WO2000023795A9 - Environmentally controllable sample holder for x-ray diffractometer (xrd) - Google Patents
Environmentally controllable sample holder for x-ray diffractometer (xrd)Info
- Publication number
- WO2000023795A9 WO2000023795A9 PCT/US1999/024678 US9924678W WO0023795A9 WO 2000023795 A9 WO2000023795 A9 WO 2000023795A9 US 9924678 W US9924678 W US 9924678W WO 0023795 A9 WO0023795 A9 WO 0023795A9
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sample
- sample holder
- xrd
- housing
- disk
- Prior art date
Links
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
Definitions
- the present invention relates to the analysis of substances using
- X-ray diffractometry is a technique for performing physical and chemical analysis of crystalline
- the radiation intensity at a point removed from the crystalline structure is determined by the phase difference
- a diffracted X-ray beam is essentially a collection of a large number of scattered X-ray waves that satisfy the conditions of constructive interference.
- the sample is irradiated with an X- ray beam produced by an X-ray source and incident at an angle.
- the X-rays diffracted by the powder sample held in the sample holder are detected by a detector positioned at a diffracted angle equal to the incident angle.
- the incident angle and hence the diffracted angle are incrementally varied as both the X-ray source and the detector move along a semi-circle above the sample and sample holder.
- the movements are synchronized so that the incident angle and the diffraction angle are always equal.
- a diffractogram which is the intensity of the diffracted X-ray as a
- the powder sample can be identified based on its diffractogram.
- signal-to-noise may be
- moisture sensitive samples may be destroyed (chemically altered) during the analysis.
- One manner in which to protect the sample is to cover the sample with a metal or plastic film thin enough to allow the X-ray beam to pass through.
- the sample holder should be made of a low background material such as single crystal quartz or silicon.
- non-routine (non-ambient temperatures and relative humidities) modes are using an X-ray diffractometer (XRD).
- XRD X-ray diffractometer
- sample holders must be utilized from time to time in order to subject powder
- X-ray diffractometer conventional X-ray diffractometer (XRD) devices provide complex environmentally controlled sample stages or holders for obtaining X-ray diffractograms under non-ambient conditions (e.g., elevated and sub-ambient temperatures).
- XRD X-ray diffractometer
- sample holder for non-ambient analysis e.g., a scan at elevated temperatures
- the present invention provides an environmentally controllable sample holder for use in combination with the sample changer of an X-ray diffractometer (XRD).
- the sample holder comprises a sample holder including a sample plate, a base adapted for removable attachment to the sample
- a heating element positioned between the sample plate and the sample holder base, and a temperature sensor adapted to provide a feedback
- a detachable housing is provided for sealingly enclosing the sample holder
- the housing includes an aperture in the bottom for sealingly receiving
- a temperature sensor is mounted in the
- the housing in order to measure the temperature therein, and the housing includes an X-ray transparent top portion or window therein.
- non-routine non-ambient temperature and relative humidity
- XRD X-ray diffractometer
- PEEK polyetheretherketone
- Figure 1 is an exploded view of the sample holder element of the o environmentally controllable sample holder of the present invention
- Figure 2 is an exploded perspective view of the housing for the sample
- Figure 3 is a perspective view of the environmentally controllable
- Figure 4 is graph of the test results from X-ray powder diffraction analysis of ACYCLOVIRTM obtained during conversion using the
- a pharmaceutical company can submit a drug application (e.g., NDA) to regulatory authorities.
- a drug application e.g., NDA
- holder can be used by technicians not skilled in X-ray diffractometer instrument alignment and thereby allows for quick conversion between normal and
- Sample holder element 10 comprises base 12, preferably formed of ceramic, and consisting of a stem and flat disk mounted thereon.
- Heating element 14 comprises a mica disk having resistive wires (not shown) mounted thereto.
- Insulation disk 16, preferably formed of ceramic material, is positioned beneath heating element
- thermosensor TS embedded therein to provide a feedback signal for use in controlling heating
- An O-ring 20 is provided and sized so as to seat around the circumference of heat sink disk 18. O-ring 20 serves to provide a sealing
- a screw 22 serves to secure together ceramic base 12, insulation disk
- a sample plate disk 24 preferably formed from a single crystal (511) or (510) silicon wafer, serves as a platform for a powder sample (not shown) to be analyzed.
- Housing 40 preferably formed of steel, is shown in Figure 2 and is adapted to cover and seal sample holder element 10 once the sample holder element is attached to the sample changer of X-ray diffractometer XRD.
- Housing 40 is provided with air inlet nozzle 42A and air exhaust nozzle 42B to provide for the introduction of gases (either inert-nitrogen-atmosphere or
- housing 40 varying relative humidity gases
- thermocouple 44 is provided in the housing and extends into the internal space in order to
- thermocouple 44 may, optionally, also be used in addition to the signal from temperature sensor TS to control heating element 14.
- housing 40 is
- an arcuate top cover 46 formed from polyetheretherketone
- ceramic base 12 insulation disk 16, heating element 14, heat sink disk 18 (including temperature sensor TS embedded
- a selected powder sample is loaded onto sample plate disk 24.
- the silicon does not produce any significant interference for radiation.
- sample holder element 10 is then covered with steel housing 40 shown in Figure 2. Air
- inlet nozzle 42A and air exhaust nozzle 42B allow for the introduction of gases into housing 40, either inert-nitrogen-atmosphere or varying relative humidity (0 to 100%).
- Thermocouple 44 is inserted into housing 40 in order to measure the temperature of the air in housing 40 surrounding the powder sample on sample plate disk 24.
- environmentally controllable sample holder consisting of sample holder element 10 and housing 40 may then be installed on sample changer SC of X-ray diffractometer XRD (see Figure 3) and sample data acquired.
- sample holder consisting of sample holder element 10 shown in Figure 1 and
- housing 40 shown in Figure 2 positioned thereover is shown mounted to sample changer SC of X-ray diffractometer XRD.
- sample changer SC of X-ray diffractometer XRD A conventional sample
- X-ray beam is critical to assure accurate diffraction data. Due to the thickness of ceramic insulating disk 16, the powder sample positioned within
- SH (see Figure 3) can be used in addition to applicants' environmentally controllable sample holder with the six-position sample changer SC of the SCINTAG XRD.
- Applicants' novel environmentally controllable sample holder for use with the sample changer of an X-ray diffractometer offers a number of advantages over conventional
- Gas inlet nozzle 42A allows for the introduction of gases of
- O-ring 20 allows for sample holder element 10 to exclude
- Glaxo Wellcome ACYCLOVIRTM (>99% pure) was used.
- mm diffracted beam scatter slit 0.3-mm receiving slit, and 0.03-deg two-theta computer (A/D) resolution.
- Soller slits were incorporated in the incident and diffracted X-ray beams.
- the diffractometer was operated in the 250-mm goniometer radius and continuous scanning mode at 10° 2-theta/minute for all
- Relative humidity in the environmental chamber was controlled by a humidity generator (RH-100 from VTI Corp. of Hialeah, Florida).
- Typical operating parameters for the humidity generator included a humidifier set
- the VTI RH-100 humidity generator is capable of producing an output
- gas stream ranging from less than 5% to greater than 95% relative humidity at
- Typical flow rate settings of the output gas range from 400 to 1500
- hotstage XRD was performed on samples of stearic acid, urea, and tin to determine the onset of melting; the XRD results are compared to that obtained from DSC as shown below in Table 1.
- Form B lost its lattice water and converted to Form B, as indicated by the appearance of peaks at 2 ⁇ angle of 8.2° and 14.8°. Form B converted back to
- Form A after subsequent exposure to 80% RH controlled with the VTI RH-100 humidity generator at 25°C.
- Form B was further heated to 160°C, it converted to Form C which exhibited distinctive peaks at 2 ⁇ angle of 8.4° and
- Scintag, Inc. provide environmentally-controlled sample holders (sample stages) for obtaining X-ray diffractograms under non-ambient conditions (e.g.,
- applicants' novel environmentally controllable sample holder can be used by those not skilled in XRD instrument alignment in order to allow for quick
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)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU11295/00A AU1129500A (en) | 1998-10-21 | 1999-10-21 | Environmentally controllable sample holder for x-ray diffractometer (xrd) |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10510398P | 1998-10-21 | 1998-10-21 | |
US60/105,103 | 1998-10-21 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2000023795A1 WO2000023795A1 (en) | 2000-04-27 |
WO2000023795A9 true WO2000023795A9 (en) | 2000-08-24 |
Family
ID=22304039
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1999/024678 WO2000023795A1 (en) | 1998-10-21 | 1999-10-21 | Environmentally controllable sample holder for x-ray diffractometer (xrd) |
Country Status (2)
Country | Link |
---|---|
AU (1) | AU1129500A (en) |
WO (1) | WO2000023795A1 (en) |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10232172B4 (en) | 2002-07-16 | 2005-03-10 | Proteros Biostructures Gmbh | Apparatus and method for creating a defined environment for particulate samples |
DE10322040A1 (en) * | 2003-05-16 | 2004-12-09 | Forschungszentrum Karlsruhe Gmbh | Coupling and adjustment device for an X-ray diffractometer |
FR2856793B1 (en) * | 2003-06-24 | 2006-04-14 | Inst Francais Du Petrole | POWDER ANALYSIS DEVICE BY X-RAY DIFFRACTION |
EP1947448B1 (en) | 2007-01-19 | 2013-07-03 | Panalytical B.V. | X-ray diffraction equipment for X-ray scattering |
ES2378045B1 (en) * | 2009-04-13 | 2013-02-15 | Consejo Superior De Investigaciones Científicas (Csic) | DEVICE FOR HOUSING A SAMPLE INSIDE A DISPERSION CHAMBER OR X-RAY DIFFACTION. |
FR2978246B1 (en) * | 2011-07-21 | 2014-06-06 | Commissariat Energie Atomique | INTEGRATED THERMOCOUPLE SAMPLE HOLDER |
GB2514125B (en) | 2013-05-13 | 2016-10-05 | Nikon Metrology Nv | X-ray imaging system with climate control |
EP2848924B1 (en) | 2013-09-11 | 2016-08-24 | Anton Paar GmbH | Tempering chamber for compact x-ray apparatus |
EP2927945B1 (en) * | 2014-04-04 | 2023-05-31 | Nordson Corporation | X-ray inspection apparatus for inspecting semiconductor wafers |
RU2650836C1 (en) * | 2016-12-14 | 2018-04-17 | федеральное государственное автономное образовательное учреждение высшего образования "Московский физико-технический институт (государственный университет)" | Sample assembly block, intended for conducting combined measurements by x-ray structural analysis in a sliding bundle and additional physico-chemical methods of the study |
WO2019215326A1 (en) * | 2018-05-11 | 2019-11-14 | Universite De Rouen-Normandie | Anti-frosting and anti-dew device for spectroscopic measurements |
US11774379B2 (en) * | 2018-11-23 | 2023-10-03 | Rigaku Corporation | Soaking machine and soaking method of sample for single-crystal X-ray structure analysis |
CN110031362A (en) * | 2019-02-26 | 2019-07-19 | 中国科学技术大学 | A kind of steam stretching, extension rheometer |
CN111933832B (en) * | 2020-09-03 | 2023-10-20 | 广州阳瑞仪器科技有限公司 | In-situ battery accessory of X-ray diffractometer and assembling method |
CN113049618B (en) * | 2021-03-10 | 2022-12-09 | 华研环科(北京)科技有限公司 | High-temperature high-pressure in-situ XRD testing device |
CN113406128B (en) * | 2021-07-23 | 2022-11-11 | 重庆大学 | Temperature control accessory for X-ray diffractometer |
CN113945594B (en) * | 2021-10-11 | 2023-03-24 | 安徽科技学院 | Rotary sample table for X-ray diffraction analysis for assembling vertical goniometer |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2683933B2 (en) * | 1989-01-20 | 1997-12-03 | 信越半導体株式会社 | Inspection device for front and back and orientation of semiconductor wafer |
US5084910A (en) * | 1990-12-17 | 1992-01-28 | Dow Corning Corporation | X-ray diffractometer sample holder |
US5390230A (en) * | 1993-03-30 | 1995-02-14 | Valence Technology, Inc. | Controlled atmosphere, variable volume sample holder for x-ray diffractomer |
JP3166638B2 (en) * | 1996-11-29 | 2001-05-14 | 株式会社島津製作所 | X-ray fluorescence analyzer |
US5848122A (en) * | 1997-03-25 | 1998-12-08 | Advanced Technology Materials, Inc. | Apparatus for rapid in-situ X-ray stress measurement during thermal cycling of semiconductor wafers |
-
1999
- 1999-10-21 WO PCT/US1999/024678 patent/WO2000023795A1/en active Application Filing
- 1999-10-21 AU AU11295/00A patent/AU1129500A/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
WO2000023795A1 (en) | 2000-04-27 |
AU1129500A (en) | 2000-05-08 |
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