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1.
X射线荧光光谱法在耐火材料成分分析中的应用   总被引:4,自引:1,他引:4       下载免费PDF全文
李国会  徐国令  李晓莉 《岩矿测试》2003,22(3):217-220224
采用熔融法制样,用X射线荧光光谱法对耐火材料中的Na2O、MgO、Al2O3、SiO2、K2O、CaO、TiO2、Cr2O3、MnO、Fe2O3、ZrO2、HfO2组分进行测定,使用康普顿散射线作内标和经验系数法校正基体效应,经标准物质检验与标准值吻合,大部分组分的RSD<5%(n=10)。  相似文献   

2.
X射线荧光光谱测定矿样中主元素及微量元素   总被引:1,自引:0,他引:1  
X射线荧光光谱是一种多元素分析的有效方法。通常对粉末样品(180目以上),可以直接压片成型进行分析测量。为提高地球化学样品中主元素的准确度,更有效地消除矿样的颗粒效应,在制样前用理学盘式振动磨研磨二分钟,然后压片成型。各元素的基体影响可采用经验系数法,利用理学DATAFLEX-151B计算机软件进行元素间的基体效应校正,选择最佳测试条件,在日本理学3080E3型全自动X射线荧光仪上测定SiO_2、Al_2O_3、Fe_2O_3、CaOMgO、K_2O、Na_2O、V、Cu、Cr、Ni、Sr等24元素。方法具有简单、快速、成本低和效率高等优点,并有较好的准确度和精密度。  相似文献   

3.
较低稀释比熔融制样X射线荧光光谱法分析铬铁矿   总被引:3,自引:3,他引:0  
铬铁矿属难熔矿物,目前对铬铁矿的分析以化学分析为主,方法成熟,但操作麻烦且步骤繁琐;而应用X射线荧光光谱法进行分析测定,一般都采用较高稀释比熔融制样,不利于低含量元素的测定。本文选用四硼酸锂+偏硼酸锂作为混合熔剂,与样品以20:1的稀释比熔融制样,利用波长色散X射线荧光光谱测定铬铁矿中多种元素(Cr、Si、Al、TFe、Mg、Ca、Mn)的方法。采用多种铬铁矿标准物质和人工配制标准物质制作工作曲线,理论α系数及康普顿散射内标法校正元素间的吸收-增强效应,方法精密度(RSD,n=10)为0.2%~5.3%。方法检出限低,如锰元素的检出限可低至60 μg/g;镁元素的检出限为225 μg/g,比文献采用高稀释比XRF测定的方法检出限(250 μg/g)要低。本方法通过选择有效的熔剂和较低的稀释比解决了铬铁矿的制样问题,熔剂的用量减少,称样量增加,提高了低含量元素分析的准确度,相应地降低了分析成本。  相似文献   

4.
X射线荧光光谱法同时测定铁矿石中主次量组分   总被引:4,自引:1,他引:3  
采用X射线荧光光谱法测定铁矿粉中的TFe(全铁量)、SiO2、Al2O3、P、S、CaO、MgO、MnO和TiO2等9个组分。以Li2B4O7和LiBO2(质量比67∶33)的混合熔剂熔融制样,将测量全铁量的内标Co2O3制备成均匀的Co玻璃粉,大大提高全铁量的测量准确度和精密度;加入LiNO3为氧化剂,解决了硫元素在制样过程中容易挥发的问题。与化学法相比,该法对铁矿石中主量和次量元素的测量结果满意,方法快速、简便、准确、精密度好。  相似文献   

5.
徐婷婷  夏宁  张波 《岩矿测试》2008,27(1):74-76
采用混合熔剂熔融制备样片,用Axios X射线荧光光谱仪测定海洋沉积物样品中SiO2、Al2O3、Fe2O3、MgO、CaO、Na2O、K2O、P2O5、TiO2、MnO、BaO、Ni、Cu、V、Cr和Zn等16种组分,用理论α系数校正基体效应,分析方法的精密度(RSD,n=12)为Cu和Cr小于6%,其余大多数主次量组分小于2%。方法用海洋沉积物国家一级标准物质验证,测定值与标准值相符。  相似文献   

6.
X射线荧光分析中最基本的测量是X荧光辐射的强度。在元素分析线角度处测得的强度并不都是样品中该元素的贡献,除元素分析线的强度(净强度)之外的计数统称为  相似文献   

7.
使用粉末样品压片制样,用Minipal 4便携式能量色散X射线荧光光谱仪测定化探样品尹的Na2O、MgO、Al2O3、SiO2、CaO、Fe2O3、K2O、As、Ba、Br、Ce、Co、Cr、Cu、Ga、La、Mn、Nb、Ni、P、Pb、Rb、Sr、Th、V、Y、Zn、Zr、Ti、Mo等30种组分。方法简便、快速,分析结果的精度和准确度能满足野外现场分析的要求。  相似文献   

8.
应晓浒  曹国洲 《岩矿测试》2003,22(3):221-224
采用熔融制样X射线荧光光谱法测定钠长石和钾长石中的Na2O、MgO、Al2O3、SiO2、P2O5、K2O、CaO、TiO2、Fe203、Rb、Sr、Y、Zr、Ba14个成分的含量,所得结果与化学分析结果相符,各组分测定33次的仪器RSD为0.10%~4.67%。在试验过程中,对功率为1kW和4kW的两种波长色散型X射线荧光光谱仪的灵敏度和检出限进行了比较,并对仪器的精密度和长期稳定性进行了考察。  相似文献   

9.
随着超细标准物质的研制,超细样品在地质分析中得到了进一步的应用。本文利用超高速行星式碎样机粉碎铬铁矿标准物质制成超细样品,采用粉末直接压片制样波长色散X射线荧光光谱测定铬铁矿中的多种元素(Cr、Si、Al、Fet、Mg、Ca、S、Co、Ni、V)。采用多种铬铁矿标准物质和人工配制标准物质制作工作曲线,经验系数和散射线内标法校正元素间的吸收-增强效应,方法精密度(RSD,n=10)为0.24%~2.95%。本方法有效地克服了样品的粒度效应,分析结果的精密度和准确度不低于化学法。  相似文献   

10.
X射线荧光光谱法同时测定石灰石中主次痕量组分   总被引:4,自引:2,他引:2  
采用熔融玻璃片和粉末压片法制样,选用标准样品,以经验α系数和散射线内标法校正元素谱线重叠干扰和基体效应,用ZSX PrimusⅡX射线荧光光谱仪对石灰石样品中CaO、Na2O、MgO、Al2O3、SiO2、K2O、TFe2O3、P2O5、TiO2、MnO和S等主次痕量组分进行测定,分析结果与标准值和化学值相符,12次测定的相对标准偏差小于10%。  相似文献   

11.
Phase Equilibria in the System CaCO3-MgCO3-FeCO3   总被引:4,自引:0,他引:4  
Experimental data on phase relations in the CaCO3-MgCO3-FeCO3ternary by Goldsmith et al. (1962) are inconsistent with thoseof Rosenberg (1967). These inconsistencies cannot be reconciledby the pressure or temperature differences between the two setsof experiments. Available reversed experiments on the binarysystems have been re-evaluated to yield consistent binary solvi.These data have been combined with analyses of natural carbonatesto yield approximate ternary phase diagrams at 250,400,550,and 700 ?C, and 4 to model ternary activity/composition relationsfor calcite- and dolomite-structure carbonates. An empiricalmodel for thermometry with calcite-ferroan dolomite was derivedfrom the ternary solvus by fitting an empirical equation tothe calcite limb of the ternary solvus. This model appears toextend reliably to higher iron contents than the models of Bickle* Powell (1977) and Powell et al. (1984).  相似文献   

12.
13.
The solvus on the Mn-rich side in the system MnCO3-CaCO3 was studied experimentally at 10 kb and lower pressures. The critical point lies at 540 °C and Mn0.68Ca0.32CO3. Reaction rates of demising are extremely sluggish. X-ray calibration curves for (Mn, Ca)CO3 solid solutions are given. Depicting microprobe analyses of about 300 carbonates from manganese calc silicate marbles affected by different degrees of metamorphism confirm the experimentally derived solvus.Margules parameters were derived from the experimental solvus, giving for spinodal unmixing W a=20.1+0.032·T and W b=18.3-0.0033·T, and for binodal unmixing W a=–22.9+0.035 ·T and W b=3.36+0.0147·T (All W, in kJ/-mol)A physical interpretation of the Margules parameters based on deformations of the ionic radii in the solid solution is presented. The Margules parameters obtained by this model agree fairly well with the experimental data.  相似文献   

14.
15.
 The order-disorder phase transitions in NaNO3 and CaCO3 are simulated by molecular dynamics. The simulations are based on the potentials calculated from the Gordon–Kim modified electron gas formalism extended to molecular ions. We successfully reproduced the transition temperature T c and the abnormally large c axis thermal expansion observed in experiment. The phase transitions in NaNO3 and CaCO3 were found to be initiated by ±60 and ±180° reorientation of the NO3 and CO3 ions about the c axis. The orientations of NO3 and CO3 ions are continuous with six preferred calcite-type orientations above the phase-transition temperature. Received: 30 January 2001 / Accepted: 11 May 2001  相似文献   

16.
徐琳  邹永廖  刘建忠 《矿物学报》2003,23(4):374-378
除了极少数非常陡峭的山脉与撞击坑和火山通道的峭壁外,整个月球表面几乎都被一层厚度不等的月尘、岩屑和岩块的混合堆积物即月壤所覆盖。由于月球无大气层等特殊环境,太阳光长驱直入,太阳风粒子直接注入到月壤细小颗粒上使月壤中富含稀有气体等太阳风粒子组分。本文在系统阐述月壤的形成过程与形成机制的基础上,分析了月壤中稀有气体的来源及其浓度与月壤的成熟度、月壤颗粒大小、月壤矿物组成和化学成分的相关关系,进而利用已有的探测数据和分析结果,对月壤中氦-3资源的开发利用前景进行了初步评估。  相似文献   

17.
超临界流体中MoO3与WO3溶解度实验探讨   总被引:1,自引:1,他引:1  
超临界地质流体以其独特的性质对金属成矿元素具有超强的萃取、层析和搬运能力,在热液矿床成矿机制研究中对揭示成矿物质的源、流和汇起着特殊和重要作用。本文利用分析纯H2MoO4在高温下脱水制备了MoO3(白色斜方晶系),在冷封式高压釜中实验测定了417℃超临界条件下,MoO3在纯水中的溶解度分别为7.3(29MPa)、14.2(45MPa)、21.6(55MPa)、27.7(78MPa)、32.5(100MPa)、和34.2(150MPa)mmol/l,热液中钼的存在形式为H2MoO4。依据前人的实验方案,补充测定了WO3在4.0%NaCl水溶液中于450%条件下的溶解度,其值分别为27.51(50MPa)和30.52(100MPa)mmol/l。结合前人研究结果发现,MoO3、WO3的溶解度在临界区域内具有超临界现象,在超临界条件下其溶解度与石英的超临界溶解度行为基本相似,表现为溶解度随体系温度和压力的升高而增大,这对揭示岩浆热液型和石英脉型钨、钼矿床的形成机制具有重要指导作用。  相似文献   

18.
Wollastonite transforms to a triclinic high-pressure polymorph, wollastonite II, at pressures > 25 kb. The equilibrium boundary [P(bars)=-4.7×T°C+32.810] has a rather flat negative P-T slope. The rapid reactivity of the transition over at least a 1000° C range, its insensitivity to T and its location around 30 kb are indicative of its potential for a pressure calibration curve at high T.  相似文献   

19.
The stable polymorph of MnTiO3 at room temperature and pressure has the ilmenite structure. At high temperatures and pressures, MnTiO3 ilmenite transforms to a LiNbO3 structure through a cation reordering process (Ko and Prewitt 1988). Single crystals of both phases have been studied with X-ray diffraction to 5.0 GPa. We have obtained the first experimental verification of the close relationship between the LiNbO3 and perovskite structures, first postulated by Megaw (1968). MnTiO3 with the LiNbO3 structure (MnTiO3 II) transforms directly to an orthorhombic perovskite structure (MnTiO3 III) between 2.0 and 3.0 GPa. The transition involves a change of volume of -5%, is reversible and has pronounced hysteresis. Only pressure is required to drive the transition because it involves no breaking of bonds; it simply involves rotation of the [TiO6] octahedra about their triad axes accompanied by displacement of the Mn cations to the distorted twelve-coordinated sites formed by the rotations. An unusual aspect of this transition is that twinned MnTiO3 II crystals transform to untwinned MnTiO3 III crystals with increasing pressure. The twin plane of MnTiO3 II, , corresponds to the (001) mirror plane of the orthorhombic perovskite structure. MnTiO3 III examined at 4.5 GPa is very distorted from the ideal cubic perovskite structure. The O(2)-O(2)-O(2) angle describing the tilting in the ab plane is 133.3(7)°, in contrast to 180° for a cubic perovskite and the O(2)-O(2)-O(2) angle describing the tilting in the ac plane is 109.3(4)°, as opposed to 90° in a cubic perovskite.  相似文献   

20.
Second-order zero-field splitting (ZFS) parameters from the literature for Fe3+ in twelve and for Cr3+ in seven minerals substituting for Al were evaluated by application of the superposition model. For Fe3+ in monoclinic site symmetries a fair agreement of the observed splitting patterns with those calculated from the crystal structure data was observed in most cases, but the distortions for Fe3+ appear to be usually larger than those of the unrelaxed Al sites. In cases of not too large local relaxation the unknown sign of the axialZFS parameterb 0 2 could be predicted, in two cases a different sign than that reported was postulated. In cordierite and scolecite the reportedEPR spectra could thus be assigned to the sites with larger average bond distances. For Fe3+ in beryl the relaxation of the axial site can be deduced within narrow limits. For Cr3+ significantly larger differences between observed and calculatedZFS patterns are found suggesting additional relaxations due to the non-spherical electron distribution in the ground state of this ion.  相似文献   

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