JP7135582B2 - Capillary holder and X-ray diffraction measurement method - Google Patents

Description

The present invention relates to a capillary holder and an X-ray diffraction measurement method.

An X-ray diffractometer is an analysis device for analyzing the crystal structure of a sample by detecting the diffracted X-rays reflected or transmitted from the sample when the sample is irradiated with X-rays emitted from an X-ray source. and is widely used for non-destructive analysis of various substances.

In the X-ray diffraction measurement of a powder sample, if there is a sufficient amount of sample, the powder sample is placed in the recess in the center of a holder made of flat glass or the like, and the excess sample is scraped off using a flat glass plate. , is repeated until the height of the powder sample becomes the same as the reference surface of the glass holder. Matching the reference plane of the glass holder with the height of the powder sample is important in preventing the angle deviation of the diffraction peak.

However, in this method, depending on the amount of force applied to the glass plate to scrape off the excess powder sample, the powder particles may be aligned in a certain crystal orientation. When such a powder sample is subjected to X-ray diffraction measurement, the intensity of some diffraction peaks is detected to be high, resulting in the influence of particle orientation. In this case, during qualitative analysis, the intensity ratio of the diffraction peaks registered in the referenced crystal structure database (ICDD) may change, causing errors in the original crystal structure analysis and quantitative analysis of the sample.

Therefore, in order to avoid the problem of particle orientation when preparing a powder sample, a method has been proposed in which the powder sample is filled, for example, in a glass capillary, and the X-ray diffraction is measured without orientation (see, for example, Patent Document 1). ).

Specifically, as shown in Patent Document 1, after a small amount of powder sample is introduced into a capillary made of glass with one end sealed, the capillary is vibrated, the powder sample is filled, and the capillary is moved appropriately. Cut to length. After that, in order to fix the cut capillary, it is inserted into a hole provided in a mounting jig (capillary holder) made of metal or the like, and the capillary is fixed in the hole of the mounting jig with an adhesive or the like. It is placed in the sample mounting part of the goniometer of the X-ray diffractometer and measured.

Since the X-ray diffractometer performs measurement while rotating the capillary, if the part of the capillary irradiated with X-rays (measurement part) becomes eccentric with respect to the center of the optical axis of the instrument, the diffraction peak position of the powder sample will shift. will be detected. Therefore, the angle of the capillary is adjusted after the capillary is attached to the mounting jig or after the sample is attached to the sample mounting portion of the apparatus.

JP 2005-291817 A

By the way, in the diffraction pattern obtained by X-ray diffraction measurement, in addition to the diffraction pattern derived from the sample, a halo peak derived from the capillary forming material (for example, glass) is detected, so it is necessary to correct this. be. This correction generally employs a method of subtracting the background. Specifically, an empty capillary that is not filled with a powder sample is measured, and then another capillary of the same material and the same size is filled with the powder sample and subjected to X-ray diffraction measurement. Background correction is performed by removing the former X-ray diffraction pattern from . By this correction, the influence of the halo peak derived from the capillary can be reduced, and the X-ray diffraction pattern of the powder sample can be accurately obtained.

However, even if the capillaries are made of the same material and have the same dimensions, there are individual differences in the wall thickness, outer diameter, and other dimensions due to the manufacturing method. The measurement may change the degree of X-ray absorption. As a result, there are individual differences in the background shape, and the background may not be subtracted well. In other words, correction may not be performed well, and an error may occur in the analysis.

In addition, since a plurality of capillaries are used at least for measurement and correction for measurement of one powder sample, it takes time to adjust the angle of the capillaries and perform measurement. That is, the measurement efficiency becomes low.

In addition, in the method disclosed in Patent Document 1, the vibration generated when the capillary is cut changes the filling state of the powder sample, which causes an error in the analysis, and the sample is scattered around, which impairs environmental safety. Sometimes.

As described above, the X-ray diffraction measurement method using a capillary sometimes lowers analysis accuracy and measurement efficiency.

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a technique for improving analysis accuracy and measurement efficiency in X-ray diffraction measurement using a capillary.

A first aspect of the present invention is
X-ray diffraction of a capillary comprising a tubular portion for filling a powder sample and an outwardly expanding funnel-shaped portion connected to the opening of the tubular portion for introducing the powder sample into the tubular portion. A capillary holder for mounting on a device,
a holder main body;
a hole penetrating in the thickness direction of the holder main body and having an insertion port into which the capillary is inserted and an insertion port into which the tubular portion of the capillary is inserted;
The hole is formed such that the diameter increases from the insertion port toward the insertion port, and when the capillary is inserted into the hole, the tubular portion protrudes from the insertion port. The capillary is fixed by engaging the funnel-shaped portion with the inner peripheral surface of the hole,
A capillary holder is provided.

A second aspect of the present invention provides the capillary holder of the first aspect,
The insertion port has a diameter larger than the diameter of the tubular portion and smaller than the diameter of the funnel-shaped portion, and the insertion port has a diameter larger than the diameter of the funnel-shaped portion.

A third aspect of the present invention is the capillary holder of the first or second aspect,
The hole has a shape similar to the outer shape of the funnel-shaped portion in a cross section in the thickness direction of the holder main body.

A fourth aspect of the present invention is the capillary holder of either the first or second aspect,
The hole has a tapered shape in a cross section in the thickness direction of the holder main body.

A fifth aspect of the present invention is
powder using a capillary having a tubular portion for filling a powder sample and an outwardly expanding funnel-shaped portion connected to an opening of the tubular portion for introducing the powder sample into the tubular portion; A method for performing X-ray diffraction measurements of a sample, comprising:
a holder main body, and an insertion opening into which the capillary is inserted and an insertion opening into which the tubular portion of the capillary is inserted, penetrating through the holder main body in the thickness direction; a preparation step of preparing a capillary holder having a hole formed so that the diameter increases toward the
By inserting the capillary into the hole of the capillary holder, protruding the tubular portion from the insertion opening, and locking the funnel-shaped portion with the inner peripheral surface of the hole, the capillary is a fixing step of fixing the
A method for X-ray diffraction measurement of powder samples is provided.

A sixth aspect of the present invention is the powder sample X-ray diffraction measurement method of the fifth aspect,
The insertion port has a diameter larger than the diameter of the tubular portion and smaller than the diameter of the funnel-shaped portion, and the insertion port has a diameter larger than the diameter of the funnel-shaped portion.

A seventh aspect of the present invention is the powder sample X-ray diffraction measurement method of the fifth or sixth aspect,
The hole has a shape similar to the outer shape of the funnel-shaped portion in a cross section in the thickness direction of the capillary holder.

An eighth aspect of the present invention is the powder sample X-ray diffraction measurement method of the fifth or sixth aspect,
The hole has a tapered shape in a cross section in the thickness direction of the capillary holder.

A ninth aspect of the present invention is the X-ray diffraction measurement method for a powder sample according to any one of the fifth to eighth aspects,
The tubular portion protruding from the insertion port and the peripheral edge portion of the insertion port are fixed with a fixing material.

A tenth aspect of the present invention is the X-ray diffraction measurement method for a powder sample according to any one of the fifth to ninth aspects,
a first measurement step of measuring an X-ray diffraction pattern derived from the capillary by irradiating the tubular portion with X-rays after fixing the capillary to the capillary holder;
a filling step of filling the powder sample into the capillary fixed to the capillary holder;
a second measuring step of measuring an X-ray diffraction pattern derived from the capillary and the powder sample by irradiating the tubular portion filled with the powder sample with X-rays;
and an analysis step of correcting and analyzing the result obtained in the second measurement step with the result obtained in the first measurement step.

According to the present invention, analytical accuracy and measurement efficiency can be improved in X-ray diffraction measurement using a capillary.

FIG. 1 is a schematic cross-sectional view of a capillary holder according to one embodiment of the present invention. FIG. 2 is a diagram for explaining when the capillary is fixed to the capillary holder. FIG. 3 is a schematic cross-sectional view of a capillary holder according to another embodiment of the invention. FIG. 4 is a perspective view for explaining when the capillary is introduced into the X-ray diffraction apparatus. FIG. 5 is a plan view for explaining the positional relationship between the capillary and the optical system. FIG. 6 is a diagram for explaining the irradiation of the capillary with X-rays. FIG. 7 is a perspective view of a capillary.

A capillary is a sample container made of materials such as quartz glass, Lindemann glass, borosilicate glass, soda glass, and the like, and is used for measuring minute amounts of powder samples with an X-ray diffractometer. Specifically, as shown in FIG. 7 , the capillary 20 is connected to a tubular portion 21 closed at one end for filling the powder sample and an opening at the other end of the tubular portion 21 . and an outwardly expanding funnel 22 for introducing the . By supplying the powder sample from the funnel-shaped portion 22 with a large diameter, the powder sample can be introduced into the tubular portion 21 with a small inner diameter (for example, about 0.1 mm), and the capillary 20 can be filled with the powder sample. can.

Conventionally, when performing X-ray diffraction measurement of a powder sample using the capillary 20, the funnel-shaped portion 22 of the capillary 20 is removed by cutting, and only the tubular portion 21 is inserted through the hole of the capillary holder and fixed. rice field. In this case, in order to cut the capillary 20, it was necessary to use a plurality of different capillaries for background measurement and powder sample measurement. As a result, analysis accuracy and measurement efficiency may be lowered.

In view of this, the inventors have investigated a method of fixing the capillary to the X-ray diffraction apparatus without cutting it. As a result, the present inventors have found that a capillary holder for inserting and fixing a capillary should preferably be configured so that the hole can accommodate the funnel-shaped portion of the capillary. As a result, it is possible to insert and fix the capillary into the hole of the capillary holder without cutting the capillary, thereby solving the problems associated with conventional cutting of the capillary. The present invention has been made based on such knowledge of the inventors.

<One embodiment of the present invention>
An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a schematic cross-sectional view of a capillary holder according to one embodiment of the present invention. FIG. 2 is a diagram for explaining when the capillary is fixed to the capillary holder. 1 and 2 show cross sections when the capillary holder 1 is cut in the thickness direction so as to pass through the hole 12. FIG.

(capillary holder)
As shown in FIG. 1, the capillary holder 1 includes a holder main body 11 and a hole 12 penetrating through the holder main body 11 in the thickness direction.

The holder main body 11 is made of, for example, a metal material and configured to be attached to the goniometer head 30 .

A hole 12 is formed in the holder main body 11 so as to penetrate in the thickness direction. The hole 12 is configured so that the capillary 20 can be inserted and fixed. Specifically, the hole portion 12 has an insertion port 12a into which the capillary 20 is inserted on one main surface side of the holder body portion 11, and an insertion port 12b through which the tubular portion 21 of the capillary 20 is inserted on the other main surface side. It has each on the face side. In this embodiment, the hole portion 12 is formed so that the diameter increases from the insertion port 12b toward the insertion port 12a, and when the capillary 20 is inserted, the tubular portion 21 protrudes from the insertion port 12b and has a funnel shape. By engaging the portion 22 with the inner peripheral surface of the hole portion 12, the capillary 20 is fixed. In other words, the hole 12 is configured such that the hole diameter becomes narrower as it moves away from the insertion port 12 a , and the funnel-shaped portion 22 of the capillary 20 is hooked inside the hole 12 .

In the hole portion 12 , the diameters of the insertion port 12 a and the insertion port 12 b are not particularly limited, but the diameter of the insertion port 12 a is larger than the diameter of the funnel-shaped portion 22 , and the diameter of the insertion port 12 b is larger than the diameter of the tubular portion 21 . It is preferably large and smaller than the diameter of the funnel 22 .

The cross-sectional shape of the hole portion 12 in the thickness direction of the holder main body portion 11 is not particularly limited as long as the diameter increases from the insertion port 12b toward the insertion port 12a. The cross-sectional shape of the hole portion 12 may be a shape similar to the outer shape of the funnel-shaped portion 22 of the capillary 20 as shown in FIG. 1, a tapered shape such that the hole diameter continuously changes as shown in FIG. It may be a shape that changes stepwise. From the viewpoint of stably fixing the capillary 20 when the capillary 20 is inserted into the hole 12 , it is preferable that the outer shape of the funnel-shaped portion 22 is similar.

(X-ray diffraction measurement method)
Next, a method of performing X-ray diffraction measurement of a powder sample using the capillary holder 1 described above will be described. The measurement method of this embodiment includes a preparation step of the capillary holder 1, a fixing step of fixing the empty capillary 20 to the capillary holder 1, a first measurement step of performing X-ray diffraction measurement on the empty capillary 20, A filling step of filling the powder sample into the capillary 20, a second measurement step of performing X-ray diffraction measurement on the capillary 20 filled with the powder sample, and analyzing the powder sample based on the results of the first and second measurement steps. and an analysis step.

(Preparation process)
First, the capillary holder 1 described above is prepared.

(fixing process)
Next, an empty capillary 20 is fixed to the capillary holder 1 . Specifically, as shown in FIG. 2, an empty capillary 20 not filled with a powder sample is inserted from the tubular portion 21 side into the insertion port 12a of the capillary holder 1, and the tubular portion 21 is inserted from the insertion port 12b. It protrudes and is inserted until the funnel-shaped part 22 hits the inner peripheral surface of the hole 12 . Thereby, the capillary 20 is inserted and fixed in the capillary holder 1 .

From the viewpoint of stably fixing the capillary 20 to the capillary holder 1, it is preferable to fix the tubular portion 21 protruding from the insertion port 12b and the peripheral edge portion of the insertion port 12b in the holder body portion 11 with the fixing material 13. . As the fixing material 13, for example, any one of wax, adhesive, clay, and heat-shrinkable tube can be used. As the wax and clay, it is preferable to use a material that can be softened and deformed when touched by hand because it is easy to handle. In this case, wax or clay may be provided between the tubular portion 21 and the peripheral portion. The material of the heat-shrinkable tube is not particularly limited, and may be appropriately selected according to the heat resistance of the capillary 20 . When a heat-shrinkable tube is used, the heat-shrinkable tube may be molded into a thin tube and placed between the tubular portion 21 and the peripheral portion before being heated.

(First measurement step)
Next, the capillary holder 1 to which the capillary 20 is fixed is introduced into the X-ray diffractometer, and the X-ray diffraction measurement is performed on the empty capillary 20 not filled with the powder sample. This is for detecting a halo peak derived from the capillary 20 and performing background correction.

Introduction of the capillary 20 into the X-ray diffraction apparatus can be performed as follows.
For example, as shown in FIG. 4, the capillary holder 1 to which the capillary 20 is fixed is attached to the goniometer head 30 . The goniometer head 30 has a hole (not shown) in which the capillary holder 1 is embedded and an angle adjusting stage (not shown) for adjusting the angle of the tubular portion 21 of the capillary 20 . By finely adjusting the position of the angle adjustment stage, the capillary 20 is rotated and the angle of the tubular portion 21 is adjusted so that the X-ray irradiation portion of the capillary 20 is not eccentric during X-ray diffraction measurement.
After adjusting the angle of the tubular portion 21, as shown in FIG. 5, the goniometer head 30 is placed on the sample mounting portion 40 (so-called sample stage) of the goniometer 50 in the X-ray diffractometer, and the capillary 20 is placed in the X-ray diffractometer. to be introduced. The goniometer 50 is provided with a first arm 51 and a second arm 52 . An X-ray source 60 for irradiating the capillary 20 with X-rays is arranged on the first arm 51 , and a detector 70 for detecting diffracted X-rays diffracted by the capillary 20 is arranged on the second arm 52 . are placed. 5 shows a plan view when the goniometer 50 is viewed from the direction in which the tubular portion 21 of the capillary 20 protrudes.

Subsequently, as shown in FIGS. 5 and 6, the X-ray source 60 irradiates the tubular portion 21 with X-rays. Then, X-ray diffraction measurement is performed by relatively changing the positions of the X-ray source 60, the light receiving slit, and the detector 70 with the goniometer 50 so as to maintain the relationship between the incident angle θ and the diffraction angle 2θ. Here, since the tubular portion 21 is not filled with the powder sample, a halo peak derived from the capillary 20 is detected. That is, the X-ray diffraction pattern obtained by this X-ray diffraction measurement contains crystal information of the material (for example, glass) forming the capillary 20 .

(Filling process)
Subsequently, the goniometer head 30 is removed from the sample mounting portion 40 and the capillary holder 1 is removed from the goniometer head 30 . Then, by supplying the powder sample from the funnel-shaped portion 22 to the capillary 20 fixed to the capillary holder 1, the tubular portion 21 is filled with the powder sample. For example, the powder sample is added to the funnel-shaped portion 22 little by little using a spatula or the like, and the powder sample is introduced into the tubular portion 21 by tapping the capillary 20. Repeat until filled. The filling of the powder sample may be performed by removing the capillary 20 from the capillary holder 1 .

(Second measurement step)
Subsequently, the capillary 20 filled with the powder sample is subjected to X-ray diffraction measurement in the same manner as in the first measurement step. Specifically, the capillary holder 1 for fixing the capillary 20 filled with the powder sample is attached to the goniometer head 30, and the angle of the tubular portion 21 is adjusted. Then, the goniometer head 30 is attached to the sample mounting portion 40, and the tubular portion 21 is irradiated with X-rays. Thereby, an X-ray diffraction pattern is obtained. This X-ray diffraction pattern contains crystallographic information of both the material forming the capillary 20 and the powder sample.

(Analysis process)
An analysis of the powder sample is then performed based on the results of the first and second measurement steps. Specifically, the diffraction intensity of the X-ray diffraction pattern derived only from the capillary 20 obtained in the first measurement step is subtracted from the diffraction intensity of the X-ray diffraction pattern obtained in the second measurement step. This treatment yields an X-ray diffraction pattern of only the powder sample. Crystal information of the powder sample is obtained by analyzing this diffraction pattern.

As described above, X-ray diffraction measurement of the powder sample is performed.

In this embodiment, the case where the goniometer head 30 is attached so that the tubular portion 21 of the capillary 20 faces upward has been described. good too. Further, the fixing material 13 may be omitted if the capillary 20 can be stably inserted and fixed in the capillary holder 1, and fixing with the fixing material 13 may be omitted when the capillary 20 is mounted horizontally.

As for the capillary 20, one end of the tubular portion 21 is preferably closed from the viewpoint of preventing the filled powder sample from dropping, but one end of the tubular portion 21 may be opened.

In the above-described embodiment, the case where the capillary holder 1 is attached to the goniometer head 30 and introduced into the X-ray apparatus has been described, but the present invention is not limited to this. For example, after arranging the capillary holder 1 to which the capillary 20 is fixed in the sample mounting portion via an attachment, the angle may be adjusted by the attachment.

<Effects of this embodiment>
According to this embodiment, one or more of the following effects can be obtained.

As described above, the conventional capillary holder is not configured to accommodate the funnel-shaped portion 22 of the capillary 20 in its hole. The X-ray diffraction measurement was performed by fixing. In this case, it is necessary to use different capillaries 20 for the background measurement and the powder sample measurement. Therefore, the decrease in the accuracy of the background correction not only deteriorates the analysis accuracy, but also lowers the measurement efficiency. there were.

In contrast, in the capillary holder 1 of the present embodiment, the hole 12 is formed so that the diameter increases from the insertion port 12b toward the insertion port 12a, and when the capillary 20 is inserted into the hole 12, The capillary 20 can be fixed by protruding the tubular portion 21 from the insertion port 12b and locking the funnel-shaped portion 22 on the inner peripheral surface of the hole portion 12 . According to such a capillary holder 1, the capillary 20 can be introduced into the X-ray diffractometer without removing the funnel-shaped part 22, that is, in a non-destructive manner.

When performing X-ray diffraction measurement of a powder sample using such a capillary holder 1, an X-ray diffraction pattern derived from the capillary 20 is obtained by irradiating the empty capillary 20 with X-rays in the first measurement step. After that, the capillary 20 fixed to the capillary holder 1 is filled with the powder sample, and in the second measurement step, the capillary 20 filled with the powder sample is irradiated with X-rays to Acquire an X-ray diffraction pattern. Then, the X-ray diffraction pattern of the powder sample can be obtained by background-correcting the result obtained in the second measurement step with the result obtained in the first measurement step. By making the capillary 20 non-destructive in this manner, the same capillary 20 can be used for both background measurement and powder sample measurement. Moreover, since the powder sample can be filled while the capillary 20 is fixed to the capillary holder 1, the number of fixing operations of the capillary 20 can be reduced. Therefore, according to the capillary holder 1 of the present embodiment, it is possible to improve the analysis accuracy and measurement efficiency when performing X-ray diffraction measurement on a powder sample.

The insertion port 12b may have a diameter larger than the diameter of the tubular portion 21 and smaller than the diameter of the funnel-shaped portion 22, and the insertion port 12a may have a diameter larger than the diameter of the funnel-shaped portion 22. preferable. By configuring the hole 12 in this way, the capillary 20 can be fixed more stably.

Moreover, the hole portion 12 preferably has a tapered shape in a cross section in the thickness direction of the holder main body portion 11 , and more preferably has a shape similar to the outer shape of the funnel-shaped portion 22 . By having the hole 12 having such a shape, the capillary 20 can be fixed more stably, and the analysis accuracy can be further improved.

Further, it is preferable to fix the tubular portion 21 of the capillary 20 protruding from the insertion port 12b of the capillary holder 1 and the peripheral edge portion of the insertion port 12b with the fixing material 13 . As a result, the capillary 20 can be more stably fixed to the capillary holder 1, and high measurement accuracy can be maintained.

Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments, and can be modified in various ways without departing from the scope of the present invention.

1 capillary holder 11 holder main body 12 hole 12a insertion port 12b insertion port 13 fixing material 20 capillary 21 tubular portion 22 funnel-shaped portion 30 goniometer head 40 sample mounting portion 50 goniometer 51 first arm 52 second arm 60 X-ray source 70 detector

Claims (8)

X-ray diffraction of a capillary comprising a tubular portion for filling a powder sample and an outwardly expanding funnel-shaped portion connected to the opening of the tubular portion for introducing the powder sample into the tubular portion. A capillary holder for mounting on a device,
a holder main body;
a hole penetrating in the thickness direction of the holder main body and having an insertion port into which the capillary is inserted and an insertion port into which the tubular portion of the capillary is inserted;
The hole portion is formed such that the diameter increases from the insertion port toward the insertion port, and has a shape similar to the outer shape of the funnel-shaped portion in a cross section in the thickness direction of the holder main body portion. When the capillary is inserted into the hole, the tubular portion protrudes from the insertion opening and the funnel-shaped portion is engaged with the inner peripheral surface of the hole to fix the capillary. configured to
capillary holder. X-ray diffraction of a capillary comprising a tubular portion for filling a powder sample and an outwardly expanding funnel-shaped portion connected to the opening of the tubular portion for introducing the powder sample into the tubular portion. A capillary holder for mounting on a device,
a holder main body;
a hole penetrating in the thickness direction of the holder main body and having an insertion port into which the capillary is inserted and an insertion port into which the tubular portion of the capillary is inserted;
The hole is formed so that the diameter increases from the insertion port toward the insertion port, and has a tapered shape in a cross section in the thickness direction of the holder main body. The capillary is fixed by causing the tubular portion to protrude from the insertion opening and locking the funnel-shaped portion on the inner peripheral surface of the hole when the capillary is inserted into the
capillary holder. The insertion port has a diameter larger than the diameter of the tubular portion and smaller than the diameter of the funnel-shaped portion, and the insertion port has a diameter larger than the diameter of the funnel-shaped portion.
A capillary holder according to claim 1 or 2 . powder using a capillary having a tubular portion for filling a powder sample and an outwardly expanding funnel-shaped portion connected to an opening of the tubular portion for introducing the powder sample into the tubular portion; A method for performing X-ray diffraction measurements of a sample, comprising:
a holder main body, and an insertion opening into which the capillary is inserted and an insertion opening into which the tubular portion of the capillary is inserted, penetrating through the holder main body in the thickness direction; a preparation step of preparing a capillary holder having a hole formed so that the diameter increases toward the
By inserting the capillary into the hole of the capillary holder, protruding the tubular portion from the insertion opening, and locking the funnel-shaped portion with the inner peripheral surface of the hole, the capillary is a fixing step of fixing the
The hole has a shape similar to the outer shape of the funnel-shaped portion in a cross section in the thickness direction of the capillary holder,
X-ray diffraction measurement method for powder samples. powder using a capillary having a tubular portion for filling a powder sample and an outwardly expanding funnel-shaped portion connected to an opening of the tubular portion for introducing the powder sample into the tubular portion; A method for performing X-ray diffraction measurements of a sample, comprising:
a holder main body, and an insertion opening into which the capillary is inserted and an insertion opening into which the tubular portion of the capillary is inserted, penetrating through the holder main body in the thickness direction; a preparation step of preparing a capillary holder having a hole formed so that the diameter increases toward the
By inserting the capillary into the hole of the capillary holder, protruding the tubular portion from the insertion opening, and locking the funnel-shaped portion with the inner peripheral surface of the hole, the capillary is a fixing step of fixing the
the hole has a tapered shape in a cross section in the thickness direction of the capillary holder,
X-ray diffraction measurement method for powder samples. The insertion port has a diameter larger than the diameter of the tubular portion and smaller than the diameter of the funnel-shaped portion, and the insertion port has a diameter larger than the diameter of the funnel-shaped portion.
The method for X-ray diffraction measurement of the powder sample according to claim 4 or 5 . fixing the tubular portion protruding from the insertion port and the peripheral portion of the insertion port with a fixing material;
An X-ray diffraction measurement method for a powder sample according to any one of claims 4 to 6 . a first measurement step of measuring an X-ray diffraction pattern derived from the capillary by irradiating the tubular portion with X-rays after fixing the capillary to the capillary holder;
a filling step of filling the powder sample into the capillary fixed to the capillary holder;
a second measuring step of measuring an X-ray diffraction pattern derived from the capillary and the powder sample by irradiating the tubular portion filled with the powder sample with X-rays;
an analysis step of correcting and analyzing the result obtained in the second measurement step with the result obtained in the first measurement step;
An X-ray diffraction measurement method for a powder sample according to any one of claims 4 to 7 .

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