A study on some elements and their phases in sediments of Changjiang Estuary by X-ray spectrometer and X-ray diffractometer

INTRODUCTIONThe studies on the quantitative distribution of the conventional elements and their phases in the sediments of the Changjiang Estuary are of great importance to the understanding of the chemical processes of ion exchange, absorption, desorption and flocculation in the estuary.

Radiological and X-Ray Diffraction Characterization of Bauxite and Rutile Ore Contaminated Environment in Kanam and Wase Mineral Exploration Sites, Plateau State-Nigeria

Two non-destructive analytical techniques (gamma spectrometer and X-ray diffractometer) were employed in the analysis of bauxite and rutile ore and their vicinity soil and control sourced within the Kanam and Wase mineral exploration sites. The activity concentrations of natural radionuclides 238U, 232Th, and 40K in the soil samples received from bauxite and rutile mineral mining vicinities revealed high concentrations of 238U, 232Th, and 40K compared to the control soil samples sourced 500 m away from the mineral exploration vicinities. Radiological detriments RLI, AUI, Hin and Hex unveiled values exceeding the radiation standard concentration (>1) for soil. X-ray diffraction characterization of bauxite ore revealed the interlocking minerals of Bauxite (18)%, Albite (11)%, Garnet (15)%, Illite (6)% and Muscovite (43)% in various proportions obtained within the 2θ range (9.18 to 64.4) and a peak value (intensity, cps) of 3400. Pure bauxite percentage in the ore meets metallurgical grade (15 - 25)%. X-ray diffraction of rutile ore revealed the minerals of rutile (40)%, quartz (21.4)%, ilmenite (27)% and garnet (11.8)% found within the 2θ range (27.5 to 35.6) and a peak value intensity of 31.1 - 100.0 cps also meeting the metallurgical grade of 15% - 25%. The major environmental concern associated with the mineral-sands industry is the radiation hazards, pollution of ground-water sources from heavy metals, mineral transport with heavy equipment’s, dredging operations in fragile coastal area and clearing of vegetation.

In situ observation of the phase transformation kinetics of bismuth during shock release

A time-resolved x-ray diffraction technique is employed to monitor the structural transformation of laser-shocked bismuth.Results reveal a retarded transformation from the shock-induced Bi-Ⅴphase to a metastable Bi-Ⅳphase during the shock release,instead of the thermodynamically stable Bi-Ⅲphase.The emergence of the metastable Bi-Ⅳphase is understood by the competitive interplay between two transformation pathways towards the Bi-Ⅳand Bi-Ⅲ,respectively.The former is more rapid than the latter because the Bi-Ⅴto B-Ⅳtransformation is driven by interaction between the closest atoms while the Bi-Ⅴto B-Ⅲtransformation requires interaction between the second-closest atoms.The nucleation time for the Bi-Ⅴto Bi-Ⅳtransformation is determined to be 5.1±0.9 ns according to a classical nucleation model.This observation demonstrates the importance of the formation of the transient metastable phases,which can change the phase transformation pathway in a dynamic process.

Method for Measuring Residual Stresses Induced by Boring in Internal Surface of Tube and Its Validation with XRD Method

Residual stresses can have a strong effect on the usability of machined parts,and the X-ray diffraction(XRD)measuring equipment,which is commonly used to measure residual stresses,is very expensive.This paper presents a method of measuring the residual stresses induced by boring in the internal surface of a tube with much cheaper equipment.The method,called the strain-based method is mainly based on the strains measured on the external surface of the tube.It is proposed on the basis of the very long tube assumption.The finite element method(FEM)analysis is thus used to validate the length of the tube.Guided by the FEM results,an appropriate length of the tube is chosen,and the residual stresses are obtained from both the strain-based method and the XRD method.Stress profiles obtained from both two methods are compared.The comparison result indicates that the profiles of the two methods agree well with each other.Therefore,it can be concluded that the accuracy of the strain-based method is high enough,and it can be applied to residual stress measurement in practice.

Understanding the influence of petrographic parameters on strength of differently sized shale specimens using XRD and SEM

Ground failure is a major contributor to fatalities in underground mines in the US.Underground coal mines in the Northern Appalachian have weak roof rock composed of shale,which is prone to failure under high horizontal stress.Understanding the relationship among strength,specimen size and rock petrographic parameters is essential for developing an effective ground control plan.Size effect studies have found that rock strength varies with specimen size.This paper attempts to understand this strength variation using three specimen sizes(254-mm,508-mm,and 762-mm).The specimen strength was measured and the major petrographic parameters affecting the strength,namely grain size,grain shape,quartz content,clay content,etc.were analyzed using X-ray diffraction(XRD)and scanning electron microscopy(SEM).The petrographic parameters were then correlated with the strength of the three differently sized specimens.The results showed that 508-mm specimen had the lowest strength.Quartz content of the 508-mm specimen was lower than that of 254-mm and 762-mm specimens.Clay content and average grain size of the 508-mm specimen were higher than those of 254-mm and 762-mm specimens.These results clearly show that grain size,quartz content and clay content contribute to strength variation observed in differently sized shale specimens.

Characterization of Average Molecular Structure of Heavy Oil Fractions by ~1H Nuclear Magnetic Resonance and X-ray Diffraction

The chemical structure of heavy oil fractions obtained by liquid-solid adsorption chromatography was character-ized by 1 H nuclear magnetic resonance and X-ray diffraction.The molecular weight and molecular formula of asphaltene molecules were estimated by combining 1 H nuclear magnetic resonance and X-ray diffraction analyses,and were also ob-tained from vapor pressure osmometry and elemental analysis.Heteroatoms,such as S,N,and O atoms,were considered in the construction of average molecular structure of heavy oils.Two important structural parameters were proposed,including the number of alkyl chain substituents to aromatic rings and the number of total rings with heteroatoms.Ultimately,the av-erage molecular structures of polycyclic aromatics,heavy resins and asphaltene molecules were constructed.The number of α-,β-,γ-,and aromatic hydrogen atoms of the constructed average molecular structures fits well with the number of hydro-gen atoms derived from the experimental spectral data.

Fitting Full X-Ray Diffraction Patterns for Quantitative Analysis: A Method for Readily Quantifying Crystalline and Disordered Phases

Fitting of full X-ray diffraction patterns is an effective method for quantifying abundances during X-ray diffraction (XRD) analyses. The method is based on the principal that the observed diffraction pattern is the sum of the individual phases that compose the sample. By adding an internal standard (usually corundum) to both the observed patterns and to those for individual pure phases (standards), all patterns can all be normalized to an equivalent intensity based on the internal standard intensity. Using least-squares refinement, the individual phase proportions are varied until an optimal match is reached. As the fitting of full patterns uses the entire pattern, including background, disordered and amorphous phases are explicitly considered as individual phases, with their individual intensity profiles or “amorphous humps” included in the refinement. The method can be applied not only to samples that contain well-ordered materials, but it is particularly well suited for samples containing amorphous and/or disordered materials. In cases with extremely disordered materials where no crystal structure is available for Rietveld refinement or there is no unique intensity area that can be measured for a traditional RIR analysis, full-pattern fitting may be the best or only way to readily obtain quantitative results. This approach is also applicable in cases where there are several coexisting highly disordered phases. As all phases are considered as discrete individual components, abundances are not constrained to sum to 100%.

X-Ray Analysis by Williamson-Hall and Size-Strain Plot Methods of ZnO Nanoparticles with Fuel Variation

In this paper, a simple and facile surfactant assisted combustion synthesis is reported for the ZnO nanoparticles. The synthesis of ZnO-NPs has been done with the assistance of non-ionic surfactant TWEEN 80. The effect of fuel variations and comparative study of fuel urea and glycine have been studied by using characterization techniques like X-ray diffraction (XRD), transmission electron microscope (TEM) and particle size analyzer. From XRD, it indicates the presence of hexagonal wurtzite structure for ZnO-NPs. Using X-ray broadening, crystallite sizes and lattice strain on the peak broadening of ZnO-NPs were studied by using Williamson-Hall (W-H) analysis and size-strain plot. Strain, stress and energy density parameters were calculated for the XRD peaks of all the samples using (UDM), uniform stress deformation model (USDM), uniform deformation energy density model (UDEDM) and by the size-strain plot method (SSP). The results of mean particle size showed an inter correlation with W-H analysis, SSP, particle analyzer and TEM results.

X-Ray Diffraction, Electron Paramagnetic Resonance and Optical Absorption Study of Bauxite

The bauxite mineral obtained from Araku, Vishakapatnam district of Andhra Pradesh, India is used in the present work. Structural characterization was performed by X-ray diffraction (XRD). The mineral was found to be gibbsite in phase. The transitional metal ions present were investigated using electron paramagnetic resonance (EPR) and optical absorption spectra. The EPR results suggest that Fe3+ has replaced Al3+ in the unit cell of bauxite. The optical absorption spectrum is due to Fe3+ which indicates that it is in distorted octahedral environment. The near-infrared (NIR) spectrum is due to water fundamentals and combination overtones, which confirm the formula of the compound. The impurities in the mineral are identified using spectroscopic techniques.

A combined IR and XRD study of natural well crystalline goethites(α-FeOOH)

Goethite(a-FeOOH)is one of the most abundant minerals on the Earth surface,occurring in temperate,tropical and equatorial climates.Fe in goethite can be substituted by many cations such as Al,Ni for instance.A large amount of research has been conducted on the effect of varying elemental compositions(mainly Al-content)on the spectral features of goethites with most of the studies based on materials synthesized with different elemental ratios.The different elemental ratios,however,may not only affect the composition of the products but also their crystallinity and/or particle size and shape.Both parameters are known to affect results of both X-ray diffraction(XRD)and infrared spectroscopy(IR).These methods are predominantely used to characterize goethites.In the present study,therefore,a significant set of natural goethites was considered in order to investigate the effect of elemental composition on XRD and IR results.The focus was on crystallised samples which had a limited chemical variability but artefacts caused by the presence of admixtures could be excluded in most cases.First of all Rietveld refinement was optimized based on varying different parameters.A fairly good correlation of Rietveld derived crystallite sizes and specific surface area determined by N-adsorption(SSA)was found which proves the importance of considering the crystallite size parameters for Rietveld refinement and at the same times proves the quality of it.Using IR spectroscopy yet published relations of band position and Al-content could be confirmed despite the fact that the range of Al-contents was small.However,the band position of the Fe–O stretching,previously used as proxy for crystallinity assessment,was found to be least variable hence contradicting yet published results.Controversial results were also published for the effect of the Al-content on the position of the asymmetric FeOH stretching band at 450 cm.The goethites investigated in the present study indicate that the crystallite size determines the band position rather than the Al-content which is at least valid for the limited range of Al-contents.The results of the present study indicate that using synthetic sample sets bears the problem that more than one parameter might show systematic differences(e.g.crystallite size in a set of chemically varied goethites).The paper,therefore,provides IR reference data based on a set of natural well crystallised goethites.

Soil Clay Mineralogical Phase Analysis of Ganges Floodplain Soils by XRD and XRF

Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements in soils. It is also essential for the soil-plant interaction purpose. To identify soil mineral phases especially clay minerals, X-ray diffraction (XRD) has been a popular technique. The clay mineralogical information of soils in Bangladesh is limited, especially in Ganges flood plain region (Agro Ecological Zone (AEZ) 12 and 13). Therefore, to overcome this limitation, in this study, we performed XRD analysis of <2 mm fractions soil samples of AEX 12 and 13. However, identifying mineralogical phases by XRD in <2 mm fractions soils is not so straight-forward due to many practical problems. We fully matched only two mineralogical phases in all the soil samples which is quartz and potassium-Aluminum-Silicate. However, the full XRD peaks indicate that more minerals are also present, but due to heterogeneity of soils samples, it is difficult to find other minerals phases by only XRD peak of <2 mm fractions. Therefore, to find more information about mineralogical phases, we performed XRF analysis that provides the elemental composition of minerals phase as oxide. XRF analysis indicated the presence of secondary minerals like illite and chlorite. The presence of high percentage Fe oxide not only indicated the iron mineral phase (goethite and ferrihydrite) but also indicated iron rich high charge smectite minerals (beidellite). The presence of iron rich smectite minerals in the Ganges sediments reported in several previous studies. Thus, we concluded that only XRD in <2 mm fractions of soils is not adequate to identify the mineralogical phases of soil samples. Others analyses like XRF, XRD in <2 μm fractions will be necessary to locate an entire image of soil mineralogical phases.

Mossbauer,X-Ray and Magnetic Studies of Black Sand from the Italian Mediterranean Sea

The study of natural magnetic sands is instrumental to investigate the geological aspects of their formation and of the origin of their territory. In particular, Mossbauer spectroscopy provides unique information on their iron content and on the oxidation state of iron in their mineral composition. The Italian coast on the Mediterranean Sea near Rome is known for the presence of highly magnetic black sands of volcanic origin. A study of the room temperature Mossbauer spectrum, powder X-ray diffraction, energy dispersive X-ray spectroscopy, and magnetic measurements of a sample of black magnetic sand collected on the seashore of the town of Ladispoli is performed. This study reveals magnetite as main constituent with iron in both tetrahedral and octahedral sites. Minor constituents are the iron minerals hematite and ilmenite, the iron containing minerals diopsite, gossular, and allanite, as well as ubiquitous sanidine, quartz, and calcite.

钢渣粉/聚酯纤维沥青混合料水稳定性研究

为了实现钢渣粉在沥青路面中的可持续利用,同时结合河南省冬季冰雪天气下路面的除冰情况,研究了掺有聚酯纤维与钢渣粉沥青混合料的水稳定性。制备4种聚酯纤维掺量(0、0.3%、0.4%、0.5%)AC-13沥青混合料开展复盐(掺量配比为NaCl∶CaCl2∶CH2COONa=1∶1∶2)冻融循环劈裂试验,结果表明聚酯纤维掺量为0.4%时,沥青混合料水稳定最好;在最佳纤维掺量下制备5种替代率(0、25%、50%、75%、100%)钢渣粉沥青混合料,采用冻融劈裂抗拉强度比(freeze-thaw splitting tensile strength ratio,TSR)确定最佳钢渣粉替代率为75%,混合料水稳定性最佳;通过冻融腐蚀因子K评价沥青混合料的抗侵蚀性能,结果表明:聚酯纤维/钢渣粉沥青混合料的抗侵蚀性能最强,聚酯纤维沥青混合料次之,普通石灰岩沥青混合料最弱。通过电镜扫描(scanning electron microscope,SEM)、X射线衍射(X-ray diffraction,XRD)技术探索钢渣粉/聚酯纤维沥青混合料界面黏附作用的改性机理。微观分析表明:掺量为0.4%的聚酯纤维形成的纤维网状结构以及沥青、钢渣粉(75%的替代率)和矿粉三者存在界面能量作用可以很好地改善沥青混合料的水稳定性。

Microstructural origins of high strength of Al-Si alloy manufactured by laser powder bed fusion:In-situ synchrotron radiation X-ray diffraction approach

The microstructural factors contributing to the high strength of additive-manufactured Al-Si alloys us-ing laser-beam powder bed fusion(PBF-LB)were identified by in-situ synchrotron X-ray diffraction in tensile deformation and transmission electron microscopy.PBF-LB and heat treatment were employed to manufacture Al-12%Si binary alloy specimens with different microstructures.At an early stage of de-formation prior to macroscopic yielding,stress was dominantly partitioned into the α-Al matrix,rather than the Si phase in all specimens.Highly concentrated Si solute(~3%)in the α-Al matrix promoted the dynamic precipitation of nanoscale Si phase during loading,thereby increasing the yield strength.After macroscopic yielding,the partitioned stress in the Si phase monotonically increased in the strain-hardening regime with an increase in the dislocation density in the α-Al matrix.At a later stage of strain hardening,the flow curves of the partitioned stress in the Si phase yielded stress relaxation owing to plastic deformation.Therefore,Si-phase particles localized along the cell walls in the cellular-solidified microstructure play a significant role in dislocation obstacles for strain hardening.Compared with the results of the heat-treated specimens with different microstructural factors,the dominant strengthening factors of PBF-LB manufactured Al-Si alloys were discussed.

Mechanical properties and acoustic emission characteristics of thick hard roof sandstone in Shendong coal field

The mechanical properties and acoustic emission characteristics of thick hard roof sandstone were investigated. Samples were taken from the 30.87-m thick sandstone roof in a mine in the Shengdong coal field, China. Firstly, the composition and microscopic characteristics were analyzed by XRD and FE-SEM, respectively. Moreover, the indirect tensile test, uniaxial compression test, three axis compression experiment and AE test are carried out by using RMT-150C mechanics experiment system with DSS-8B AE test system. The experiment results indicate that the main framework particles of sandstone are quartz and feldspar, and mainly quartz. Cements are mainly pyrite, kaolinite, chlorite and zeolite cross needle, clinochlore, and clay minerals. The microstructure of sandstone is very dense, with few pores and high cementation degree. The tensile strength, compressive strength and elastic modulus of sandstone are 4.825, 85.313 MPa, 13.814 GPa, respectively, so the sandstone belongs to hard rock. The AE cumulative counts of sandstone can be divided into three phases： relatively flat growth period, rapid growth period and spurt period. The signal strength of AE waveform can be used as a warning signal. In the tensile fracture zone, the warning value is 0.4 mV, and in the compression shear failure zone, it is 4 mV. The numbers of cumulative counts of AE under different stress conditions have obvious difference. Moreover, the growth of cumulative counts of acoustic emission is more obvious when the stress is more than 60% of the peak stress.

O_2/CO_2气氛下醋酸调质石灰石直接硫化实验研究

提出了采用醋酸溶液调质石灰石的方法来提高其直接硫化反应过程中的固硫能力。实验研究了醋酸浓度、温度、SO2浓度等参数对醋酸调质前后2种石灰石在硫酸化过程中钙转化率的影响规律,并采用氮吸附和X射线衍射(X-ray diffractometer,XRD)技术对石灰石及其硫化产物进行了分析。结果表明:调质改善了石灰石的孔结构特性,在直接硫化过程中比原始石灰石具有更高的钙转化率;在所实验的温度范围内,调质石灰石都可获得很高的钙转化率;随SO2浓度增大,直接硫化反应速率升高,调质石灰石钙转化率增大;随醋酸浓度增大,调质石灰石的钙转化率提高,提高幅度因石灰石种类而异,采用浓度为50%醋酸溶液作为调质剂可达到经济高效的目的;XRD图谱验证了醋酸调质石灰石直接硫化时钙转化率更高。

神府煤低温灰与高温灰的高温熔融特征

煤灰中无机组分在加热过程中的熔融特性,是评价煤炭对各种气化、燃烧工艺的适应性以及选择最佳操作条件的重要依据。以典型煤种神府煤为研究对象,采用热台显微镜、扫描电镜观察低温灰与高温灰在熔融过程的行为特征,并结合X射线衍射仪分析该过程煤中矿物质的转化。结果表明：低温灰与高温灰均以难熔物质Si O2为骨架向内收缩,熔融物增多后包裹难熔物质并逐渐将其熔解,分别形成辉石类和长石类共熔物。在800~1 000℃和1 100~1 200℃阶段,神府煤低温灰和高温灰的体积均有明显收缩。800~1 000℃阶段,低温灰中有斜辉石形成,高温灰中有钠长石形成;1 100~1 200℃阶段,两样品均熔融形成共熔物。

云母矿粉中游离二氧化硅含量的快速测定

以具有复杂晶体结构、X射线衍射峰与游离二氧化硅衍射峰严重重叠及易择优取向等特点的云母矿粉为研究对象,探讨了利用具有超能探测器的X射线衍射仪在连续扫描模式下收谱以及Rietveld全谱拟合快速测定其中游离二氧化硅含量的可行性。结果表明:与步骤复杂、测试周期长等的传统X射线衍射标准曲线法相比较而言,该方法不仅操作简便、收谱快速而且结果准确性高、重现性好。重现性测定的最大标准偏差为1.39%。实际样品测试也表明此方法是一种简便易行的测定各类粉尘中游离二氧化硅含量的好方法。

国产X射线衍射仪对金属变温测试的温度准确性验证

选用熔点为183℃的锡铅焊料(Sn63/Pb37)作为标准试样,验证国产X射线衍射仪对金属进行变温XRD测量时的温度准确性。结果表明:变温样品室内热电偶的监控温度(To)与锡铅焊料样品表面的实际温度(Ta)的偏差小于5℃,直接证实所开发的变温样品室具有较高的温度准确性。

宣城网纹红土成分与微结构的定量研究

网纹红土红色基质和白色网纹的成分和结构差异性影响并控制着工程特性。文章通过扫描电子显微镜(scanning electron microscope,SEM)实验和数字图像处理技术定量研究原状网纹红土的微孔隙特征,进而基于能量色散谱仪(energy dispersive spectrometer,EDS)和X射线衍射仪(X-ray diffractometer,XRD)分析了红色基质和白色网纹的化学成分和黏土矿物构成,以探讨网纹红土微结构和成分与其力学特征的内在联系。研究得出,网纹红土孔隙主要为小于0.5μm2面积的微孔隙,而面积超过50μm2的大孔隙则较少,但红色基质颗粒表面粗糙、棱角分明,主要由绿泥石/蒙脱石混层和伊利石以及少量的绿泥石和高岭石构成,而白色网纹颗粒则较为圆滑,由伊利石/蒙脱石混层和伊利石构成,且红色基质中Fe元素质量分数高于白色网纹,而两者中的Ti元素质量分数稳定。研究结果可为深入分析网纹红土工程特征提供依据。