JP2000338063A - Fluorescent x-ray analyzing apparatus and method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enhance measuring accuracy by sufficiently substituting air of an X-ray passing route with inert gas while reducing measuring cost. SOLUTION: The sample housing space A formed to a container 7 and an X-ray passing route 5 of primary X-rays irradiating a sample and secondary X-rays discharged from the sample are demarated by an X-ray transmitting member 29 and a sample is analyzed on the basis of secondary X-rays. In this fluorescent X-ray analyzing method, inert gas is introduced into the X-ray passing route 5 and the samaple is analyzed in such a state that the X-ray passing route 5 is hemetically closed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray fluorescence analyzer and a method thereof for use in, for example, measuring the content of sulfur contained in crude oil, determining the type of steel, or analyzing the plating composition. .

[0002]

2. Description of the Related Art A conventional X-ray fluorescence spectrometer of this type includes a mounting base on which an X-ray detector and an X-ray generator are mounted, and a sample provided on the periphery of an opening formed on one surface of the mounting base. And a storage container. The mounting base is formed with a space through which primary X-rays emitted from the X-ray generator to the sample and secondary X-rays emitted from the sample pass, that is, an X-ray passage path. Further, the mounting base is formed with a gas introduction hole for introducing an inert gas such as helium or nitrogen into the X-ray passage, so that X-rays can be absorbed by air in the X-ray passage or argon in the air. Prevents measurement interference.

[0003] A sample such as crude oil or steel material is stored in the sample storage container, and the sample is irradiated with primary X-rays from an X-ray generator, and secondary X-rays emitted from the sample are radiated.
The lines are analyzed by an X-ray detector. At this time, an inert gas is continuously introduced from the gas introduction hole into the X-ray passage.

[0004]

However, in the case of the above-mentioned conventional X-ray fluorescence spectrometer, an inert gas is introduced into the X-ray passage through the gas introduction hole at the time of measurement. Since air cannot be sufficiently replaced with inert gas,
There is a problem that measurement accuracy is low. Further, since the inert gas is continuously introduced, there is a problem that the cost is increased.

Accordingly, the present invention has been made in view of the above problems, and
It is an object of the present invention to provide an inexpensive X-ray fluorescence analyzer and a method thereof capable of improving measurement accuracy by sufficiently replacing air in a line passage with an inert gas.

[0006]

According to a first aspect of the present invention, there is provided a fluorescent X-ray analysis method according to the first aspect of the present invention. X of primary X-rays and secondary X-rays emitted from the sample
In the fluorescent X-ray analysis method in which the X-ray passage 5 is partitioned by the X-ray transmitting member 29 and the sample is analyzed based on the secondary X-rays, an inert gas is introduced into the X-ray passage 5, The sample analysis is performed with the line passage 5 closed.

[0007] The X-ray fluorescence spectrometer according to the second aspect of the present invention comprises a container 7 having a housing space A for housing a sample;
An X-ray generator 3 for irradiating the sample with primary X-rays;
An X-ray detector 2 for performing sample analysis based on secondary X-rays emitted from the sample, an X-ray of the accommodation space A and X-rays of both X-rays
In the X-ray fluorescence analyzer 1 having the X-ray transmitting member 29 for dividing the X-ray passage 5, an inert gas is introduced into the X-ray passage 5, and the X-ray passage 5 is sealed. .

Therefore, by closing the X-ray passage 5 for the primary X-ray radiated to the sample and the secondary X-ray emitted from the sample, the flow of air to the outside is eliminated, and the absorption of X-rays by air and Interference due to argon in the air can be prevented. In addition, since the inert gas is sealed in the X-ray passage 5, the sample analysis is performed in the atmosphere of the inert gas, which is very effective in improving the measurement accuracy. In addition, since a certain amount of inert gas is sealed instead of continuously introducing inert gas, the cost is low.

Further, the X-ray fluorescence spectrometer according to the third aspect of the present invention comprises a sample accommodating space A formed in the container 7, a primary X-ray radiated to the sample and a secondary X-ray emitted from the sample. In the X-ray fluorescence analysis method in which the X-ray passage 5 and the X-ray passage 5 are partitioned by the X-ray transmitting member 29 and the sample is analyzed based on the secondary X-ray, the X-ray passage 5 is evacuated to a sample. An analysis is performed.

Therefore, since the X-ray passage 5 is evacuated and the sample analysis is performed in a vacuum atmosphere, the accuracy of measurement can be effectively improved, and no inert gas is used. Become cheap.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION One embodiment of a sulfur analyzer for measuring the content of sulfur contained in crude oil will be described below as an example of an X-ray fluorescence analyzer with reference to FIG. In FIG. 1, reference numeral 1 denotes a sulfur analyzer (fluorescent X-ray analyzer), and a mounting table 4 on which an X-ray detector 2 and a X-ray generator 3 each composed of a proportion counter are mounted.
And a lid 6 mounted on the mounting base 4 and hermetically closing an X-ray passage 5 to be described later, and a sample container 7 provided on the lid 6.

An X-ray detector 2 is mounted on the mounting base 4 in the left-right direction, and grooves 4 formed on both sides of the mounting base 4 are provided.
The ring-shaped gas seal material 8 is attached to each of a. Further, the X-ray generator 3 is mounted on the upper surface of the mounting table 4 inclined rearward via an annular gas seal material 9. Further, a circular concave portion 1 is provided at the center of the front surface of the mounting base 4.
0 is formed, and a through hole 11 having a smaller diameter than the concave portion 10 is formed on the bottom surface of the concave portion 10, and the through hole 11 is located at a detection portion of the X-ray detector 2. A communication hole 12 is formed above the through hole 11, and one end of the communication hole 12 is located at an output portion of the X-ray generator 3, and the other end communicates with the through hole 11.

The cover 6 is inserted into the recess 10 of the mounting base 4 and makes contact therewith. A circular recess 13 is formed in the center of the cover 6, and the bottom of the recess 13 communicates with the through hole 11. A through hole 14 having a smaller diameter than the recess 13 is formed. The X-ray passage 5 is constituted by the through hole 11, the communication hole 12 of the mounting base 4, and the through hole 14 of the lid 6. An annular groove 6a is formed on the peripheral surface on one side of the lid 6, and a gas seal material 8 is mounted in the groove 6a. further,
A flange 15 protrudes from the peripheral surface on the other side of the lid 6, and the flange 15 contacts the front surface of the mounting base 4.

The sample container 7 has a large-diameter projection 16.
And the small-diameter projection 1 formed integrally with the large-diameter projection 16.
7 and a flange 18 formed on the peripheral surface at the boundary between the two projecting portions 16 and 17. A crude oil inlet 19 is formed at the upper part of the end face of the large diameter projecting part 16, and a crude oil outlet 20 is formed at the lower part. The crude oil inlet 19 and the crude oil outlet 20 are located on the vertical center line of the end face. are doing.

A detection channel 21 is formed at the center of the end surface of the small-diameter projecting portion 17, and the crude oil introduction port 19 and the detection channel 21 are formed.
An inlet 22 is formed to communicate with one end of the crude oil outlet port 2.
0 and the other end of the detection flow path 21 communicate with each other to form a lead-out path 23. The sample inlet space A is constituted by the inlet 19, the outlet 20, the detection channel 21, the inlet 22, and the outlet 23.

Further, the small-diameter projecting portion 17 is inserted into the concave portion 13 of the lid 6 and is in contact with the wall surface of the concave portion 13. A ring-shaped oil seal material 25 is mounted on an annular groove 24 formed on the end face of the small diameter projecting portion 17, and a gas seal material 8 is mounted on an annular groove 26 formed on the flange 18. Further, a plurality of bolts 27 penetrating through the flange 15 of the lid 6 and the flange 18 of the sample container 7 are screwed into the screw holes 28 on the front surface of the mount 4, and the mount 4, the lid 6, and the sample container 7 Are integrated by each bolt 27.

An X-ray transmitting member 29 of a metal thin film made of beryllium is interposed between the lid 6 and the small-diameter projecting portion 17 of the sample receiving container 7, and one surface of the X-ray transmitting member 29 is used for storing the sample. The other surface faces the detection channel 21 of the container 7 and the through hole 14 of the X-ray passage 5. The X-ray passage 5 is hermetically sealed by the lid 6, the gas sealing material 8 of the sample container 7, and the X-ray transmitting member 29, and an inert gas such as helium Gas is introduced.

According to this method of filling an inert gas, the sulfur analyzer 1 is inserted into a chamber, and the X-ray passage 5 is evacuated through a pore (not shown) communicating with the X-ray passage 5. Then, helium gas is introduced into the chamber, helium gas is introduced into the X-ray passage 5 through the pores, and the pores are closed with plugs.

Next, a method for analyzing sulfur contained in crude oil will be described. In a state where helium gas is sealed in the X-ray passage 5 of the sulfur analyzer 1, crude oil is introduced from the crude oil introduction port 19 of the sample container 7, and the introduction passage 22 and the detection passage 2
1 and from the crude oil outlet 20 through the outlet 23, while the primary X-ray is directed from the X-ray generator 3 toward the detection channel 21.
Irradiation of X-rays excites the analytical elements in the crude oil to produce secondary X
A line is emitted. The secondary X-rays are analyzed by the X-ray detector 2 based on the ratio between the intensity of the fluorescent X-rays and the intensity of the scattered X-rays,
The content of sulfur contained in the crude oil is measured by the X-ray detector 2.

At this time, since the X-ray passage 5 is sufficiently replaced with helium gas, there is no absorption of X-rays by air or interference by argon gas in air as in the prior art, and high-precision measurement is performed. The result is obtained.

In the above embodiment, the crude oil was used as a sample to measure the sulfur content contained in the crude oil. However, the steel material may be used as a sample to determine the type of the steel material or to analyze the plating composition. . Although helium is used as the inert gas, nitrogen gas may be used. Furthermore, although a metal thin film made of beryllium is used for the X-ray transmitting member 29, a resin film such as polyester may be used, and the X-ray transmitting member 29 may be a member having a good X-ray transmittance. .
Further, although the proportion counter is used as the X-ray detector 2, a solid state detector may be used.

Further, in the case of the above-described embodiment, the sample analysis is performed by enclosing the inert gas in the X-ray passage 5.
The sample analysis may be performed in a state where the line passing path 5 is evacuated. In this case as well, there is no absorption of X-rays by air or interference of measurement by argon in the air, and the measurement accuracy can be effectively improved. Further, since no inert gas is used, the cost is low. However, since the sample accommodating space A is in the atmospheric state when the sample is accommodated, the X-ray transmitting member 29
Has a thickness that does not bend toward the X-ray passage path 5 side.

[0023]

As described above, according to the present invention,
Rather than conducting a sample analysis while introducing an inert gas into the X-ray passage path in the atmosphere, the inert gas is sealed in the X-ray passage path or the X-ray passage path is evacuated to create an inert gas. The sample analysis is performed in the atmosphere of the atmosphere or in the vacuum, so that the flow with the external air can be stopped, and the absorption of X-rays by the air and the obstruction by the argon gas in the air can be eliminated. Can be effectively improved.

[Brief description of the drawings]

FIG. 1 (a) is a cut-away side view of one embodiment of the present invention,
FIG. 2B is a front view of FIG.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Sulfur analyzer (X-ray fluorescence analyzer), 2 ... X-ray detector, 3 ... X-ray generator, 5 ... X-ray passage path, 29 ... X-ray transmission member, A ... Sample accommodation space.

 ────────────────────────────────────────────────── ─── Continued on the front page F term (reference) 2G001 AA01 BA04 CA01 DA01 FA12 FA30 GA01 JA11 JA14 KA01 KA09 LA02 LA04 MA02 MA05 NA08 PA07 PA18 SA01

Claims (3)

[Claims] 1. A sample storage space (A) formed in a container (7).
) And the X-ray passage path (5) of the primary X-ray radiated to the sample and the secondary X-ray emitted from the sample,
In the fluorescent X-ray analysis method in which the sample is analyzed based on the secondary X-ray by partitioning with a X-ray transmitting member (29), an inert gas is introduced into the X-ray passing path (5), (Five
A) performing a sample analysis in a sealed state. 2. A container (7) having an accommodation space (A) for accommodating a sample, and an X-ray for irradiating the sample with primary X-rays.
A radiation generator (3), an X-ray detector (2) for analyzing a sample based on secondary X-rays emitted from the sample, and the accommodation space.
(A) and an X-ray transmissive member (29) for partitioning the X-ray passage path (5) for both X-rays, the X-ray fluorescence analyzer (1) has An X-ray fluorescence analyzer characterized in that an active gas is introduced and the X-ray passage (5) is sealed. 3. A sample storage space (A) formed in a container (7).
) And the X-ray passage path (5) of the primary X-ray radiated to the sample and the secondary X-ray emitted from the sample,
In a fluorescent X-ray analysis method in which the sample is analyzed based on the secondary X-rays, which is partitioned by a ray transmitting member (29), the X-ray passage path (5) is subjected to a vacuum state and the sample analysis is performed. X-ray fluorescence analysis method.