The importance of surface roughness to the measurement of integrated intensity in X-ray powder diffraction is discussed following studies conducted with materials in both powder and bulk (rolled sheet/billet) forms possessing different absorption characteristics. A simple procedure is described which allows for surface roughness effect.

The crystal structure of monoclinic CuF2 has been refined by the Rietveld method from X-ray powder diffraction data. The structure is monoclinic, space group P21/n, a = 3.2973(2), b = 4.5624(3), c = 4.6157(3) Å, β = 83.293(3)°, V = 68.96(2) Å3, with Cu+2 at (0,0,0) and F−1 at (−0.04176(68), 0.29410(35), 0.29410(35)). Final RB = 0.97%, RP = 1.99%, Rwp = 2.32%, RWP(expected) = 1.46%. The structure has a rutile-type arrangement, but with a monoclinic distortion that produces a highly distorted octahedral coordination around the Cu2+ ion with equatorial and apical Cu-F distances of 1.92 and 2.32 Å respectively.

Crystal data for p-bromoiodobenzene (pBIB) at 293 K and a powder diffraction pattern are reported. The unit cell is monoclinic with S.G. = P21/a and Z = 2. The cell parameters are: a = 16.196(6) Å, b = 5.872 (3) Å, c = 4.233 (2) Å, β = 113.86 (2)°.

The beautiful methods of crystal analysis that have been developed by Laue and the Braggs are applicable only to individual crystals of appreciable size, reasonably free from twinning and distortion, and sufficiently developed to allow the determination of the direction of their axes. For the majority of substances, especially the elementary ones, such crystals cannot be found in nature or in ordinary technical products, and their growth is difficult and time-consuming.

The method described below is a modification of the Bragg method, and is applicable to all crystalline substances. The quantity of material required is preferably 0.005 c.c., but one tenth of this amount is sufficient. Extreme purity of material is not required, and a large admixture of (uncombined) foreign material, twenty or even fifty per cent, is allowable provided it is amorphous or of known crystalline structure.

The structure and powder diffraction data of Hägg-carbide (χ-Fe5C2) have been redetermined and improved by X-ray diffraction. Experimental values of 2θ, corrected for systematic errors, relative peak intensities, lattice spacings, and the Miller indices of 27 observed reflections up to 100° 2θ are reported. The unit cell is monoclinic (space group C2/c, Z=4) with a=11.588 Å, b=4.579 Å, c=5.059 Å, and β=97.75°. The crystal structure has been refined by Rietveld analysis, resulting in Rwp=0.073.

The boron and iron for aluminum substitution in the Rb-leucite structure (RbAlSi2O6, ICDD card 38-201) has been examined by sol-gel preparation of different samples along the three compositional joins Rb(X,Y)Si2O6, where X and Y are any two of the elements Al, Fe, B. The compound RbBSi2O6 (a0=12.831 Å) is here described and characterized by X-ray powder diffraction for the first time, while the compound RbFeSi2O6 is reexamined with a more precise determination of lattice parameters and diffraction intensities with respect to ICDD card 31-1189. The lattice parameters and the space groups of different selected terms of the three solid solutions are reported.

Indexed X-ray diffraction data are reported for 1-adamantanol. The data were indexed on a tetragonal unit cell with a=15.869 Å and c=6.879 Å, P44/nZ=8.

Methods for precise control of the cutting angles of quartz by x-ray measurements are described. The quartz must first be oriented by some other method (usually optically) before the x-ray method can be applied. The sense of direction of the cut is indicated by an arrow drawn on the outer surface of the test cut at the saw and this direction is preserved in making the x-ray measurement. The x-ray technique is an adaptation of the Bragg ionization chamber method and involves measuring the angle between the surface of the test cut or blank and an atomic reference plane parallel (or nearly parallel) to the surface. All measurements are direct, and require no computation. A Gieger-Muller tube operated in the proportional counter region is employed. Accuracy of the method is approximately ±1.5′, the measurement requires about 10-15 seconds, and is used by unskilled help. The procedures for calibrating the x-ray goniometer and measuring various types of cuts are described in detail. Methods involving precise angular adjustments of sections approximately oriented by other methods and the use of reflection intensity differences of certain planes on either side of the optic axis for detecting usable portion of electrical twins and negative and positive directions from Z are described. The methods are applicable to other fields.

The compounds, BaR2Ti3O10: R = La, Pr, Nd and Sm; BaR2Ti4O12: R = La, Pr, Sm, Gd, Eu have been prepared by solid state reaction and characterized by X-ray powder diffraction. Unit cell data are summarised; lattice parameters and unit cell volumes increase approximately linearly with lanthanide ion size.