Energy-dispersive X-ray Spectroscopy for the Quantitative Analysis of Pyrite Thin Specimens

To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantitative analysis of pyrite materials.Additionally,the k factor of pyrite is calculated experimentally.To develop an appropriate non-standard quantitative analysis model for pyrite materials,the experimentally calculated k factor is compared with that estimated from the non-standard quantitative analytical model of the instrument software.The experimental findings demonstrate that the EDS attached to a TEM can be employed for precise quantitative analysis of micro-and nanoscale regions of pyrite materials.Furthermore,it serves as a reference for improving the results of the EDS quantitative analysis of other sulfides.

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.

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.

Quantitative Phase Analysis Based on Rietveld Structure Refinement for Carbonate Rocks

QPA (Quantitative Phase Analysis) of carbonate rocks bearing calcite and dolomite using X-ray diffractometry (XRD) can be performed using the combined Rietveld Structure Refinement (RSR) and semiquantitative Reference Intensity Ratio (RIR) methods, providing an estimation of crystalline phase in a mixture. Different ratios of five samples were prepared by mixing these crystal minerals with high sensitively. The scan speeds, adequate to determine mineral phases in rock samples, were used as 6 degrees per minute with 0.08 steps. The XRD analysis with commercial TOPAS 3.0 program, defined by a new generation of profile and structure analysis software, based on RSR provides Bragg reflection profiles and the dimension of the unit cell of a phase. The weight fractions of each phase were found by Le Bail and Pawley methods in RSR using a pseudo-Voigt peak shape model. The samples were also characterized by using X-ray fluorescence (XRF) and atomic absorption spectrometer (AAS). These analyses were conducted to compare these results with those obtained from the RSR. In addition to these, RSR of phases is very important to improve the goodness of fit (GOF). Therefore, the discussions of refinement of the carbonate mixing were made and a refinement procedure was given for these mixing in detail. Taking advantage of the RSR with the addition of an internal standard, the phase fraction of all the crystalline phases as well as the amorphous component, has been accurately determined. RSR technique offers a valid support for the characterization of marble in the light of industrial products.

Automatic recognition and quantitative analysis of Ω phases in Al-Cu-Mg-Ag alloy

The main methods of the second phase quantitative analysis in current material science researches are manual recognition and extracting by using software such as Image Tool and Nano Measurer. The weaknesses such as high labor intensity and low accuracy statistic results exist in these methods. In order to overcome the shortcomings of the current methods, the Ω phase in A1-Cu-Mg-Ag alloy is taken as the research object and an algorithm based on the digital image processing and pattern recognition is proposed and implemented to do the A1 alloy TEM （transmission electron microscope） digital images process and recognize and extract the information of the second phase in the result image automatically. The top-hat transformation of the mathematical morphology, as well as several imaging processing technologies has been used in the proposed algorithm. Thereinto, top-hat transformation is used for elimination of asymmetric illumination and doing Multi-layer filtering to segment Ω phase in the TEM image. The testing results are satisfied, which indicate that the Ω phase with unclear boundary or small size can be recognized by using this method. The omission of these two kinds of Ω phase can be avoided or significantly reduced. More Ω phases would be recognized （growing rate minimum to 2% and maximum to 400% in samples）, accuracy of recognition and statistics results would be greatly improved by using this method. And the manual error can be eliminated. The procedure recognizing and making quantitative analysis of information in this method is automatically completed by the software. It can process one image, including recognition and quantitative analysis in 30 min, but the manual method such as using Image Tool or Nano Measurer need 2 h or more. The labor intensity is effectively reduced and the working efficiency is greatly improved.

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.

CORRELATION OF THE COMPONENTS OF PORTLAND CEMENT CLINKER AND SINTERING PROCESS BY MEANS OF XRD QUANTITATIVE ANALYSIS

In this paper, the cement clinkers from various industrial Kilns were investigated by a superposing peaks method for X-ray quantitative analysis (XRQA) of clinker minerals, the results show that the clinker mineral contents measured by XRQA method better accord with the reality of clinkers made in different conditions than theoretic contents calculated by Bouge formula do. The measured contents of C3S of clinkers manufactured in rotary kilns are higher than theoretically calculated values,whereas, the results of clinker man manufactured in shaft kilns are contrary to that. This is because in rotary kiln, the raw meals are fully pre-heated and have high sintering temperature, the clinkers are well solid-solutioned and rapidly cooled,on the contrary,owing to the struetural defects, it is easy to exist reducing atmosphere and lower temperature in shaft kiln,moreover the cooling rate is slower, all these can evidently Lead to worse clinker quality. Adding CaF2-Ca-SO4 complex mineralizer can remarkably modify the sintering situation in shaft kiln ,especially can evidently increase C3S content and make it well crystallized, therefore, im prove the sintered quality of clinker.

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.

Performance analysis of quantitative phase retrieval method in Zernike phase contrast X-ray microscopy

Since the invention of Zernike phase contrast method in 1930,it has been widely used in optical microscopy and more recently in X-ray microscopy.Considering the image contrast is a mixture of absorption and phase information,we recently have proposed and demonstrated a method for quantitative phase retrieval in Zernike phase contrast X-ray microscopy.In this contribution,we analyze the performance of this method at different photon energies.Intensity images of PMMA samples are simulated at 2.5 keV and 6.2 keV,respectively,and phase retrieval is performed using the proposed method.The results demonstrate that the proposed phase retrieval method is applicable over a wide energy range.For weakly absorbing features,the optimal photon energy is 2.5 keV,from the point of view of image contrast and accuracy of phase retrieval.On the other hand,in the case of strong absorption objects,a higher photon energy is preferred to reduce the error of phase retrieval.These results can be used as guidelines to perform quantitative phase retrieval in Zernike phase contrast X-ray microscopy with the proposed method.

焊缝缺陷三维成像及亚像素定量方法研究

为实现工业设备中焊缝结构内部缺陷准确地定量分析,针对构造缺陷三维重构模型时缺陷图谱的过分割和欠分割导致定量分析不够精确的问题,提出了一种基于图谱颜色分割的新算法。利用该算法处理缺陷切片并进行三维重构获取其长度,应用Canny算子与三次样条插值法结合获取缺陷亚像素边缘,基于缺陷区域连通标记算法和累加法可获取缺陷面积和体积的方法。研究结果表明:与实际数据对比,未焊透、未熔合、夹渣缺陷重构的长度误差分别为8.18%、5%、9.62%,基于此对分割缺陷的亚像素边缘内连通域进行标记以准确地获取其面积及体积。该方法能够在不破坏焊缝结构的情况下即时获取焊缝内部缺陷的形貌并对其进行精准且全面的定量分析。

固相萃取-一标多测高效液相色谱法测定化妆品中5种苯并三唑类防晒剂

建立了固相萃取技术结合高效液相色谱测定化妆品中5种苯并三唑类防晒剂的一标多测定量分析方法。该方法待测样品使用HLB固相萃取小柱净化处理,以亚甲基双-苯并三唑基四甲基丁基酚为内参物,通过建立该物质与另外4种物质的相对校正因子,计算出各物质的含量。研究了不同进样量、不同流动相流速及不同柱温对相对校正因子的影响,比较了一标多测法和外标法的计算结果。结果表明,5种物质的线性关系良好(R^(2)≥0.9997),检测限和定量限分别为4.00~26.43μg/L和10.00~60.42μg/L;各物质的相对校正因子重复性较好,其相对标准偏差(RSD)为0.25%~1.16%;两种方法计算结果无明显差异,其相对平均偏差(RAD)为0.12%~2.19%。该方法操作简单,使用标准物质少,检测效率高,可用于化妆品中5种防晒剂的含量测定和质量控制。

地磁感应电流作用下三相五柱变压器无功功率定量分析

无功功率作为电力系统运行重要指标,其波动影响电力设备的安全稳定运行以及整个系统的电压稳定。为分析三相五柱变压器在地磁感应电流作用下的无功功率分布,根据变压器的实际参数,通过串联电阻及电压补偿的办法,建立三相五柱变压器磁场-电路耦合有限元计算模型,对不同大小地磁感应电流下的变压器无功功率进行定量分析。通过计算三相五柱空载及额定负载下无功功率的分布以及单相自耦变压器无功功率,发现随着地磁感应电流的增大,三相五柱空载及负载无功功率特性曲线均大体呈线性增加,且单相自耦变压器相较于三相五柱变压器无功曲线对于地磁感应电流更为敏感。并结合不同芯柱结构变压器的磁路特点,分析了无功差异变化的原因。研究结果可为地磁感应电流作用下三相五柱变压器稳定运行提供参考依据。

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.

Quantitative Phase Analysis of the Calcium Silicate Slag as the Residue of Extracting Alumina from High-Alumina Fly Ash

Calcium silicate slag is the residue of process of pre-desilication alkali lime sintering applied in the high-alumina fly ash to extract the alumina.The quantitative phase analysis(QPA) of the calcium silicate slag has been performed by the Rietveld method based on the powder X-ray diffraction(XRD) with the aid of noncommercial software GSAS-EXPGUI.A known weight of crystalline internal standard(10% CaF_2) was added to the calcium silicate slag to calculate the fraction of amorphous phase and other crystalline phases on an absolute basis.Besides,the calcium silicate slag was characterized by X-ray fluorescence(XRF) and thermo gravimetric(TG) differential scanning calorimetry(DSC) to test the QPA results and investigate its other characters.Finally,the results show that the amorphous fraction is 17.5%(hereinafter,the percentages refer to the mass fraction),and the major crystalline phases detected in the calcium silicate slag consist of 23.5% Beta-Ca_2 SiO_4,10.0% bredigite,10.3% Ca_3Al_2O_6(C_3A) and 21.6% CaCO_3.

Quantitative analysis results of CE-1 X-ray fluorescence spectrometer ground base experiment

As the nearest celestial body to the earth, the moon has become a hot spot again in astronomy field recently. The element analysis is a much important subject in many lunar projects. Remote X-ray spectrometry plays an important role in the geochemical exploration of the solar bodies. Because of the quasi-vacuum atmosphere on the moon, which has no absorption of X-ray, the X-ray fluorescence analysis is an effective way to determine the elemental abundance of lunar surface. The CE-1 X-ray fluorescence spectrometer （CE-1/XFS） aims to map the major elemental compositions on the lunar surface. This paper describes a method for quantitative analysis of elemental compositions. A series of ground base experiments are done to examine the capability of XFS. The obtained results, which show a reasonable agreement with the certified values at a 30% uncertainty level for major elements, are presented.

硫酸盐-氯盐环境下粉煤灰-水泥砂浆物相演变及定量分析

为了分析硫酸盐-氯盐环境下的水泥基材料的物相演变规律,本工作粉煤灰-水泥砂浆为研究对象,开展腐蚀溶液中的长期浸泡实验,并通过QXRD、SEM、MIP微观测试,分析砂浆中氯离子和硫酸根离子的交互作用、物相演变规律以及微结构变化。结果表明:在硫酸盐-氯盐侵蚀前、中期,离子间竞争作用导致侵蚀产物含量降低,延缓了试件中氯盐和硫酸盐的侵蚀进程;侵蚀后期,试件中侵蚀产物累积造成孔结构劣化,导致更多离子进入其内部,加速氯盐和硫酸盐侵蚀进程,此时,氯盐的存在不能再延缓硫酸盐的侵蚀。

啤酒花挥发性有机化合物及感官特征分析

为明确不同品种啤酒花挥发性有机化合物(VOCs)及感官特征差异,采用气相色谱-离子迁移谱(gas chromatography-ion mobility spectroscopy,GC-IMS)、气相色谱-质谱(gas chromatography mass spectrometry,GCMS)及定量描述分析(quantitative description analysis,QDA)对德国马革努门(Magnum)、美国芭乐西(Palisade)、捷克萨兹(Saaz)及德国赫斯布鲁克(Hersbrucker)四种不同品种啤酒花进行挥发性有机化合物(VOCs)及感官特征分析。结果显示,啤酒花具有柑橘类水果香、非柑橘类水果香、木质香、花香、草本、辛辣及生青味的香气属性,且不同品种啤酒花感官特征存在差异。GC-IMS共解析出79种VOCs,包括萜类、醇类、酯类、醛类及酮类等化合物。GC-MS共解析出140种VOCs,包括萜类、醇类、酮类、酯类、酸类、醛类等化合物,其中萜类和酯类化合物为啤酒花中含量最高的化合物种类。对不同品种啤酒花VOCs进行主成分分析(principal component analysis,PCA),有效鉴别出啤酒花品种之间差异性。该研究为啤酒花挥发性有机化合物(VOCs)及感官特征差异分析提供了参考方法,并为啤酒花在啤酒中的精准应用提供了理论支持。

多晶X射线衍射在石油炼制与化工催化剂研究中的应用

在石油化工领域,多晶X射线衍射是一种最有效、应用最广泛的研究催化材料晶体结构的分析方法。简要介绍了X射线衍射技术的基本原理。重点从物相定性/定量分析对催化材料组成确定、相对结晶度的现行标准及其对分子筛水热环境下结构变化的研究、晶胞参数的现行标准及其对催化活性中心的辨识、晶粒大小测定方法及其对反应扩散的影响等多个方面综述了近年来X射线衍射基础方法在石油炼制与化工催化剂研究中的应用,并阐明了这些方法的注意事项及适用范围。此外,介绍了中石化石油化工科学研究院有限公司在该领域取得的研究进展。并对X射线衍射技术在技术升级、机器学习、原位表征及联用技术等4个方面的发展进行了展望。