JPH01105146A - Vessel for liquid sample of fluorescent x-ray analysis apparatus - Google Patents

Abstract

PURPOSE:To improve the accuracy of detection in the case in which the volume of a sample is small by providing a 1st sample chamber for housing the sample of a small volume to a central part and providing concentrical 2nd and 3rd sample chambers for housing the samples of a large volume to the outside. CONSTITUTION:The title vessel V is formed of a plastic material to a bottomed circular cylindrical shape. The 1st sample chamber 1 sized about 15mm in diameter is provided to the central part thereof and the 2nd and 3rd sample chambers are provided concentrically via a partition wall 6 to the outside thereof. Grooves 5 of about 1mm depth are provided the wall 6 between the chambers 2 partitioned by partition walls 4 and the chamber 1. The sample of the small volume is passed in the chamber 1 in the case of measuring said sample and the sample of the large volume is passed in the chamber 1 and the chambers 2 through the grooves 5 in the case of measuring said sample, by which the samples are respectively packed in both the chambers. Measurement is, therefore, carried out with the sample of the small volume by lowering the height of the chamber 1 and the chambers 2 and the waving motion by a thin high-polymer film for preventing splashing is blocked by the walls 4, 6 by which the accuracy is improved.

Description

DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to a liquid sample container for a fluorescence X-ray analyzer. More specifically, it is used when performing elemental analysis in solution samples using characteristic X, II (fluorescence X-rays) generated under strong primary X-ray irradiation, especially for samples with a small amount of sample. The present invention relates to a liquid sample container that can be used effectively.

(Prior art) When measuring a liquid sample using a fluorescence X-ray analyzer, the liquid sample to be measured is coated with a thin polymer film such as polypropylene or polyethylene terephthalate on the upper window of a container made of resin such as polyfluoroethylene. It is used by being sealed in a sealed container and fixed with metal fittings.

This type of liquid sample container is designed to have a large internal volume in order to increase the detection intensity of characteristic X-rays. Therefore, 5 usually a sample amount, for example 20 g, is required to sufficiently fill a liquid sample container for measurement. Since this type of container is expensive, it is cleaned and reused for repeated measurements.

However, the above-mentioned containers for liquid samples have problems such as inability to measure small amounts of samples, such as samples for which a sufficient amount cannot be secured as a measurement sample, and poor measurement efficiency due to the necessity of cleaning the container. There is.

An improved method for measuring a small amount of sample is the drip filter method, in which the sample is dropped onto a filter paper (Japanese Patent Laid-Open No. 59-5
Publication No. 8344).

In this drip filter paper method, a streak (e.g. circular shape) is applied to the filter paper using a water-repellent substance (paraffin, wax, etc.), a sample is dripped into a plane surrounded by the streak, and the sample is surrounded by the streak.・Alternatively, leave the part connected to the filter paper and make a circular incision through the hole, attach paraffin or wax to the connection part, and then make a circular incision. There are methods that allow the sample to be dropped into a plane surrounded by a through hole.

However, with this drip filter paper method, it is possible to improve the detection intensity by repeating dripping and drying the sample in the case of an aqueous sample, but it is possible to improve the detection intensity by repeating dripping and drying of the sample in the case of an aqueous sample. In the case of a sample that dissolves the titration, the number of titrations is limited to one, making it impossible to improve the detection intensity, resulting in poor fluorescence X-ray analysis accuracy and lack of reliability. Furthermore, as described above, in the case of an aqueous solution sample, the sample must be repeatedly dripped and dried, which poses difficulties in preparing the measurement sample.

(Problems to be Solved by the Invention) The present invention was made in view of the above-mentioned drawbacks of liquid sample containers used in fluorescence X-ray analyzers, and is effective even for samples with a small amount of sample. The object of the present invention is to provide a liquid sample container that can be used for various purposes.

[Structure of the invention]

(Means for Solving the Problems) To summarize the present invention, the first invention of the present invention is that
In a cylindrical liquid sample container with one end open and the other end bottomed, of a line analyzer, - a concentric first sample chamber for accommodating a small sample amount in the center; - the above-mentioned. A concentric second sample chamber for accommodating a large amount of sample separated by a desired number of partition walls is provided outside the first sample chamber; and a first sample chamber on the open side. This invention relates to a container for a liquid sample of a fluorescent X-ray analyzer, characterized in that a groove is provided in the upper part of the container to allow liquid to flow into each chamber of a second sample chamber partitioned by a partition wall. relates to a liquid sample container for a fluorescence X-ray analyzer, characterized in that a concentric third chamber is provided outside the second sample chamber of the first invention to receive an overflow of the sample. It is something.

The structure of the liquid sample container of the fluorescence X-ray analyzer of the present invention will be explained in detail based on the drawings.

FIG. 1 is a plan view of a liquid sample container used in the fluorescence X-ray analyzer of the present invention, and FIG. 2 is a sectional view taken along line A-A' in FIG.

FIG. 3 shows a sectional view of a liquid sample container of the present invention mounted on a holder, and FIG. 4 shows a sectional view of a conventional liquid sample container mounted on a holder.

As shown in FIGS. 1 and 2, the liquid sample container (V) of the present invention is manufactured from a plastic material such as polyolefin resin, and has an outer diameter of 50 nm and a height of 1.
It is a cylindrical shape with a bottom of about 5 m, and there are 3 concentric circles within the cylinder.
It was constructed to have two rooms.

In other words, there is a concentric first sample chamber (2) in the center of which accommodates a small amount of sample with a diameter of about 15 m, and a concentric circle with a diameter of about 301 mm outside of the first sample chamber (2) that accommodates a large amount of sample. 2nd sample chamber ■.

Furthermore, a concentric third chamber (2) is located outside the second sample chamber,
Each one has a partition wall about the thickness of one cabinet. The second sample chamber (■) is partitioned by four partition walls (support plates) with a thickness of about 1 m+a at 90° intervals, and the first sample chamber (■) is partitioned by four partition walls (support plates) (from the partition walls). Second
A groove (2) is provided in the upper part of the partition wall constituting the first sample chamber (2) so that the sample chambers can communicate with each other when the first sample chamber (2) is filled with sample liquid.

The height of the first sample chamber and the second sample chamber ■ is 1.5~
It is said that the groove is about 3 cm deep, and the depth of the groove is about 1 kaku.

It is considered a degree. Further, as shown in FIG. 2, the upper surfaces of the partition walls 0 and the partition walls constituting each chamber are configured to be flush with each other.

The liquid sample container (V
) is used in the following manner.

First, when measuring a small amount of sample, it is sufficient to fill the first sample chamber (2) with the sample.

In addition, when measuring a relatively large amount of sample, it is recommended to use the first sample chamber ■ and the second sample chamber ■ by passing the liquid through groove 0 and filling both chambers with the sample. good.

Although it is a sample with a small amount of sample, the volume of the first and second sample chambers of the liquid sample container (V) of the present invention is small compared to the conventional one (Fig. 4). It goes without saying that even in the case of a small sample, it is not necessary to use only the first sample chamber (2), but the second sample chamber (2) may be used.

In any case, the sample is dropped into the first sample chamber (2) and the second sample chamber (2) until they are full. At that time, the sample may overflow into the third chamber (■), and as shown in Figure 4,
During sample measurement, a thin polymer film made of polyolefin or the like is pasted to prevent the sample from scattering during irradiation with fluorescent X-rays and from contaminating the measurement equipment due to the sample scattering. Note that if the sample solidifies easily or is highly viscous, a thin film may not be used.

The liquid sample container (V) of the present invention has the first
The sample chamber and the second sample chamber ■ are characterized by their low height and small volume, which causes the liquid surface of the sample, that is, the thin film, to easily cause waving motion when irradiated with fluorescent X-rays. Become. However, this waving motion is effectively prevented by the partition wall 0 of each room (partition wall 0), especially the latter partition wall 0), so that the accuracy of analysis can be improved.

The structure of the liquid sample container of the present invention has been described above based on FIGS. 1 and 2, but it goes without saying that the structure is not limited to what is shown in the figures unless it goes beyond the gist of the present invention.

(Example) Next, the liquid sample container of the fluorescence X-ray analyzer of the present invention and the analysis accuracy when using the same will be described together with comparative examples.

(i) Liquid sample container A polypropylene container having the shape shown in FIGS. 1 and 2 was used as the liquid sample container.

That is, the inner diameter of the first sample chamber (2) is 15 m5. The inner diameter of the second sample chamber (■) is 30 m, the inner diameter of the third chamber (■) is 48 m, and the
．． The height of the second sample chamber is 211Im, and the height of the third chamber is 7Im.
m was used. Further, the depth of the groove (in the groove) was 1 pupil, and the thickness of each partition wall (0) and the partition wall (in the partition wall) was 1 m.

For comparison, drip filter paper and a conventional container shown in FIG. 4 were used.

(n) Measurement System System 3070 manufactured by Rigaku Denki Kogyo Co., Ltd. was used as a fluorescence X-ray analyzer. In addition, as a measurement sample, VGO (
The Ni content and 7 min contained in the sample were measured using vacuum gas oil (Note).

A low-concentration sample and a high-concentration sample were used).

(jii) Results The results are shown in Tables 1 and 2 below.

In Tables 1 and 2, the variable variable (dispersion) is the value obtained by dividing the standard deviation of the analytical values measured several times (3 to 5 times) by the average value.
It is multiplied by O.

・Chemical analysis value indicates the basic data of analysis obtained by atomic absorption spectrophotometry.

Atomic absorption spectrometry is a method of determining the concentration of a target element in an aqueous solution sample by comparing the absorbance of the target element with a standard sample, and is often used as basic data for comparison in the analytical field.

・Analysis value indicates the value obtained when a liquid sample container is filled with a sample and one analysis is performed using a fluorescence X-ray analyzer (unit: vt)
PP-).

As shown in Table 1 (results for Ni) and Table 2 (results for V), the coefficient of variation (dispersion) in the drip filter method of the comparative example
However, the container of the present invention also has a small coefficient of variation (it can be seen that the analytical accuracy equivalent to that of the conventional holder is obtained).

Furthermore, the average value of the container of the present invention also agrees well with the chemical analysis value, indicating that it is a highly reliable container.

(The following is a blank space) [Effects of the Invention] The liquid sample container of the fluorescence X-ray analyzer of the present invention has the following excellent effects; (i) When the sample amount is small; It also has a structure that allows for improved detection strength.

(n) The container itself can be easily and inexpensively manufactured by molding polyolefin resin or the like.

Therefore, from the viewpoint of complexity of analysis work and analysis accuracy, the container can be made disposable.

(Of course, it can be reused if washed thoroughly) (■)
Preparation of a measurement sample into a container can be easily carried out using a dropping method.

[Brief explanation of the drawing]

FIG. 1 is a plan view of a liquid sample container of the fluorescence X-ray analyzer of the present invention, and FIG. 2 is a sectional view taken along the line A-A' in FIG. FIG. 3 is a sectional view of a liquid sample container of the present invention mounted on a holder, and FIG. 4 is a sectional view of a conventional liquid sample container mounted on a holder. ■... Liquid sample container 1... First sample chamber 2.
...Second sample chamber 3...Third chamber 4...Partition wall (support plate) 5...Groove 6...Partition wall Patent applicant Petroleum Industry Revitalization Center Foundation
Fuji Electric Co., Ltd. Toa Fuel Industry Co., Ltd. Representative Patent Attorney Yoshio Mizuno Figure 1 Figure 2 Figure 3 Figure 4 (Conventional liquid sample container)

Claims (1)

[Scope of Claims] 1. In a cylindrical liquid sample container with one end open and the other end bottomed, for a fluorescence - A concentric second sample chamber for accommodating a large sample volume partitioned by a desired number of partition walls is provided outside the first sample chamber; and a fluorescence X-ray analyzer for liquid samples, characterized in that grooves are provided in the upper part of the first sample chamber on the opening side to allow liquid to pass through each chamber of the second sample chamber partitioned by a partition wall. container. 2. In a cylindrical liquid sample container with one end open and the other end bottomed in a fluorescence X-ray analyzer, a concentric first sample is placed in the center to accommodate a small sample amount a concentric second sample chamber for accommodating a large amount of sample separated by a desired number of partition walls outside the first sample chamber; - the second sample A concentric third chamber is provided outside the chamber to receive the overflow of the sample, and each chamber of the second sample chamber is partitioned by a desired number of partitions above the first sample chamber on the opening side. A liquid sample container for a fluorescent X-ray analyzer, characterized by having a groove for allowing liquid to pass through.