MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTI-TATIVE X-RAY DIFFRACTION PHASE ANALYSIS

A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

AN INCREMENTAL METHOD OF X-RAY DIFFRACTION QUANTITATIVE PHASE ANALYSIS OF SAMPLESCONTAINING AMORPHOUS MATERIAL

A new method for quantitative X-ray diffraction phase analysis of a powder misture has been developed according to Popovic's doping method. The weight fraction of amorphous material in the analysed sample is obtained. For a multicomponent system in which (n-2) pure phases are added into an n-phase compnent sample and theweight fractions of all n phases can be determined by the method. The test results of confirmation agree well with the theory.

A SOLUTION OF MINIMUM NORM FOR QUANTITATIVE PHASE ANALYSIS BY STANDARDLESS X-RAY DIFFRACTION

A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus,The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.

A SOLUTION OF MINIMUM NORM FOR QUANTITATIVE PHASE ANALYSIS BY STANDARDLESS X-RAY DIFFRACTION

A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus.The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.

THE DEGREE OF CRYSTALLINITY OF MULTICOMPONENT POLYMERS BY X-RAY DIFFRACTION ANALYSIS

Based on the X-ray scattering intensity theory,the correction factors of the degree of crystallinity formulae of the multicomponent polymers have been clearly defined.The formula of degree of erystallinity of the multicomponent polymers was derived in terms of the WAXD theory ahd improved graphic multipeak resolution methods.The results calculated are compatible with the density measurement.

Simulation of X-ray Diffraction Line Broadening Caused by Stress Gradients and Determination of Stress Distribution by Fourier Analysis

Different physical, mechanical and chemical processes, such as： ion implantation, oxidation, nitridation and others create on the surface of materials residual stress state, characterized by high level and strong gradient. X-ray diffraction method widely used for stress measurements has some difficulties in interpretation of experimental data, when the depth of X-ray penetration is compared with thickness of surface layer where inhomogeneous stress distribution is localized. Early it has been shown by authors that diffraction line broadening occurs when analyzed surface is characterized by strong gradient. The interest to study the diffraction line broadening is connected to the possibility of obtaining information about parameters of surface stress distribution. In the present paper the convolution and deconvolution concepts of Fourier analysis were applied to study X ray diffraction line broadening caused by surface stress gradients. Developed methodology allows determining of stress distribution in superficial layers of materials.

Investigation of Changes in the Fine Structure of Graphitizing Carbon Materials during Heat Treatment by X-Ray Diffraction Analysis

The properties of synthetic graphite materials, widely used in advanced fields, are determined by their structure, which is formed in the process of high-temperature (~2500°C) heat treatment. The fine structure of a graphitizing carbon material based on petroleum coke containing 1.3 wt% S at various stages of graphitization was studied by X-ray diffraction analysis. Some of the samples contained the addition of dispersed Fe2O3. It is shown that the heat-treated material in the range 1200°C - 2600°C is heterogeneous, its component composition is determined by the processing temperature and the presence of Fe2O3 additive. The observed dependence of the component composition on the heat treatment temperature suggests that the process of graphitization of the carbon material, apparently, develops through a number of metastable states.

AN EXTERNAL STANDARD METHOD OF QUANTITATIVE PHASE ANALYSIS OF THE SAMPLE CONTAINING AN AMORPHOUS PHASE BY X—RAY DIFFRACTION

A new method of the quantitative phase analysis of the sample containing an amorphous phase or a standardless phase by X-ray diffraction is proposed in the paper. The addtion of a reference phase or some analytical phase to the analyzed sample is not required in this method and the experimental results are satisfactory.

X-ray peak profile analysis of dislocation type,density and crystallite size distribution in cold deformed Pb-Ca-Sn alloys

The density,nature of the dislocations and distribution of the domain sizes in cold-deformed Pb-Ca-Sn solid solution were determined by X-ray diffraction profile analysis.The dislocation densities are of the order of 1010 cm-2.The strain broadening of diffraction profiles was accounted for by dislocation contrast factor.The coherent domain size was determined by the recently developed PM2K software package.Assuming that the domain size distribution is log-normal,the distribution function（median μ and variance σ） was calculated from the size parameters determined from X-ray diffraction profile analysis.

DATA PROCESSING OF UNIVERSAL QUANTITATIVE METHOD IN STANDARDLESS X-RAY PHASE ANALYSIS

Accuracy of coeffcient A_(isp) is related to the reference phase chosen during analysis. The cri- terion of choosing reference phase which may minimize the error of A_(isp) was deduced. The optimum results could be obtained by using the method of least squares if the number of sam- pies for analysis is more than the phase in samples. The procedure presented here is satisfacto- ryfor ordinary phase analysis.

X-Ray Powder Diffraction: Why Not Use CuKβ Radiation?

CuKβ radiation with a wavelength of λ = 1.3923 ? is recommended for crystal structure determination from X-ray powder diffraction using the Rietfeld method. A highly sensitive image plate detector is able to collect enough intensity to record a brilliant X-ray powder pattern in a reasonable time, compared to CuKα1 radiation used today. Especially atomic displacement coefficients could be determined more precisely with the much greater number of reflections recorded. A double-radius Guinier camera attached to a micro-focus rotating anode tube ensures increased brilliance besides high resolution. A simple construction specification is presented to make smart cylindrically bent Ge(111) or Si(111) X-ray monochromators that deliver focused CuKβ radiation. The highly linear response of image plate detectors allows removing of fluorescence radiation simply as background of the pattern. The proposed equipment is a cost-efficient alternative to a liquid gallium-metal-jet X-ray source with maximum power load and a similar wavelength of λ(GaKα1) = 1.34013 ?.

A New Method for Clay Mineral Analysis and Its Application in Geology

X-ray diffraction (XRD) peaks in a low-angle diffraction section of clayminerals, especially those of authigenic origin, have broadening and tailing features in shape.Using the five basic parameters, peak position, peak height, width, shape coefficient and asymmetry,to describe an XRD peak is more accurate, comprehensive and integrated than using only 3 of them,position, height and width. Following the concept of the five basic parameters of an XRD peak, theprogram Decoform proposed in this study provides more information in mineralogical analyses byfitting actual XRD profiles. In combination with the HW-IR plot, Decoform can he systematically andaccurately used in the comprehensive analyses of crystallinity, domain size, lattice strain andquantitative phase. It is also of value for the geological investigations of diagenesis,metamorphism, basin maturity, structural stress field and so on.

Measurement of integral diffraction coefficients of crystals on beamline 4B7 of Beijing Synchrotron Radiation Facility

Integral diffraction coefficients of the crystal are the essential data of a crystal spectrometer which is extensively used to measure quantitative x-ray spectra of high temperature plasmas in kilo-electron-volt region. An experimental method has been developed to measure the integral diffraction coefficients of crystals on beamline 4B7 of Beijing Synchrotron Radiation Facility. The integral diffraction coefficients of several crystals including polyethylene terephthalate （PET）, thallium acid phthalate （T1AP） and rubidium acid phthalate （RAP） crystals have been measured in the x-ray energy range 2100-5600 eV and compared with the calculations of the ＇Darwin Prins＇ and the ＇Mosaic＇ models. It is shown that the integral diffraction coefficients of these crystals are between the calculations of the ＇Darwin Prins＇ and the ＇Mosaic＇ models, but more close to the ＇Darwin Prins＇ model calculations.

Structural Analysis of Eu_2Mn_(2/3)Ta_ 4/3O_7 with a Pyrochlore-Related Structure

Eu 2Mn 2/3Ta 4/3O 7 specimen was synthesized from Eu 2O 3, MnO and Ta 2O 5 in a reducing atmosphere. Structure analysis was carried out by Rietveld method from X-ray diffraction data. The X-ray diffraction profile calculated with monoclinic C2/c model was in a good agreement with the observed X-ray diffraction patterns since several small peaks of super lattice could be also assigned with C2/c symmetry in addition to fundamental reflection peaks. Eu 2Mn 2/3Ta 4/3O 7 has two kinds of distorted (Mn, Ta)O 6 octahedra and HTB layers, which deviates from the regular forms. Europium atoms coordinate to eight or seven oxygen atoms and lead to two kinds of polyhedra, EuO 8 and EuO 7 in this compound.

Multifrequency Magneto-optic Bragg Diffraction and Radio Frequency Signal Parallel Processing

Magneto-optic(MO)coupling of guided optical waves with microwave magnetostatic waves(MSWs)simultaneously excited by multiple radio frequency(RF)signals can lead to multifrequency diffraction effects and then parallel processing of RF signals can be realized by using of the characteristics that diffraction efficiencies(DEs)are approximately in direct proportion to RF signals intensities and diffraction angles are related to frequencies of the corresponding RF signals within linear MO interaction region.In this paper,studied is the multifrequency MO Bragg diffraction in first-order MO interaction approximation,and obtained was the approximate analytical expression for principle diffraction efficiency(PDE).Also,put forward was a parallel imaging method of relative intensity of RF signals based on single-frequency diffraction.By calculation and analysis,it is shown that the relative error is not more than 0.3dB for the case of three RF signals within the frequency space of 60MHz.

不同产地蓝铜矿矿物学及谱学特征研究

蓝铜矿是含铜的碳酸盐矿物,它产于铜矿床的氧化带,是一种次生矿物,因此蓝铜矿的出现可作为寻找原生铜矿床的标志。国内学者对蓝铜矿的谱学研究比较少,且对世界不同著名产地蓝铜矿矿物学与谱学特征对比是空白区。通过扫描电镜能谱分析仪、粉晶X射线衍射仪、同步热分析仪、红外光谱仪等仪器对2块中国产地蓝铜矿矿物样品(安徽六峰山、广东阳春)与2块外国产地蓝铜矿矿物样品(老挝、澳大利亚)的成分、结构及谱学特征进行了分析与探讨。能谱元素分析结果显示4块矿物样品的主要元素为C、O、Cu三种元素。X衍射结果表明除产于安徽六峰山矿物外,其他3种产地矿物X衍射物相分析结果均为蓝铜矿Cu_(3)(OH)_(2)(CO_(3))_(2)。产于安徽六峰山矿物除了主物相蓝铜矿的衍射峰外,在其他位置也检测出衍射峰,表明产于安徽六峰山的矿物含有第二物相孔雀石CuCO_(3)·Cu(OH)_(2)。从同步热分析仪热重曲线可以看出主要有两个失重台阶,300℃之前的失重可能是蓝铜矿中含有小部分的孔雀石的分解失重,而300~600℃的失重对应的是蓝铜矿的分解失重。从红外光谱上看主要的红外峰为蓝铜矿的特征峰,四个不同产地的红外光谱比较相似。结合蓝铜矿的外观特征,可为不同产地蓝铜矿的产地鉴定和检测提供依据。

Leaching behavior of phosphorous compounds from sewage sludge ash based on quantitative X-ray diffraction analysis

Phosphorus(P)is an essential and limited resource.Incineration sewage sludge ash(ISSA)contains a high amount of P,which can be recovered using chemical leaching methods.However,the recovery ratio depends on the speciation of P and the leaching conditions.In this study,hydrochloric acid was used as a leaching agent,and the effects of the hydrochloric acid concentration,leaching time,temperature,and liquid-solid ratio on the P leaching ratio were investigated.Furthermore,the co-leaching of macro-metals Ca,Al,Fe,and Mg was analyzed.The results showed that P leached rapidly within 30 min,where the leaching rate reached more than 80%and then gradually stabilized.The leaching concentrations of Ca and Mg had a significant correlation(correlation coefficient r^(2)>0.90),and both were leached completely.Al and P had similar leaching patterns,where the leaching rates increased initially and then decreased with time at 0.2 mol/L HCl.According to X-ray diffraction analysis and Rietveld refinement,the P in ISSA was mainly present in the forms of Mg_(3)Ca_(3)(PO_(4))_(4) and AlPO_(4).When leached using 0.2 mol/L HCl at 55℃ with a liquid-to-solid ratio of 20 L/kg,the AlPO_(4) and Fe_(3)(H_(2)O)_(3)(PO_(4))_(2) in ISSA dissolved initially and then precipitated on the surface of the solid phase,thereby impeding further P leaching.

SEPARATION OF DIASTEREOISOMERSNEOCLAUSENAMIDE AND ISONEOCLAUSEAMIDE AND X-RAY DIFFRACTION ANALYSIS

Neoclausenamide with lowering effect on the elevated SGPT levels was isolated from leaves of Clausena Lansium (lour) Skeels. Its content in the plant is less than 0.01%. For more intense pharmacological studies, larger amount of

物相定性分析的综合实验设计与实践

物相定性分析主要用来判定物质组成及其存在状态,是材料、化工和地质等学科专业学生必须掌握的综合性实验技能。为培养学生对材料的物相分析测试能力,设计了未知粉末物相定性分析的综合实验。以氧钼矿、黑铜矿、斜锆石和六方软锰矿的混合粉末作为盲样,依据X射线衍射和能谱元素结果,通过实验数据和综合解析推导,撰写实验分析报告,全面提高学生的仪器操作和数据分析能力。

基于Cook距离的阻尼多道奇异谱分析分离绕射波

地震绕射是提升小尺度不规则地质体成像横向分辨率的重要手段。常规地震记录中的绕射波会被能量强的反射波掩盖,因此需要分离出绕射波并成像。阻尼多道奇异谱分析是一种秩约束类的去噪方法,其原理为地震数据经过Hankel变换后做奇异值分解,反射波和绕射波分别对应着数值较大和较小的奇异值。然而该算法依赖人工确定反射波场的秩,不适用于海量地震数据处理。为了克服人工选择奇异值的问题,提出使用Cook距离作为自动计算反射波场秩的解决方案。将Cook距离和阻尼多道奇异谱分析算法相结合以实现反射和绕射波分离。模拟共炮检距道集和叠后实际数据实验表明,该方法能够有效获得高质量绕射波场。