JPS60129651A - Preparation of specimen for fluorescent x-ray analysis - Google Patents

Abstract

PURPOSE:To enhance analytical accuracy by reducing a number of defects on the surface of a specimen and to attain to shorten a preparation time while achieving the reduction in the number of analytical processes, by mixing and crushing a specimen such as an ore or slugs and a binder material in such a state that the mixing ratio of both of them is set to a specific range. CONSTITUTION:In preparing a specimen by mixing a binder material with a specimen for fluorescent X-ray analysis, the binder material is mixed with the specimen in a range of 1/2,000-1/1,000 on a wt. basis while the resulting mixture is crushed and subjected to compression molding to obtain a smooth and homogenous X-ray irradiation surface. At this time, the analytical specimen changes corresponding to the mixing ratio with the binder material and a good result is obtained by bringing the mixing ratio to 1/1,000 or less in order to adjust analytical accuracy to about 0.3-0.4% or less. Therefore, the mixing ratio is well if 1/700 or less, pref., 1/1,000 or less while the mixing ratio of 1/2,100 or more, pref., 1/2,000 or more is an optimum range from the aspect of the generation frequency of a surface defect.

Description

[Detailed Description of the Invention] Lee invented Firefly 2. x, *qq, @Related to the field, in detail, fluorescent X-ray analysis samples of ores, minerals, and slag, and their pie and powder materials are mixed in a tension rod to perform good ;'F, Q analysis. Interested in ways to earn money. 8 Ore 1. Fluorescent X41 for qualitative or intermediate quantitative analysis such as slurry
! Applying the analytical method, , T, , Fe, S i O
2, A I 20.3, Ca0. Qq,Oll,,T
After mixing I, O2, MnO4, S6, etc., we pressurize and mold it into a predetermined shape to obtain a smooth linear irradiation surface. ,be. 2. , For this reason, conventional disc vibration milling, -return milling, etc. are shorter! Finely pulverize to 75 μm or less for as long as 2 to 4 minutes to make a sample with a constant particle size from a wide particle size distribution range.1. .

In addition, there is a sample preparation method outside R4-5 in which briquette flavoring is prepared by press-molding at a constant pressure using a press and used as an analytical sample or material. , ,This method involves adding stearic acid, styrene maleic acid, etc. as a binder material to a ground sample at a weight ratio of about 1/10 of the sample, mixing thoroughly using an isk vibrating mill, etc., and then using a press r&
Due to the process being carried out for a while, there were the following problems: 1, 1.

(1) Accurately weighing the sample and binder material.

Work is necessary! Dederu. , 1.11.4, (2) After pulverization, there is a process of mixing the base binder with the sample. 2-(3) Areas where the sample and binder material are not evenly mixed tend to occur on the X-ray irradiated surface of the sample during analysis, causing measurement errors.

5 to 5 in fluorescent X-ray analysis of general materials, ores, slag, etc.
50 mm block and 1 to 5 mm granular sample to 75 μm
A sample preparation method is used in which stearic acid, styrene maleic acid, etc. is mixed with about 1/10 of the binder material in order to crush and mold into a disk-shaped sample, and then press molding. Mixing tends to vary, and measurement accuracy tends to decrease. On the other hand, if the mixing ratio with the binder material is lowered, the measurement accuracy improves, but the molding accuracy decreases, such as cracks appearing on the disk-shaped surface of the analysis sample, resulting in samples that cannot be measured.

The present invention seeks to overcome these previous drawbacks when preparing X-ray specimens.

The present invention is characterized by mixing the sample and binder material within a specific range and pulverizing the sample in order to obtain a sample that maintains a good shape on the surface of the molded sample and does not reduce analysis accuracy. That is.

The present invention is based on the results of various experimental investigations of the relationship between the shape of the molded sample and the mixing ratio, and the relationship between the mixing ratio of the binder material and analysis (measurement) accuracy, by changing the mixing ratio of the sample and the binder material in stages. This was done based on knowledge.

The present invention will be explained in detail below.

Figure 1 shows the results of investigating the relationship between the shape of the molded sample, especially the frequency of surface defects, by changing the mixing ratio of the sample and the binder material in stages. In other words, the frequency of defects occurring on the surface of the molded sample is 2%, 12%, 4, and 20% at each point where the mixing ratio of the sample and binder material (hereinafter referred to as the ratio of binder material/sample) is 1/2000 weight ratio or less. and the mixing ratio increases to 1.
/2500 weight ratio, it became clear that the frequency of surface defect occurrence increased rapidly to 32%.

Furthermore, sample S! FIG. 2 shows the experimental results of the relationship between the mixing ratio of binder materials and analysis (measurement) accuracy in a typical case of O2, Al□O, and CaO.

In the graphs 1, 2, 3 and 4, the mixing ratio is 1/1, respectively.
0.1/700.1/1000 and 1/3-200 (l is shown, and in the case of SiO2, A I 203 and CaO, when considering the analysis accuracy, the analysis is not possible at the mixing ratio of 1/10 and 1/700 Even for Al2O3, where the error deviation σ (hereinafter referred to as analysis accuracy) is small, it is about 0.4%, and for 5in2, there is a large variation of about 0.4% to 0.8%.'For CaO, it is about 0. .6% to 0.7
The analysis accuracy has a relatively large error of . □ On the other hand, at a mixing ratio of 1/100'0 to 1/2000, Ca
Although the analysis accuracy σ of O is about 0.4%, which is inferior, the analysis accuracy is significantly improved compared to the mixing ratio of 1/10 to 1/700.

The analysis accuracy σ of other ALO1 and 5i02 is extremely good, about 0.2% to 0.3%.

Even when it was added to other components such as S', MnO, T, F''et, etc., the mixture ratio was good within the range of 1/1000 to 1/2000.

As mentioned above, the analysis sample changes depending on the mixing ratio with the binder material, and if the analysis accuracy σ is about 0.3 to 0.4% or less, the mixing ratio is 1/10005-14. = The following will bring about good results.

Therefore, the mixing ratio is 1/700 or less, preferably 1/10.
On the other hand, from the surface defect occurrence frequency, it can be determined that a mixing ratio of 1/2100 or more, preferably 1/2000 or more is a suitable mixing ratio range.

Next, examples will be explained. “Using a disc vibrating mill and a 30-5'OT press,
Fluorescent X-ray analysis samples were press-molded from bulk and granular specimens according to the following procedure. That is, (1) about 50 g of a sample was mixed with 0.0 g of stearic acid. Add '02-0.06'li. (2
) Ink to be charged into the vessel of the vibrating mill (3) 2~ with the vibrating mill
Pulverize for 3 minutes. (4) Remove the fine powder sample from the vessel. (5) Place the fine powder in a metal cup and press-mold at 30T for about 1 minute.

(6) Analyze the sample. Samples prepared using this procedure can obtain a smooth and homogeneous X-ray irradiated surface in about 5 minutes per sample.
The time required for the analysis was significantly reduced by 10 minutes, and the analytical accuracy was almost doubled as shown in Table 1.

Table 1 Analytical accuracy (0%) Sio2 Al2O, CaO Compound method 0.0B 0.04 0.07 method 0.0
3 0.02 0.07 According to the present invention, X
This reduced the number of defects on the surface of line analysis samples, improved analysis accuracy, and reduced the work time and analysis man-hours required for sample preparation.

[Brief explanation of the drawing]

FIG. 1 is a graph showing the relationship between the analysis sample surface defect occurrence frequency and the mixing ratio, and FIG. 2 is a graph showing the relationship between the analysis accuracy and the mixing ratio. In Figure 2, 1 indicates that the amount of binder mixed with the sample is at a chopstick weight ratio, 2 indicates an 11 weight ratio, and 3 indicates a T-
Normal 1 weight ratio, 4 is 7- 1 1 1 1 11500 /1000 /1500 /2000 /
2500 Mixing ratio (binder/sample) SiO2A1□03Ca0

Claims (1)

[Claims] A method of preparing a sample by mixing a binder material with a sample for fluorescent X-ray analysis, the weight ratio of the four samples
1/20 (10 to 1. / j, Q OO,,
After mixing 7 parts of Pai and Ngu wood and crushing 1 part,
Our special equipment section aims to obtain a smooth, homogeneous X-ray irradiation surface using a pressure-sensitive type, and how to prepare samples for fluorescence X-ray analysis.