding a reagent and heating and melting, then dissolving in water, filtration, neutralization, dilution, precipitation separation, solvent extraction, liquid separation, The mainstream is wet analysis in which various elemental techniques such as reagent addition, colorimetry, etc. are combined to calculate the amount of contained component metals. For this reason, there are problems that a lot of time is required for the analysis and skill is required to obtain an accurate measurement value.

On the other hand, an X-ray fluorescence analysis method having an advantage that analysis can be performed in a relatively short time with a small number of steps (for example, JIS R 2216 "Method for X-ray fluorescence analysis of refractory brick and refractory mortar") However, it has been used frequently as a simple method. According to this method, a refractory powder to be analyzed is mixed with a lithium borate flux such as lithium tetraborate or lithium metaborate and placed in a platinum container or the like, and then melted in an induction heating furnace to form a glass bead. It is carried out in the procedure of preparing, applying this to a fluorescent X-ray analyzer, determining the relative amounts of the component metals, and calculating the composition.

[0004]

Although the above-mentioned X-ray fluorescence analysis method is simple and gives accurate measurement results, carbon-based components such as graphite cannot be expected to have sufficient accuracy by the X-ray fluorescence analysis method. For this reason, in the case of a sample containing a carbon-based component, a sample that has been oxidized at 1050 ° C. is used as an analysis sample. However, even in an oxidized sample, a metal carbide such as silicon carbide or a free metal such as metal silicon is not completely oxidized, and an unoxidized portion reacts with platinum, making it difficult to form a glass bead. For this reason, the fact is that it is necessary to rely on the above-mentioned chemical analysis which takes time.

The present invention is intended to accurately measure the composition of ceramics containing carbon, metal carbide, or free metal elements by X-ray fluorescence spectroscopy. Irrespective of the composition of, a glass bead used as a specimen for X-ray fluorescence analysis can be safely and easily prepared.
It is an object of the present invention to provide an improved method for preparing a specimen for composition analysis.

[0006]

According to the present invention, there is provided a method for preparing a refractory specimen for X-ray fluorescence analysis which can achieve the above-mentioned object. In preparing, a powder mixture of the ceramic refractory and the lithium borate-based flux is oxidized and melted by indirect heating in a noble metal flat container, and then the melt is uniformly heated by induction heating. It is characterized in that after being made into a melt, it is made into a glass bead to obtain a test specimen for analysis.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION A particularly advantageous ceramic refractory for applying the method for preparing a refractory specimen for X-ray fluorescence analysis of the present invention is JIS R 2216 "Fluorescent X-ray of refractory brick and refractory mortar". As described in "Analysis method", a ceramic refractory containing a carbon component such as free carbon or metal silicon which could not be glass-beaded by a conventional method of preparing a test piece, or metallic silicon And the like, or a ceramic refractory containing a metal carbide component such as silicon carbide. However, the present invention is not limited to these, and it is possible to apply ceramic refractories which can be made into a glass bead by a conventional production method in exactly the same manner.

That is, the method of preparing a refractory specimen for X-ray fluorescence analysis according to the present invention can be performed without any trouble by exactly the same operation, regardless of what component the ceramic contains. Since a glass bead, which is a specimen for analysis, can be prepared, the versatility is higher than that of the conventional method.

As the lithium borate-based flux used in the method of preparing a test piece of the present invention, fluxes such as lithium metaborate and lithium tetraborate can be used. Lithium borate can be more preferably used. The amount of the lithium borate-based flux used for the ceramic refractory to be analyzed is preferably about 10 times in weight.

The heating apparatus used for carrying out the method for preparing a refractory specimen for X-ray fluorescence analysis of the present invention is, for example, an electric furnace equipped with a resistance heating element or the like at about 1100 ° C.
A heating device capable of performing indirect heating to about 200 ° C. and a heating apparatus capable of performing induction heating to about 1200 ° C., such as an electric furnace equipped with an induction coil, are required.

The noble metal container used for melting the mixture of the ceramic refractory and the lithium borate flux is preferably, for example, a flat dish, and its material is strength, heat resistance and peeling off from glass. 5% by weight
It is preferably a platinum alloy containing about gold.

[0012]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to embodiments. Ceramic refractory sample A oxidized at high temperature (1050 ° C)
~ C were prepared. Then, these samples are pulverized until they pass through a 100 μm sieve, 0.4 g is taken, mixed well with 4.0 g of dried lithium metaborate, and made of a platinum alloy containing 5% by weight of gold. In a flat-bottomed evaporating dish with a diameter of 50 mm, it was spread evenly. The thickness of the powder layer at this time is about 7
mm.

Next, a resistance heating type vertical electric furnace having a capacity of 5 kW is preheated to 900 ° C., and the above flat bottom evaporating dish is put therein, the temperature is reset to 1050 ° C., and heating is performed for 30 minutes. Oxidized by air and melted,
A cloudy melt was obtained. Thereafter, the melt was transferred to a 30 mm deep dish made of a platinum alloy containing 5% by weight of gold, and placed in a 3 kW capacity induction heating type vertical electric furnace.
The mixture was completely melted by heating at 150 ° C. for 13 minutes to form a uniform melt, and then cooled to form a glass bead.

Using the glass bead thus obtained, JI
The measurement was performed according to the fluorescent X-ray analysis method described in SR 2216, and the obtained analysis values are shown in Table 1. On the other hand, the analysis values separately obtained by the chemical analysis method (wet method) described in JIS R 2212 for the refractory samples A to C are also shown in Table 1.

[0015]

[Table 1]

According to the above results, according to the method for producing a refractory specimen for X-ray fluorescence analysis of the present invention, a conventional method for producing a glass bead specimen, that is, only using an induction heating type vertical electric furnace. It can be seen that the method can easily obtain a glass-beaded test specimen even with a refractory that cannot be glass-beaded, and thus can obtain an accurate analysis result.

[0017]

According to the method for preparing a refractory specimen for X-ray fluorescence analysis of the present invention, a powder mixture of a ceramic refractory and a lithium borate flux is oxidized and melted by indirect heating, This melt is made into a uniform bead by induction heating and then formed into a glass bead.Even ceramics containing free metals and reducing substances such as carbon are used to form a glass bead. It does not damage the precious metal containers or give errors in the composition analysis results. Therefore, it is possible to easily prepare a glass bead specimen for X-ray fluorescence analysis without considering the composition of the ceramic refractory, and it is possible to obtain an accurate analysis result. Also, for example, in the conventional wet analysis method, six days are required to process one sample, whereas in the fluorescent X-ray analysis method using the present invention, the analysis time is about two days. Is obtained, and the analysis time can be greatly reduced.

Claims (7)

[Claims] When preparing a specimen for performing composition analysis of a ceramic refractory by X-ray fluorescence analysis, an indirect heating of a powder mixture of the ceramic refractory and a lithium borate flux in a noble metal container is performed. A refractory for X-ray fluorescence analysis, wherein the refractory is oxidized and melted, and then the melt is induction-heated to form a uniform melt, which is then beaded to obtain a test specimen for analysis. How to make a specimen. 2. The method for preparing a refractory specimen for X-ray fluorescence analysis according to claim 1, wherein the ceramic refractory contains a carbon component. 3. The method for preparing a refractory specimen for X-ray fluorescence analysis according to claim 2, wherein the carbon component is free carbon. 4. The method for producing a refractory specimen for X-ray fluorescence analysis according to claim 1, wherein the ceramic refractory contains a free metal component. 5. The method for preparing a refractory specimen for X-ray fluorescence analysis according to claim 4, wherein the free metal component is metallic silicon. 6. The method for producing a refractory specimen for X-ray fluorescence analysis according to claim 1, wherein the ceramic refractory contains a metal carbide component. 7. The method for preparing a refractory specimen for X-ray fluorescence analysis according to claim 6, wherein the metal carbide component is silicon carbide.