萃取色谱分离偶氮氯膦-mN光度法测定矿石中铈

本文提出以P_(507)为固定相,盐酸为流动相的萃取色谱法把铈从溶液中分离出来,以偶氮氯膦-mN与铈的高灵敏显色反应进行比色。本法灵敏度ε=7.8×10~4。 实验部分 色谱柱:φ8×120m/m 硅烷化硅球100—120目(上试一厂出品) P_(507)(上海有机化学所实验工厂) 偶氮氯膦-mN0.05％水溶液 杂质洗除液:5％NH_4Cl,2％磺基水杨酸,1％抗坏血酸,调至ρH2—3 铈、镧、镨标准液:用光谱纯的氧化铈,氧化镧,氧     

偶氮氯磷-mN直接光度法测定矿石中铈族稀土元素

本文研究了偶氮氯膦-mN在磷酸—草酸—焦磷酸钠体系中以锌-EDTA二乙酯作缓冲掩蔽剂①在钇族稀土和常见元素存在下,不经分离,直接测定铈族稀土元素的可能性。一、实验部分偶氮氯膦-mN:0.05%水溶液(上海师大)。Zn-EDTA二乙酯0.15%水溶液:称取EDTA二乙酯15克,乙酸锌15克溶于1000毫升水中,摇均。混合铈组稀土标准:用光谱纯的稀土氧化物按     

偶氮氯磷-mN直接光度法测定矿石中铈族稀土元素

本文研究了偶氮氯膦-mN在磷酸—草酸—焦磷酸钠体系中以锌-EDTA二乙酯作缓冲掩蔽剂在钇族稀土和常见元素存在下,不经分离,直接测定铈族稀土元素的可能性。 一、实验部分 偶氮氯膦-mN:0.05％水溶液(上海师大)。 Zn-EDTA二乙酯0.15％水溶液:称取EDTA二乙酯15克;乙酸锌15克溶于1000毫升水中,摇均。 混合铈组稀土标准:用光谱纯的稀土氧化物按La∶Ce∶Pr∶Nd:Sm等于50∶30∶20∶10∶10配成每毫升含10微克的酸性稀土溶液(0.1N盐酸)。 混合钇族稀土标准:按Y∶Ho∶Yb∶Lu等于66∶4∶18∶6配制成每毫升10微克的标准溶液(0.1N盐酸)。     

P-(507)—萃取树脂分离偶氮氯膦-PN光度法测定矿石中稀土总量

萃取树脂作为一种化学分离手段,国外七十年代就有报导,近年国内兄弟单位研制合成了各类型萃取树脂,并相继用于分析工作中,P_(507)萃取树脂最近问世,给稀土元素的分离富集带来了佳音。该树脂是在P_(507)萃取色层的基础上研制而成的,并具有离子交换的优点。本文研究了P_(507)萃取树脂分离稀土的条件及偶氮氯膦—PN与稀土元素的显色反应;拟定了一个     

一些不对称双偶氮氯膦类显色剂测定钪的比较

华东师大合成的不对称双偶氮氯膦类显色剂是一类新型的稀土显色剂。这类显色剂有偶氮氯膦-mA,偶氮氯膦-mN,偶氮氯膦-mK,偶氮氯膦-PN(以下简称CPA-mA、mN、mK、pN)它们的结构式分别为:     

P_(507)—萃取树脂分离偶氮氯膦-PN光度法测定矿石中稀土总量

萃取树脂作为一种化学分离手段,国外七十年代就有报导,近年国内兄弟单位研制合成了各类型萃取树脂,并相继用于分析工作中,P_(507)萃取树脂最近问世,给稀土元素的分离富集带来了佳音。该树脂是在P_(507)萃取色层的基础上研制而成的,并具有离子交换的优点。 本文研究了P_(507)萃取树脂分离稀土的条件及偶氮氯膦—PN与稀土元素的显色反应;拟定了一个分离效果良好、简便、灵敏度比偶氮胂Ⅲ高一倍的稀土总量的分析流程,可作为稀土分析的新方法。 实验部分     

稀土元素新型显色剂偶氮溴膦-PN测定地质样品中稀土总量

本文首次报导用[2-(4-溴-2-膦酸基苯偶氮)-7-(4′-硝基苯偶氮)1,8-二羟基-3,6-萘二磺酸](简称偶氮溴膦-PN)作为稀土元素的新显色剂,研究了它与稀土元素的显色条件,并将其用于矿石中稀土总量的测定。该试剂为深紫红色粉末,易溶于水,在0.08～0.32N硝酸介质中,它与稀土元素形成蓝紫色络合物,其稳定时间可高达25小时以上。络合物的摩尔吸光系数(以铈计)为7.53×10~4。样品经通常的碱熔,PMBP-苯萃取分离后,即可用它测定稀土总量。     

新显色剂1-(2-咪唑偶氮)-2-萘酚-4-磺酸分光光度法测定铜

新显色剂1-(2-咪唑偶氮)-2-萘酚-4-磺酸在pH 3的介质中光度法测定Cu的摩尔吸光系数为1.94×10~4 L.mol~(-1).cm~(-1),络合物的组成为1:1,最大吸收在530nm,对比度△λ为120nm,表观稳定常数为6.96×10~6,Cu~(2+)在0～0.8μg/ml范围内遵守比尔定律,方法已用于镁介金及铁矿石中Cu的测定。     

间羧基偶氮氯膦光度法测定矿石中微量钪

间羧基偶氮氯膦(简称CPA—mk)曾用于钢中铈族稀土的测定。本文研究了试剂与钪形成有色络合物的条件。在0.12～0.48mol/L盐酸介质中,于610和660nm处有两个吸收峰,摩尔吸光系数为4.0×10~4,Sc:CPA-mk为1:2,25毫升中0～10微克Sc_2O_3符合比尔定律。室温28°以下可稳定24小时。比偶氮氯膦mA法灵敏度高,稳定性好。用PMBP萃取分离干扰元素后,可测定矿石和岩石中1×10~(-4)～0.1％Sc_2O_3的含量。     

某铀矿床成矿物理化学条件的研究

某铀矿床位于L花岗岩体外接触带,成矿围岩为中泥盆统碳酸盐岩,为多阶段中低温热液型铀矿化。本文详细地讨论了该矿床的成矿物理化学条件:成矿温度为100—300℃,沥青铀矿形成温变为150—200℃;矿前期热液压力为(1—2)×10~8SPa,矿期为(5—10)×10~7pa,矿后期为(3—5)×10~7Pa。从矿前期至矿后期,矿液fo_2和fs_2皆有降低的趋势fo_2为10~(-31.81)—10~(43.58),fs_2为10~(-6.67)—10~(-16.56);矿液pH为7.12—7.59,Eh为-0.2702—-0.2848V;铀以K_4[UO_2(CO_3)_3]形式迁移,随着物理化学条件的改变,铀络合物解体,形成沥青铀矿。     

Influence of alcohols on the extraction of cerium(IV) by Aliquat-336 in kerosene

Tricaprylmethylammonium chloride (Aliquat-336) diluted with kerosene was used to extract cerium(IV) from nitric acid medium. Various alcohols were used as modifiers to overcome the third phase problem. The different parameters affecting the extraction process including nitric, nitrate, hydrogen ion, extractant and metal concentrations as well as the temperature were separately investigated. The effect of the investigated alcohols on the extraction process was also studied in detail at two different concentrations and correlated to their physical constants. Based on the obtained results, the extraction equilibrium was deduced and the optimum conditions for the extraction of cerium(IV) were proposed. The method was tested and applied to the separation of cerium from the hydrous oxide cake resulting from monazite sand.     

新型铈铁硼中铅含量的测定方法研究

通过对新型铈铁硼材料中铅含量的测定方法研究,开发了以电感耦合等离子体发射光谱(ICP-OES)法测定铈铁硼中铅含量的方法。实验研究了分析谱线的选择,以铈和铁为基体配制标准溶液,用6%体积浓度的稀硝酸低温加热消解铈铁硼,用基体匹配法测定了铈铁硼中铅的含量。最后通过方法检出限的计算、加标回收率实验、平行实验和重复性测试,验证了方法的可靠性。实验结果表明,该方法的检出限为0.007 mg/L,加标回收率为100.6%,样品中铅含量为0.006%,两次实验平行性好,重复性低于2.3%,数据准确可靠。该方法具备实验室可操作性,可以为新型铈铁硼生产中的铅含量杂质分析提供依据,也可为重金属污染检测提供参考。     

The redox state of cerium in basaltic magmas: an experimental study of iron-cerium interactions in silicate melts

Ce(IV)-Ce(III) and Fe(III)-Fe(II) redox equilibria in Ca-Mg-Al-silicate melts have been individually measured with respect to the base composition, melt temperature, imposed oxygen fugacity, and multivalent element concentration (up to about 1.5 wt%). The mutual interaction of these two redox couples has been studied in analogous glasses which simultaneously contained iron and cerium. Analyses of Fe(III) concentrations in iron-cerium glasses by electron paramagnetic resonance and optical absorption spectroscopy indicate that Ce(IV) is stoichiometrically reduced by Fe(II) in the melt to produce Fe(III) and Ce(III) and that Ce(III)-O-Fe(III) complexes are formed in the melt. Consequently, it is concluded that cerium exists only as Ce(III) in basaltic magmas; cerium anomalies cannot be ascribed to the stabilization of Ce(IV) in magmas.     

稀土Ce,Tb在SrAl2O4基质中发光性的初步试验研究

本文报道了利用CeO2,Tb4O7和SrAl2O4为主原料合成SrAl2O4:(Ce,Tb)光致绿色发光粉体研究结果，实验研究表明Ce^3 ，Tb^3 含量、保温时间等主要合成条件对合成样品发光性能具有重要影响，并对其发光机理进行了初步探讨。     

The Nature of Oscillatory Zoning and Mechanism of Crystal Growth in a Paragenic Intergrowth of Florencite and Xenotime

Geology of Ore Deposits - REE fractionation into cerium Ceg (La–Eu) and yttrium Yg (Gd–Lu) groups, as well as Lasg (La–Pr), Smsg (Nd–Eu), Gdsg (Gd–Dy), and Ybsg (Y,...     

少砬哈子碱性岩体铌钽矿化特征及吉中地区碱性岩找矿方向

在吉中地区敦密断裂带上,分布大小不等的碱性杂岩体已发现的大约20余个。本文对蛟河南部少砬哈子碱性岩体地质特征及蚀变矿化进行了详细的野外地质调查,发现该岩体具有很好的铌、铈矿化,Nb5O2平均品位0.043%,最高为0.049%（未分析钽）,铈族稀土质量分数0.109%,且不同的岩相带矿化蚀变存在较大差异,细粒结构相矿化...     

Fluid inclusions in apatite from Jacupiranga calcite carbonatites: Evidence for a fluid-stratified carbonatite magma chamber

Carbonatites of the Jacupiranga alkaline–carbonatite complex in São Paulo State, Brazil, were used to investigate mineral–fluid interaction in a carbonatite magma chamber because apatite showed a marked discontinuity between primary fluid inclusion-rich cores and fluid inclusion-poor rims. Sylvite and burbankite, apatite, pyrite, chalcopyrite and ilmenite are the common phases occurring as trapped solids within primary fluid inclusions and reflect the general assemblage of the carbonatite. The apatite cores had higher Sr and REE concentrations than apatite rims, due to the presence of fluid inclusions into which these elements partitioned. A positive cerium anomaly was observed in both the core and rim of apatite crystals because oxidised Ce⁴⁺ partitioned into the magma. The combined evidence from apatite chemistry, fluid inclusion distribution and fluid composition was used to test the hypotheses that the limit of fluid inclusion occurrence within apatite crystals arises from: (1) generation of a separate fluid phase; (2) utilization of all available fluid during the first stage of crystallization; (3) removal of crystals from fluid-rich magma to fluid-poor magma; (4) an increase in the growth rate of apatite; or (5) escape of the fluids from the rim of the apatite after crystallization. The findings are consistent with fractionation and crystal settling of a carbonatite assemblage in a fluid-stratified magma chamber. Secondary fluid inclusions were trapped during a hydrothermal event that precipitated an assemblage of anhedral crystals: strontianite, carbocernaite, barytocalcite, barite and norsethite, pyrophanite, magnesian siderite and baddeleyite, ancylite-(Ce), monazite-(Ce) and allanite. The Sr- and REE-rich nature of the secondary assemblage, and lack of a positive cerium anomaly indicate that hydrothermal fluids have a similar source to the primary magma and are related to a later carbonatite intrusion.     

Acid leaching of ash and coal: Time dependence and trace element occurrences

The leaching of coal and coal/asphaltite/wood-ashes in sulfuric acid (pH 1.0, 25 °C, S/L, 1:10) was studied as a function of time; acid consumption and extracted metal concentrations are presented. Whole coals consumed acid rapidly during the first few minutes, followed by slow acid consumption. Wood-, lignite-, and asphaltite-ashes consumed acid in two stages, the rapid phase extending < 30 min and the slow phase extended up to 10 days. The rapid phase was dominated by the dissolution of Ca, K and Mg ions for wood-ash, by Ca, Al and Mg ions for lignite-ash and Ca and Mg ions for asphaltite-ash. The sulfur concentration in solution and the concentrations of Ca, Fe, K, Mg, Na, P, Al and Mn in the aqueous phase verified the neutralizing capacity of the untreated ashes as well as the formation of insoluble sulfates in the residues. The slow phase kinetics differed for different fuels and exhibited leaching of several abundant elements—Fe, Al, K, Na and Mn. Trace elements (Ba, Cd, Co, Cr, Cu, Mo, Ni, Pb, Th, U, V, Zn) sometimes required up to 32 h for maximal extraction from ashes. Suggestions are presented regarding the chemical nature of trace elements in the untreated coals and ashes and suitable residence times for economical industrial processes. We think it possible to combine bacteriological oxidation of sulfidic concentrates of acid leaching from ash of various qualities or even whole coals.     

一种新产状的含铈褐钇铌矿

关于褐钇铌矿族的研究,国内外积累了不少资料。其主要产在黑云母花岗岩、花岗伟晶岩、微斜长石岩、交代变质岩、蚀变花岗岩、白岗岩及花岗岩的残坡积和冲积砂中。1979年我们在进行内蒙白云鄂博铌、稀土、铁矿床物质成分的研究时,在白云石型铌、稀土矿石中发现含铈褐钇铌矿,与该区原已发现的褐铈铌矿等矿物组成了褐钇铌矿-褐铈铌矿系列。     

The formation of cobalt-bearing ferromanganese crusts under fluid destruction of silicate matter

The processes of fluid destruction of various silicate rocks under diffusion of flows of compressed gases (mainly carbonaceous) were studied. The gas condensate nature was ascertained for the forming alumoslilicate and ore (cobalt–iron–manganese hydroxide) substances produced under this fluid destruction in the forms of microcrusts and microconcretions. The ore condensates contained in high concentrations the typomorphic elements of oceanic ferromanganese formations (Mn, Co, Ni, Cu, Pb, Ce, and Pt). The elemental composition of the ore oxide substance formed under the destruction of various silicate matrices exhibits a definite degree of endemism with prevalence of the Co–Mn association. The pronounced concentration of barium is related to the substantially carbonaceous composition of the fluid systems. A cerium paradox is revealed: Ce³⁺ is oxidized into Ce⁴⁺ and absorbed by ferromanganese hydrogel and the minimum of cerium appears in rare-earth phosphates.