Certification of Standard Reference Material 660B

2011 ◽  
Vol 26 (2) ◽  
pp. 155-158 ◽  
Author(s):  
David R. Black ◽  
Donald Windover ◽  
Albert Henins ◽  
James Filliben ◽  
James P. Cline

This report describes SRM 660b, the third generation of this powder diffraction SRM used primarily for determination of the instrument profile function (IPF). It is certified with respect to unit-cell parameter. It consists of approximately 6 g LaB6 powder prepared using a 11B isotopically enriched precursor material so as to render the SRM applicable to the neutron diffraction community. The microstructure of the LaB6 powder was engineered to produce a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST -built diffractometer, incorporating many advanced design features, was used to certify the unit-cell parameter of the LaB6 powder. Both type A, statistical, and type B, systematic, errors have been assigned to yield a certified value for the unit-cell parameter of a=0.415691(8) nm at 22.5°C.

2020 ◽  
Vol 35 (1) ◽  
pp. 17-22 ◽  
Author(s):  
David R. Black ◽  
Marcus H. Mendenhall ◽  
Craig M. Brown ◽  
Albert Henins ◽  
James Filliben ◽  
...  

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to evaluate specific aspects of instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 660c, the fourth generation of this powder diffraction SRM, which is used primarily for calibrating powder diffractometers with respect to line position and line shape for the determination of the instrument profile function (IPF). It is certified with respect to lattice parameter and consists of approximately 6 g of lanthanum hexaboride (LaB6) powder. So that this SRM would be applicable for the neutron diffraction community, the powder was prepared from an isotopically enriched 11B precursor material. The microstructure of the LaB6 powder was engineered specifically to yield a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the LaB6 powder. Both Type A, statistical, and Type B, systematic, uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.415 682 6 ± 0.000 008 nm (95% confidence).


1991 ◽  
Vol 35 (A) ◽  
pp. 431-438
Author(s):  
Hideo Toraya ◽  
William Parrish

AbstractA procedure for the accurate determination of unit-cell parameters using conventional Xray powder diffractometry is described. Two important factors in the procedure are: 1) the use of high-resolution-type diffractometer, which can suppress the axial beam divergence and thus gives nearly symmetric diffraction profiles in the low 2θ region and 2) the use of a new algorithm for systematic peak shift correction during the least-squares determination of unit-cell parameters of a sample with an internal standard [Toraya & Kitamura (1990). J. Appl. Cryst. 23 , 282-285]. The procedure has been tested by measuring successively the unit-cell parameter of W, CeO2, and Si in three mixtures, Si+W, W+CeO2, and CeO2+Si: the unit-cell parameter of W, which was first determined by using NIST SRM 640b Si powder as an internal standard reference material, was used as a standard reference value to determine the unit-cell parameter of CeO; in the next W+CeO2 mixture, and so on. The difference between the end value of observed Si unit-cell parameters and the starting value of 5.430940(35) Å were just 1 to 5 p.p.m. High accuracy is attainable in measuring the uni-cell parameters even with the conventional powder diffractometry provided with the nearly symmetric diffraction profile and the algorithm for peak shift correction used in the present study.


1987 ◽  
Vol 2 (4) ◽  
pp. 225-226
Author(s):  
Peter Bayliss ◽  
Slade St. J. Warne

AbstractMagnesium-chlorophoenicite may be differentiated from the Mn-analogue chlorophoenicite, because for magnesium-chlorophoenicite at 7Å, whereas for chlorophoenicite.In a review of the literature for the Mineral Powder Diffraction File by Bayliss et al. (1980), powder X-ray diffraction data could not be found of the mineral species magnesium-chlorophoenicite, (Mg,Mn)3Zn2(AsO4)(OH,O)6. Dunn (1981) states that the powder X-ray diffraction data of magnesium-chlorophoenicite is essentially identical to that of chlorophoenicite (Mn analogue) and confirms that the minerals are isostructural.With the crystal structure parameters determined by Moore (1968) for a Harvard University specimen from New Jersey of chlorophoenicite, a powder X-ray diffraction pattern was calculated with the programme of Langhof, Physikalische Chemie Institute, Darmstadt. The calculated pattern was used to correct and complete the indexing of the powder X-ray diffraction data of chlorophoenicite specimen ROM M15667 from Franklin, Sussex County, New Jersey, U.S.A. by the Royal Ontario Museum (PDF 25-1159). With the correctly indexed data of ROM M15667, the unitcell parameters were refined by least-squares analysis and are listed in Table 1.The most magnesium-rich magnesium-chlorophoenicite found in the literature is a description of Harvard University specimen 92803 from Franklin, Sussex County, New Jersey, U.S.A. by Dunn (1981), where Mg is slightly greater than Mn. A 114.6 mm Debye-Schemer film taken of HU92803 with Cu radiation and a Ni filter (CuKα = 1.5418Å) was obtained from Dr. P. Dunn and measured visually. The unit-cell parameters, which were refined by least-squares analysis starting from the unit-cell parameters of PDF 25-1159 in space group C2/m(#12), are listed in Table 1, and give F28 = 4.1(0.050,136) by the method of Smith & Snyder (1979).The hkl, dcalulated, dobserved and relative intensities (I/I1) of HU92803 are presented in Table 2. With the atomic positions and temperature factors of chlorophoenicite determined by Moore (1968), the Mn atomic positions occupied by 50% Mg and 50% Mn, and the unit-cell parameters of HU92803, a powder X-ray diffraction pattern was calculated and Icalculated is recorded in Table 2. A third powder X-ray diffraction pattern was calculated with the Mn atomic positions fully occupied by Mg. Because the atomic scattering factor of Mn is more than twice greater than Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the calculated intensities of the first three reflections given in Table 3.Although the a, c and β unit-cell parameters of chlorphoenicite are similar to those of magnesium-chlorphoenicite, the b unit-cell parameter of chlorophoenicite is significantly greater than that of magnesium-chlorophoenicite (Table 1). The b unit-cell parameter represents the 0–0 distance of the Mn octahedra (Moore, 1968). Since the size of Mn is greater than that of Mg, chlorophoenicite may be differentiated from magnesium-chlorophoenicite based upon the b unit-cell parameter given in Table 1.American Museum of Natural History (New York, N.Y., U.S.A.) specimen 28942 from Sterling Hill, Ogdensburg, New Jersey is composed of willemite, haidingerite and magnesian chlorophoenicite. A spectrographic analysis of the magnesian chlorophoenicite shows As, Mg, Mn and Zn. Powder X-ray diffraction data (PDF 34-190) of the magnesian chlorophoenicite was collected by diffractometer with Cu radiation and a graphite 0002 monochromator (Kα1 = 1.5405) at a scanning speed of 0.125° 2θ per minute. The unit-cell parameters, which were refined by leastsquares analysis starting from the unit-cell parameters of PDF 25-1159, are given in Table 1. Specimen AM 28942 is called chlorophoenicite, because of its large b unit-cell parameter (Table 1), and the I/I1 of 25 for reflection 001 and of 50 for reflection 201 compared to the Icalculated in Table 3.


2010 ◽  
Vol 25 (1) ◽  
pp. 25-30 ◽  
Author(s):  
Ryouichi Yokoyama ◽  
Jimpei Harada ◽  
Yoshiaki Akiniwa

Biaxial residual stress in a 〈111〉 textured cubic TiN polycrystalline thin film was analyzed by linear least-squares refinement using the method proposed by Yokoyama and Harada [J. Appl. Crystallogr. 42, 185–191 (2009)]. Values of the unstressed (or stress-free) unit-cell parameter a0=4.2332±0.0006 Å and the stress components of σ11=397(88), σ22=401(88), and σ12=−110(100) were obtained. The values of the in-plane stresses σ11 and σ22 presented in the TiN film are practically the same, while σ12 is relatively small. The results obtained in this study confirm that the above theoretical prediction by Yokoyama and Harada can be used to obtain reliable values of stress-free unit-cell parameter and three biaxial stress components of a textured cubic thin film.


1996 ◽  
Vol 11 (1) ◽  
pp. 31-34 ◽  
Author(s):  
Nicole M. L. N. P. Closset ◽  
René H. E. van Doorn ◽  
Henk Kruidhof ◽  
Jaap Boeijsma

The crystal structure of La1−xSrxCoO3−δ (0≤x≤0.6) has been studied, using powder X-Ray diffraction. The crystal structure shows a transition from rhombohedral distorted perovskite for LaCoO3−δ into cubic perovskite for La0.4Sr0.6CoO3−δ. The cubic unit cell parameter is ac=3.8342(1) Å for La0.4Sr0.6CoO3−δ, the space group probably being Pm3m. Using a hexagonal setting, the cell parameters for La0.5Sr0.5CoO3−δ, are a=5.4300(3) Å, c=13.2516(10) Å; a=5.4375(1) Å, c=13.2313(4) Å for La0.6Sr0.4CoO3−δ; a=5.4437(1) Å, c=13.2085(5) Å for La0.7Sr0.3CoO3−δ; a=5.4497(2) Å, c=13.1781(6) Å for La0.8Sr0.2CoO3−δ and a=5.4445(2) Å, c=13.0936(6) Å for LaCoO3−δ with the space group probably being R3c.


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