GB2165430A - Sample holder jig - Google Patents
Sample holder jig Download PDFInfo
- Publication number
- GB2165430A GB2165430A GB08523871A GB8523871A GB2165430A GB 2165430 A GB2165430 A GB 2165430A GB 08523871 A GB08523871 A GB 08523871A GB 8523871 A GB8523871 A GB 8523871A GB 2165430 A GB2165430 A GB 2165430A
- Authority
- GB
- United Kingdom
- Prior art keywords
- sample holder
- jig
- section
- sample
- recess
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 5
- 238000002441 X-ray diffraction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 47
- 238000000034 method Methods 0.000 description 11
- 239000011521 glass Substances 0.000 description 8
- 238000012856 packing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A jig for use in the preparation of samples for analysis by X-ray diffraction comprises a support block comprising a fixed section and a moveable section 2 connected to the fixed section by means of a screw 3. The fixed section includes a recess 1 for a sample holder 5 which the moveable section 2 locks in position. An optically flat disc 4 fits into the recess and a guide ring 6 fits on top of the sample holder. <IMAGE>
Description
SPECIFICATION
Sample Holder Jig
This invention relates to a jig for use in the preparation of samples for analysis by X-ray diffraction.
The principal factors requiring attention in the preparation of a sample specimen for X-ray diffraction are crystallite or grain size, sample thickness, preferred orientation and sample surface planarity. Adequate crystallite size ( < 10 micron) is normally obtained by grinding which ensures that the number of crystallites contributing to each reflection is sufficiently large to generate signals of reproducible intensity. Grinding also reduces preferred orientation due to crystal habit or shape.
"Preferred orientation" is a term of art and can be definedas uniform alignment of corresponding planes of crystals. In the context of the present invention, despite the terminology, it is not the desired configuration.
Sample thickness is dealt with by providing an adequate depth of recess in the sample holder (approximately 2 mm).
Sample loading precedure is important for further
reducing the preferred orientation and at the same time obtaining good planarity of the sample surface.
It can ensure even distribution and uniform packing density of sample material in the sample holder and, in general, provides a uniform mounting technique so that the intensities of reflections from materials
prone to preferred orientation are more
reproducible. A favoured method is to fill the sample holder from the back.
Previous sample holders were of a simple
rectangular design and were easy to back load.
Recently a new automated system has been introduced (Phillips PW 1710) which requires the use of a more complex circular two piece sample
holder which is not so readily adaptable to back
loading.
We have now devised a jig which enables such sample holders to be back filled with ease and
precision.
Thus according to the present invention, there is
provided a jig for retaining a sample holder in
position, the jig comprising:
(a) a support block comprising a fixed section and a moveable section adjustably connected to the fixed section by means of a screw-threaded clamp
passing loosely through the moveable section and screwing into the fixed section; the fixed section
including a recess adapted to receive a sample
holder and the moveable section being adapted in conjunction with the recess to lock the sample
holder in position,
(b) an optically flat disc adapted to fit into the
recess, and
(c) a guide ring adapted to fit on top of the sample
holder.
Preferably a compresspon spring is fitted on to
the screw section of the clamp between the fixed
and moveable sections so that the two sections are
biassed apart.
Preferably the sample holder is circular.
The jig is primarily designed for a back loading procedure which involves sieving sample material into the sample holder. This disperses the sample
material evenly over the flat disc surface and enables the sample holder cavity to fill uniformly and in such a way that the individual particles, whilst supporting one another, maintain a random orientation of the crystallites. The cavity of the sample holder is slightly over4illed and then the excess tamped down gently with the edge of a glass slide or spatula. This causes the cavity to fill with a minimum amount of flow at the disc face.
The above procedure ensures a uniform packing density of sample material in the sample holder.
When the flat disc is eventually removed the cavity is left filled with a self-supporting layer of sample with reduced preferred orientation and good surface planarity.
It should be mentioned that the reduction of preferred orientation results in a more accurate and representative X-ray pattern being obtained and one that is more amenable for both qualitive and quantitative analysis. Overall, the jig enables samples to be prepared in a uniform and standard manner, and in such a way that the results are reproducible.
An alternative method which minimizes preferred orientation uses serrated sample surface where the particles are likely to be even more randomly oriented. This can be achieved either by chopping the surface with a fine blade or alternatively using a grooved mould. The former method, which avoids sticking of the sample material to the mould, is preferred for use with the jig.
A simple disc attachment enables a protruding surface layer of sample to be obtained for the serration procedure. This technique may have application in special cases, for example in the analysis of clays, san'dstone minerals and zeolites.
The jig may also be used in a front loading procedure and in this case the flat disc is retained as a packing plate only.
The invention is illustrated with reference to the accompanying drawings in which Figure lisa plan of the jig containing a sample holder and Figures 2 and 3 are elevations.
The jig is rectangular in shape but has a circular recess (1 ) to support a circular sample holder. The right hand section (2) of the jig is capable of horizontal movement so that by rotating an attached spring loaded clamping knob (3), the sample holder or any part of it can be locked in position in the recess.
The jig incorporates an optically flat glass disc (4) of similar diameter to the sample holder and its location underneath the holder is shown in Figure 2.
The jig is used in the following manner: Back Loading Procedure
The glass disc (4) is initially placed in the circular recess of the jig and then the front plate (5) of the holder is placed on top with the reverse side uppermost, Figure 1. These two are then clamped together in the jig. An additional guide ring (6) is next placed on top of the front plate (5) and sample material sieved through a 100 mesh sieve (7) into the sample holder cavity Figure 2. The guide ring (6) helps to confine the sample material to the cavity area and is removed once sufficient sample has been sieved. In this respect sample material is allowed to slightly overfill the cavity and is then subsequently gently pressed down with a glass slide. The back plate (8) of the sample holder is then pressed into position on to the front plate (5), Figure 3. Two bull-dog clips are fastened either side of the sample holder and glass disc and the whole released from the jig and turned over so that the glass disc (4) is now uppermost. Both the clips and glass disc (4) are then removed to leave the sample holder in correct orientation for analysis.
Front Loading Procedure
The two sections (5) and (8) of the sample holder are pressed together and clamped in the jig with the front section (5) uppermost. The glass disc (4)ris also used but only as a packing piece underneath the holder. The sample cavity is now filled directly from the top using the sieve (7) and guide ring (6) and the sample material levelled and pressed down with a glass slide to obtain a flat surface. The sample holder is then released from the jig for analysis of the sample.
Claims (4)
1. A jig for retaining a sample holder in position, the jig comprising:
(a) a support block comprising a fixed section and a moveable section adjustably connected to the fixed section by means of a screw-threaded clamp passing loosely through the moveable section and screwing into the fixed section; the fixed section including a recess adapted to receive a sample holder and the moveable section being adapted in conjunction with the recess to lock the sample holder in position,
(b) an optically flat disc adapted to fit into the recess, and
(c) a guide ring adapted to fit on top of the sample holder.
2. A jig according to claim 1 wherein a compression spring is fitted on to the screw section of the clamp between the fixed and moveable sections so that the two section are biassed apart.
3. A jig according to either of the preceding claims wherein the sample holder is circular.
4. A jig is hereinbefore described with reference to
Figures 1-3 of the accompanying drawings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB08523871A GB2165430B (en) | 1984-10-05 | 1985-09-27 | Sample holder jig |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB848425267A GB8425267D0 (en) | 1984-10-05 | 1984-10-05 | Sample holder jig |
| GB08523871A GB2165430B (en) | 1984-10-05 | 1985-09-27 | Sample holder jig |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB8523871D0 GB8523871D0 (en) | 1985-10-30 |
| GB2165430A true GB2165430A (en) | 1986-04-09 |
| GB2165430B GB2165430B (en) | 1987-11-25 |
Family
ID=26288311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB08523871A Expired GB2165430B (en) | 1984-10-05 | 1985-09-27 | Sample holder jig |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2165430B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009007636A1 (en) * | 2009-01-12 | 2010-07-15 | Raumplus Gmbh & Co. Kg | Profile system for a sliding door |
| CN104020027A (en) * | 2014-06-06 | 2014-09-03 | 酒泉钢铁(集团)有限责任公司 | A kind of D8-Advance diffractometer sample holder and using method thereof |
-
1985
- 1985-09-27 GB GB08523871A patent/GB2165430B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009007636A1 (en) * | 2009-01-12 | 2010-07-15 | Raumplus Gmbh & Co. Kg | Profile system for a sliding door |
| CN104020027A (en) * | 2014-06-06 | 2014-09-03 | 酒泉钢铁(集团)有限责任公司 | A kind of D8-Advance diffractometer sample holder and using method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| GB8523871D0 (en) | 1985-10-30 |
| GB2165430B (en) | 1987-11-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |