A general expression for the method of QXRPD without standards is given in this paper to solve the problem of phase analysis on samples containing a non-crystalline component. Its application to some specific cases is discussed. The experiments have proved successful in the analysis of cement and sand-lime samples. The technique may also be applicable for the analysis of fly-ash, glass, ceramics, and metals. It is especially convenient in the study of kinetics and mechanism of reactions when the chemical composition of all samples does not change, because it is not necessary to know the mass absorption coefficient of samples. In the mathematical treatment of non-linear equations given in this paper, a method called linearized iteration procedure is first presented by the author.

The kinetics of γ'-phase formation in a Ni-base superalloy were studied. The data (pairs of cps and 2θ) were processed by the deconvolution program (Wiedemann, Unnam and Clark, 1987), which was rewritten in FORTRAN and installed on an IBM/VM and a VAX/VMS host computer. Optimal program parameters were found. Pure nickel was used as a standard. The only evidence obtained from the raw data is that the early stage of the aging process is accompanied by broadening. Deconvolution resolved the peaks into three kinds of diffraction lines: Ni(γ), precipitate (γ'), and undefined lines which have been interpreted as satellites. The results show that our X-ray diffraction lines are composed of the main diffraction lines of nickel-base A1 type alloy and additive satellites. In an advanced stage of aging the satellites assume the typical diffraction pattern of γ' phase.

A procedure for Sr-analysis of vein barites by X-ray powder diffraction is described. It is based on the measurement of barite d210 spacing change referenced to NaCl as the internal standard. This procedure covers a range of Sr isomorphic substitution of 0 to 12% SrSO4. Comparison with other values, derived from literature data, shows they are in good agreement with the experimental ones. Statistical analysis of the results yields a maximum absolute error of ±0.50 %SrSO4 in Sr determination. This measurement error proves to be acceptable for most studies of barite in mineral deposits. The effect of Pb-substitution is smaller, in most cases, than this error.

The reported method has the advantage of being fast and simple. It can routinely handle large number of samples as well as small samples isolated from large crystals. Moreover, it allows the recovery of the original sample after the analysis by dissolving the NaCl in water. The main disadvantage is that fair amounts of quartz interfere with the measurement of the position of the barite 210 line.

Simple relationships exist between the individual phase scale factors derived from Rietveld analysis of multiphase mixtures and (i) the ‘reference intensity ratio’ used in traditional methods of discrete-peak phase analysis, (ii) the phase abundance itself and (iii) the relative pattern intensities in simulated powder patterns. These relationships are shown to follow naturally from the fundamental integrated-intensity phase-analysis equations provided in standard texts. In the event that preferred orientation, crystallinity, extinction and/or microabsorption cannot be adequately incorporated into the Rietveld models for individual phases, it is demonstrated that the Rietveld ab initio ‘pattern intensity constants’ can be scaled/calibrated experimentally, as in other whole-pattern methods of analysis, while retaining all the advantages of the Rietveld method.

Diffracted intensities from an X-ray diffractometer operating with fixed or variable divergence slits were compared, following a reported systematic deviation from the theoretical 1/sinθ intensity ratio between these two slit configurations. The theoretical relationship was found to hold over a wide 2θ range provided the anti-scatter slit did not obstruct the beam at higher diffraction angles as the variable slit increased beam divergence. Such obstruction was found to be a possible explanation for the reported deviation.

A previously manually operated film comparator used to evaluate Guinier films has been automated as a film scanner of the flat film type. The film movement is controlled by a stepper motor and the intensity of the transmitted light is recorded as a function of position on the film. A personal computer controls the stepper motor and records the measurements of the transmitted light intensity. The data quality is judged from refinements of lattice constants for α-SiO2 and ZrO2. The powder pattern for Pb2Sr2Ho0.625Ca0.375Cu3O8 and a high temperature study of the thermal expansion of GeO2 are presented.

The binary phase diagram of para-dibromobenzene and para-chloroiodobenzene is characterized by a partial miscibility with a peritectic invariant. Unit cell parameters have been determined and their variation analyzed as a function of composition.

An iterative external standard method of X-ray diffraction is presented to overcome the difficulties of preferred orientation and peak overlap encountered in quantitative phase analysis. Instead of using only a single line intensity in the traditional external standard technique, all the reflection data are used in the calculation. The accuracy and applicability of this method was tested on a series of two-phase powder mixtures with known composition. The results show markedly good agreement with the actual values. As an example, the analysis was applied to the data collected from an as plated electrodeposited Zn-Fe coating. The determined phase composition of the coating was found to be 88.2 +/− 5.3 wt % δ-phase and 11.8 +/− 0.7 wt % η -phase.

This report is one of a series on the nomenclature for spectrochemical analysis issued by the International Union of Pure and Applied Chemistry. It concerns a new notation for X-ray emission lines and absorption edges, to be called IUPAC NOTATION, which replaces the existing Siegbahn notation. It is based upon the energy level designation and has the advantage of being simple and easy to apply to any kind of transition. Moreover, it is consistent with the notations used in electron spectroscopy.

The document first discusses the terms currently used in X-ray spectroscopy and then describes the principles of the IUPAC notation with reference to the X-ray levels and the X-ray transitions. The correspondence between Siegbahn and IUPAC notations for all X-ray lines is given in a table. Finally, the document gives the units and conversion factors used in the X-ray range.

X-ray powder diffraction data for the compound 2,2′,2″-triaminotriethylamine-trihydrochloride, N-(CH2−CH2−NH2)3 (HCL)3 are reported. The crystals are cubic and the space group is P213 with a = 10.8734(12) Å. Dx = 1.320Mg/m3. The data were obtained both by photographic and diffractometric methods.

X-ray powder diffraction data for clemizole hydrochloride (1-p-chlorob-enzyl-2-pyrrolidin-1′-ylmethyl-benziminazole hydrochloride, C19H20ClN3.HCl) and cyclizine hydrochloride (1-benzhydryl-4-methylpiperazine hydrochloride, C18H22N2.HCl) are reported. Crystals of clemizole hydrochloride are monoclinic, space group P21/n with a = 29.940(5) Å, b = 10.963(2)Å, c = 5.515(2)Å, β = 90.98 (3)°, Z = 4 and Dx = 1.330g cm−3. Crystals of cyclizine hydrochloride are orthorhombic, space group Pna21 (or Pnam), with a = 11.816(1)Å, b = 13.609(2)Å, c = 9.999(1 )Å, Z = 4 and Dx = 1.251g cm−3.

Six acentric tartrates and tartrato-antimonates have been investigated by means of X-ray powder diffraction. Single crystals were obtained by evaporation from aqueous solutions. The compounds have attracted attention because of their electrostrictive and electro-optical effects. Complete crystal data for the six compounds are reported. X-ray powder diffraction patterns for Rb2C4H4O6 and Ca [Sb2{C4H2O6}2]·2H2O are given.

Single crystals of Cs3A[B2(SCN)7] with A = Sr, Ba and B = Ag, Cu have been synthesized from aqueous solutions by the evaporation method. The complex thiocyanates are isostructural and crystallize in the tetragonal system with space group .

Complete crystal data and optical data for the four compounds are reported. An X-ray powder diffraction pattern for Cs3Sr[Cu2(SCN)7] is given.