US3307036A - Sample carrier with adhesive tape for the analysis of powders by means of a guinier x-ray camera - Google Patents

Sample carrier with adhesive tape for the analysis of powders by means of a guinier x-ray camera Download PDF

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US3307036A
US3307036A US325972A US32597263A US3307036A US 3307036 A US3307036 A US 3307036A US 325972 A US325972 A US 325972A US 32597263 A US32597263 A US 32597263A US 3307036 A US3307036 A US 3307036A
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ray
frame
window
sample carrier
opening
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US325972A
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Bouvelle Georges
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European Atomic Energy Community Euratom
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European Atomic Energy Community Euratom
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    • 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

Definitions

  • the present invention intends to improve and facilitate the preparation of the diffraction analysis of several powder samples by a Guinier X-ray camera.
  • the invention stems from two existing types of sample carriers the features of which consist in that the analysis window is integral with the base support of the sample carrier and in that the window has markings thereon determining the limits between which the three powders to be analyzed are deposited on the adhesive strip.
  • the strip is retained by a frame secured to the base support by means of four screws.
  • This type of sample carrier is used for transmission analysis as well as reflection analysis.
  • the sample carrier of the invention which has a known rectangular frame as a base support, answers these requirements. It is characterized by the provision of an experimentation frame capable of being removably secured on the base support and provided with two window partitioning bars dividing the free space of the frame into three separate areas, the frame serving, at the same time, to receive the adhesive strip.
  • the operator may have an array of different types of experimentation frames (transmission, reflection) and may thus prepare the samples without having to tie up the base supports themselves.
  • FIG. 1 is a plan view of the base support of the sample carrier of the invention
  • FIG. 2 is a longitudinal cross-sectional view along line 22 of FIG. 1;
  • FIG. 3 is a plan view of the experimentation frame of the sample carrier
  • FIG. 4 is a plan view of the complete sample carrier according to the invention.
  • FIGURE 5 is a schematic elevation view of a known apparatus for the X-ray diffraction analysis of powder samples and with which the sample carrier of the invention is used;
  • FIGURE 6 is a cross-sectional view of the Guinier X-ray camera, taken along line VIVI of FIGURE 5.
  • the base support of the sample carrier is formed as a rectangular frame 1 provided with lateral shoulders 2, forward chamfered abutments 3, a hole 4 for the securement of a clamping member 5 (see FIG. 4) at the rear end thereof and an opening 6 for the passage of X-rays through the center of the support.
  • the experimentation frame 7 (see FIG. 3) is adapted to be releasably secured on the base support 1 and provided with window bars 8 dividing the opening of the frame into separate areas 9.
  • the securement of the frame on the support is obtained by means of the cooperating shoulders 2 and eccentric clamp 5, as illustrated in FIG. 4.
  • the clamp may be operated by means of a wing key.
  • Grooves 10 on the experimentation frame according to FIG. 3 are used for cutting the adhesive strip which is disposed over the upper face of the frame.
  • FIG. 4 illustrates the operating cam or eccentric clamp 5, rotating into its initial clamping position and locking the experimentation frame 7 on the base support 1.
  • the angle of inclination of the conical edge of the clamping cam is 60 and so is that of the chamfered edges of the experimentation frame.
  • the base sup-port being made of brass
  • the experimentation frame is made of stainless steel.
  • Two similar frames have been provided, one for the transmission analysis and the other for the reflection analysis.
  • the two frames only differ in the length of the windows; besides, they are symmetrical in order to avoid the necessity of an adjustment.
  • the sample carrier of the invention is to be used on a known apparatus for the X-ray refraction analysis of powder samples as shown in FIGURES 5 and 6.
  • This apparatus comprises a Guinier camera 11 mounted on a tripod 12 provided with levelling means 13.
  • Camera 11 has a main body 14 fast with a ring 15 slidably mounted on a disk 16, the latter being secured to the tripod 12.
  • the camera body 14 defines a pair of exposure chambers 17 and, for each chamber 17, a plurality of Xray windows 18 leading into said chamber.
  • the films 19 are themselves retained in the exposure chambers by means of resilient split rings 20.
  • the sample carrier denoted in FIGURES 5 and 6 by the capital letter C, are held against the camera by any known means such as the slideways 21 and so positioned that the openings 6 through the base support 1 for the passage of X-rays corresponds to the X-ray window 18 against which the sample carrier is applied.
  • the source of X-rays is from a generator 22 having an emitter head 23.
  • the rays from head 23 are diverted by means of rotating crystal 24.
  • a linear X-ray camera having a main body defining a film exposure chamber and an X-ray window leading into said chamber;
  • a sample carrier as claimed in claim 3, wherein the inner faces of said shoulders in relation to said opening are outwardly and downwardly inclined and the four edges of said experimentation frame are correspondingly inclined, and wherein said means is an eccentric rotatable disc mounted on the fourth edge of said base support; the peripheral face of said disc being so chamfered and positioned in relation to the adjacent inclined edge of said frame as to cause the said frame to move between the guiding shoulders and to abut the abutment shoulder and to be clamped to said base support.

Description

Feb. 28, 1967 G. BOUVELLE 3,307,036
SAMPLE CARRIER WITH ADHESIVE TAPE FOR THE ANALYSIS OF POWDERS BY MEANS OF A GUINIER X-RAY CAMERA Filed Nov. 26, 1963 2 Sheets-Sheet 1 INVENTOK Georges BOUVELLE A TTORNEYS G. BOUVELLE [H ADHESIVE TAPE FOR THE ANALYSIS Feb. 28, 1967 SAMPLE CARRIER WI 0F POWDERS BY MEANS OF A GUINIER X-RAY CAMERA Filed Nov. 26, 1963 2 Sheets-Sheet 2 INVENTOR Georges BOUVELLE ATTORNEY United States Patent C) SAMPLE CARRiER WITH ADHESIVE TAPE FOR THE ANALYSIS OF POWDERS BY MEANS OF A GUIWEER X-RAY CAMERA Georges Bouveile, Olginasio di Besozzo, Varese, Italy, assignor to European Atomic Energy Community- Euratom, Brussels, Belgium Filed Nov. 26, 1963, Ser. No. 325,972
Claims priority, application Belgium, Dec. 11, 1962,
Claims. (a. 2s0 s1.s
The present invention intends to improve and facilitate the preparation of the diffraction analysis of several powder samples by a Guinier X-ray camera.
The invention stems from two existing types of sample carriers the features of which consist in that the analysis window is integral with the base support of the sample carrier and in that the window has markings thereon determining the limits between which the three powders to be analyzed are deposited on the adhesive strip. The strip is retained by a frame secured to the base support by means of four screws.
This type of sample carrier is used for transmission analysis as well as reflection analysis.
In using these sample carriers, it appeared desirable to have available a carrier wherein the separation between the powders would be more definite and clear and, more important still, a carrier wherein the window and the base support would operate independently.
The sample carrier of the invention, which has a known rectangular frame as a base support, answers these requirements. It is characterized by the provision of an experimentation frame capable of being removably secured on the base support and provided with two window partitioning bars dividing the free space of the frame into three separate areas, the frame serving, at the same time, to receive the adhesive strip.
The sample carrier of the instant invention has the following advantages:
(1) Depositing of the various powders is made easier by the partitioning eifect of the bars. There is no danger of mixing the powders to be analysed. The bars being in the optical path of the inner diaphragms of the Guinier camera, they do not influence the X-ray beam.
(2) The experimentation frame with its partitioning bars is inedependent, that is, separable from the base support of the sample carrier.
(3) The adhesive strip, with its powders to be analysed, is glued on the experimentation frame and no longer on the base support. The frame may consequently be preserved as is for a further analysis.
(4) The operator may have an array of different types of experimentation frames (transmission, reflection) and may thus prepare the samples without having to tie up the base supports themselves.
The invention will be better understood by the description that follows of a preferred, although non-limitative, embodiment of the invention having reference to the appended drawings wherein:
FIG. 1 is a plan view of the base support of the sample carrier of the invention;
FIG. 2 is a longitudinal cross-sectional view along line 22 of FIG. 1;
FIG. 3 is a plan view of the experimentation frame of the sample carrier;
FIG. 4 is a plan view of the complete sample carrier according to the invention.
FIGURE 5 is a schematic elevation view of a known apparatus for the X-ray diffraction analysis of powder samples and with which the sample carrier of the invention is used;
FIGURE 6 is a cross-sectional view of the Guinier X-ray camera, taken along line VIVI of FIGURE 5.
In FIGS. 1 and 2, the base support of the sample carrier is formed as a rectangular frame 1 provided with lateral shoulders 2, forward chamfered abutments 3, a hole 4 for the securement of a clamping member 5 (see FIG. 4) at the rear end thereof and an opening 6 for the passage of X-rays through the center of the support.
According to the invention, the experimentation frame 7 (see FIG. 3) is adapted to be releasably secured on the base support 1 and provided with window bars 8 dividing the opening of the frame into separate areas 9. The securement of the frame on the support is obtained by means of the cooperating shoulders 2 and eccentric clamp 5, as illustrated in FIG. 4. The clamp may be operated by means of a wing key.
Grooves 10 on the experimentation frame according to FIG. 3 are used for cutting the adhesive strip which is disposed over the upper face of the frame.
FIG. 4 illustrates the operating cam or eccentric clamp 5, rotating into its initial clamping position and locking the experimentation frame 7 on the base support 1. The angle of inclination of the conical edge of the clamping cam is 60 and so is that of the chamfered edges of the experimentation frame.
The base sup-port being made of brass, the experimentation frame is made of stainless steel. Two similar frames have been provided, one for the transmission analysis and the other for the reflection analysis. The two frames only differ in the length of the windows; besides, they are symmetrical in order to avoid the necessity of an adjustment.
The sample carrier of the invention is to be used on a known apparatus for the X-ray refraction analysis of powder samples as shown in FIGURES 5 and 6.
This apparatus comprises a Guinier camera 11 mounted on a tripod 12 provided with levelling means 13. Camera 11 has a main body 14 fast with a ring 15 slidably mounted on a disk 16, the latter being secured to the tripod 12. The camera body 14 defines a pair of exposure chambers 17 and, for each chamber 17, a plurality of Xray windows 18 leading into said chamber. The films 19 are themselves retained in the exposure chambers by means of resilient split rings 20.
The sample carrier, denoted in FIGURES 5 and 6 by the capital letter C, are held against the camera by any known means such as the slideways 21 and so positioned that the openings 6 through the base support 1 for the passage of X-rays corresponds to the X-ray window 18 against which the sample carrier is applied.
The source of X-rays is from a generator 22 having an emitter head 23. The rays from head 23 are diverted by means of rotating crystal 24.
I claim:
1. In an apparatus for the X-ray diffraction analysis of powder samples, the combination comprising:
(I) a linear X-ray camera having a main body defining a film exposure chamber and an X-ray leading into said chamber;
(II) an X-ray source to emit X-rays through said X- ray opening;
(III) a sample carrier mounted across said X-ray opening, said carrier comprising:
(a) a base support having a central opening for the passage of X-rays, said central opening corresponding to said camera X-ray window;
(b) an experimentation frame for the reception of powders to be analyzed; said frame slidably mounted over said support and removably secured thereto;
(c) said frame having a window adapted to register with said opening, and
(d) bars extending across said window to divide the said window into separate areas, and
(e) an adhesive strip fixed over said frame.
2. In an apparatus for the X-ray diffraction analysis of powder samples, the combination comprising:
(1) a linear X-ray camera having a main body defining a film exposure chamber and an X-ray window leading into said chamber;
(II) an X-ray source to emit X-rays through said X- ray Opening;
(III) a sample carrier mounted across said X-ray opening, said carrier comprising:
(a) a base support having guiding and clamping means along the edges thereof and an opening substantially centrally thereof for the passage of X-rays, said central opening corresponding to said camera X-ray window;
(b) an experimentation frame for the reception of powders to be analyzed; said frame slidably mounted over and clamped to said base support in predetermined position by means of said guiding and clamping means;
(0) said frame having a window therethrough adapted to register with the opening through said base support; and
(d) at least two substantially parallel bars mounted thereon to divide said window into three separate areas, and
(e) an adhesive strip fixed over said frame.
3. In an apparatus for the X-ray diffraction analysis of powder samples, the combination comprising:
(I) a linear X-ray camera having a main body defining a film exposure chamber and an X-ray window leading into said chamber;
(II) an X-ray source to emit X-rays through said X- ray opening;
(III) a sample carrier mounted across said X-ray opening, said carrier comprising:
(a) a rectangular base support having guiding and abutment shoulders along three edges thereof and a central opening therethrough for the passage of X-rays, said central opening corresponding to said camera X-ray window;
(b) an experimentation frame for the reception of powders to be analyzed; said frame adapted to be slidably mounted over said support snugly between said shoulders and having a window adapted to register with the opening through said support when mounted thereover;
(c) at least two substantially parallel bars mounted across said window to divide said window into three separate areas, and
(d) means along the fourth edge of said base support to clamp said frame thereover and against said abutment flange, and
(e) an adhesive strip glued over said frame.
4. A sample carrier, as claimed in claim 3, wherein the inner faces of said shoulders in relation to said opening are outwardly and downwardly inclined and the four edges of said experimentation frame are correspondingly inclined, and wherein said means is an eccentric rotatable disc mounted on the fourth edge of said base support; the peripheral face of said disc being so chamfered and positioned in relation to the adjacent inclined edge of said frame as to cause the said frame to move between the guiding shoulders and to abut the abutment shoulder and to be clamped to said base support.
5. A sample carrier as claimed in claim 4, wherein said frame has two transverse grooves, one on each side of said window, for cutting off said adhesive strip glued thereover.
References Cited by the Examiner UNITED STATES PATENTS 2,025,488 12/1935 Chu-Phay Yap 250'51.5 2,317,312 4/1943 Swanson et al. 49449 2,317,329 4/1943 McLachlan 250-515 2,499,019 2/1950 Dornfeld 250-495 2,993,992 7/1961 Craig 250-4l.9
RALPH G. NILSON, Primary Examiner.
A. L. BIRCH, Assistant Examiner.

Claims (1)

  1. 3. IN AN APPARATUS FOR THE X-RAY DIFFRACTION ANALYSIS OF POWDER SAMPLES, THE COMBINATION COMPRISING: (I) A LINER X-RAY CAMERA HAVING A MAIN BODY DEFINING A FILM EXPOSURE CHAMBER AND AN X-RAY WINDOW LEADING INTO SAID CHAMBER; (II) AN X-RAY SOURCE TO EMIT X-RAYS THROUGH SAID XRAY OPENING; (III) A SAMPLE CARRIER MOUNTED ACROSS SAID X-RAY OPENING, SAID CARRIER COMPRISING: (A) A RECTANGULAR BASE SUPPORT HAVING GUIDING AND ABUTMENT SHOULDERS ALONG THREE EDGES THEREOF AND A CENTRAL OPENING THERETHROUGH FOR THE PASSAGE OF X-RAYS, SAID CENTRAL OPENING CORRESPONDING TO SAID CAMERA X-RAY WINDOW; (B) AN EXPERIMENTATION FRAME FOR THE RECEPTION OF POWDERS TO BE ANALYZED; SAID FRAME ADAPTED TO BE SLIDABLY MOUNTED OVER SAID SUPPORT SNUGLY BETWEEN SAID SHOULDERS AND HAVING A WINDOW ADAPTED TO REGISTER WITH THE OPENING THROUGH SAID SUPPORT WHEN MOUNTED THEREOVER; (C) AT LEAST TWO SUBSTANTIALLY PARALLEL BARS MOUNTED ACROSS SAID WINDOW TO DIVIDE SAID WINDOW INTO THREE SEPARATE AREAS, AND (D) MEANS ALONG THE FOURTH EDGE OF SAID BASE SUPPORT TO CLAMP SAID FRAME THEREOVER AND AGAINST SAID ABUTMENT FLANGE, AND (E) AN ADHESIVE STRIP GLUED OVER SAID FRAME.
US325972A 1962-12-11 1963-11-26 Sample carrier with adhesive tape for the analysis of powders by means of a guinier x-ray camera Expired - Lifetime US3307036A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3445152A (en) * 1965-01-05 1969-05-20 Ici Ltd Microscope slides and method of manufacturing
US3654460A (en) * 1969-02-12 1972-04-04 Continental Oil Co Automatic sample changer for a goniometer with means to accomodate samples of different thicknesses
US3736042A (en) * 1971-05-05 1973-05-29 Clinical Sciences Inc Microscope slide assembly
EP0185351A2 (en) * 1984-12-20 1986-06-25 Europäische Atomgemeinschaft (Euratom) Sample support, especially for an X-ray diffractometer
US4646341A (en) * 1985-03-28 1987-02-24 Upa Technology, Inc. Calibration standard for X-ray fluorescence thickness
US4770593A (en) * 1987-01-12 1988-09-13 Nicolet Instrument Corporation Sample changer for X-ray diffractometer
US5084910A (en) * 1990-12-17 1992-01-28 Dow Corning Corporation X-ray diffractometer sample holder

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2025488A (en) * 1933-03-29 1935-12-24 Yap Chu-Phay X-ray diffraction apparatus
US2317312A (en) * 1940-10-18 1943-04-20 Andersen Corp Window construction
US2317329A (en) * 1942-10-20 1943-04-20 American Cyanamid Co Specimen holder for x-ray analyses
US2499019A (en) * 1949-01-29 1950-02-28 Rca Corp Adjustable specimen support for electron-optical instruments
US2993992A (en) * 1959-01-23 1961-07-25 Ass Elect Ind Mass spectrometers

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2025488A (en) * 1933-03-29 1935-12-24 Yap Chu-Phay X-ray diffraction apparatus
US2317312A (en) * 1940-10-18 1943-04-20 Andersen Corp Window construction
US2317329A (en) * 1942-10-20 1943-04-20 American Cyanamid Co Specimen holder for x-ray analyses
US2499019A (en) * 1949-01-29 1950-02-28 Rca Corp Adjustable specimen support for electron-optical instruments
US2993992A (en) * 1959-01-23 1961-07-25 Ass Elect Ind Mass spectrometers

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3445152A (en) * 1965-01-05 1969-05-20 Ici Ltd Microscope slides and method of manufacturing
US3654460A (en) * 1969-02-12 1972-04-04 Continental Oil Co Automatic sample changer for a goniometer with means to accomodate samples of different thicknesses
US3736042A (en) * 1971-05-05 1973-05-29 Clinical Sciences Inc Microscope slide assembly
EP0185351A2 (en) * 1984-12-20 1986-06-25 Europäische Atomgemeinschaft (Euratom) Sample support, especially for an X-ray diffractometer
EP0185351A3 (en) * 1984-12-20 1989-02-08 Europäische Atomgemeinschaft (Euratom) Sample support, especially for an x-ray diffractometer
US4646341A (en) * 1985-03-28 1987-02-24 Upa Technology, Inc. Calibration standard for X-ray fluorescence thickness
US4770593A (en) * 1987-01-12 1988-09-13 Nicolet Instrument Corporation Sample changer for X-ray diffractometer
US5084910A (en) * 1990-12-17 1992-01-28 Dow Corning Corporation X-ray diffractometer sample holder

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