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本文用作者合成的新试剂——钒金试剂Ⅱ为指示剂,该试剂在酸性溶液中被V(ν)氧化变为紫红色,灵敏度达5.13×10~(-15)gV(ν)/ml。试样经磷酸处理,在磷酸介质中用三氯化钛(或氯化亚锡)还原U(Ⅵ)呈U(Ⅳ),过量Ti(Ⅲ),Sn(Ⅱ)用亚硝酸钠氧化呈Ti(Ⅳ),Sn(Ⅳ),而U(Ⅳ)不被氧化。过量亚硝酸钠用脲素消除,在24％—26％磷酸酸度下,以2滴0.2％钒金试剂Ⅱ为指示剂,依据铀量用相应浓度钒酸铵标准溶液,滴定度T=0.003,0.01,0.03,0.1,0.3,1,3,10,30,100,300,1000,3000,10000,30000,100000,300000ngU/ml滴定U(Ⅳ)至溶液出现紫红色为终点。其他离子无干扰。测定天然水、海水、雨水中铀的范围为0.3—5000000ng/L;测定岩石、矿物中铀的范围为10—0.0000001％。0.005ng铀,5次重复测定的相对标准偏差为6.2％。铀的检测限为0.6pg/ml。 相似文献
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矿样经酸分解后，用硫酸肼还原，将Mo（Ⅵ）还原为Mo（Ⅴ），用8-羟基喹啉除去过量的硫酸肼，然后以钒试剂为指示剂，用钒酸铵滴定Mo（Ⅴ）。方法应用于尾矿样品中钼的测定，加标回收率为99.0％～102.0％，对钼含量3．54％（质量分数）的样品重复测定5次，精密度（RSD）为0．51％；适用于1％以上钼的测定。 相似文献
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基体分离-电位滴定法测定高硫金属矿中的微量氯 总被引：2，自引：1，他引：1
使用碳酸钠-氧化锌混合碱焙烧样品,将硫化物矿中的低价硫转化为硫酸盐或高价硫,过滤分离基体,采用电位滴定法测定硫化物矿(铜精矿、锌精矿、硫铁矿)中的微量氯,消除由于硫化银沉淀的产生对氯化银测定结果的干扰。通过电位突越,确定滴定终点,消除色度和浊度对滴定终点的影响。采用电极电位-浓度二次微商滴定曲线,计算滴定终点。对混合碱的选择及加入量、焙烧温度、溶液酸度、测定温度、滴定介质以及基体和共存元素的干扰进行了试验。方法精密度(RSD,n=9)均小于9%,回收率为94.1%~105.6%。 相似文献
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钒金试剂Ⅱ为指示剂钒酸铵滴定法测定岩石矿物中微量金 总被引：3，自引：0，他引：3
本文用作者合成的新试剂－钒金试剂Ⅱ做指示剂钒酸铵滴定法测定岩石矿物中微量金，终点明显，操作简便，测金量范围很宽，而且灵敏度很高。岩石矿物经王水－磷酸溶解，聚氨酯泡塑富集分离后，Ａｕ（Ⅲ）在硫磷混酸介质中经Ⅰ－还原至ＡｕＩ４３－，以钒金试剂Ⅱ为指示剂，钒酸铵滴定ＡｕＩ４３－中络合的Ⅰ－到溶液出现紫红色为终点。试样中测金范围在０．０００００１—１００μｇ／ｇ，相应测定的相对标准偏差在１４．３％－１．６９％。检出限为０．２ｐｇ／６ｍｌ。 相似文献
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用直接光谱分析法分析化学成分复杂的样品会遇到一系列的困难。基物定量组成和定性组成的变化对谱线的绝对强度和相对强度的大小有影响,因为当样品成分不同时,电弧温度的变动范围很大。本文所研究的是关于天然物质中经常与铀伴生的元素钛、锆和钍对微量铀的光谱测定准确度的影响问题。被测的铀含量为5×10(-7)-1×10(-4)克,伴生元素的含量大大超过了样品中的铀含量。研究方法是:用含有呈溶液状态而加入到样品中去的不同数量的钛、锆和钍的合成混合物为 相似文献
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高纯度的钛及钛合金具有良好的可塑性,当有杂质存在时变得脆而硬而影响其性能,准确分析杂质元素的含量有利于对钛生产工艺进行质量控制。对于杂质元素的分析,现行国家标准方法是采用样品蒸发温度较高的直流电弧作为光源,摄谱仪测定,需要经过显影、定影、测量黑度等步骤,操作繁琐,流程长,测量误差较大。本文应用中阶梯光栅和电荷耦合器件(CCD)组成的直流电弧(DC Arc)原子发射光谱仪(波长范围200~800nm),谱线干扰分析和谱线强度测量可以同时进行,能更大限度地获取光谱信息,建立了快速测定钛及钛合金中10种微量杂质元素(锰锡铬镍铝钼钒铜锆钇)的分析方法。实验讨论了测定过程中的四类谱线干扰,包括钛作为基体元素的谱线干扰、钛合金中添加的化学成分元素干扰、铁谱线的干扰、杂质元素之间的干扰,确定了适当的分析线;并应用一种浅孔薄壁细颈杯形电极装入试样,提高了样品的蒸发效果;用氯化银和碳粉的混合物作缓冲剂,提高了待测元素的谱线强度。本方法的检测范围为0.001%~0.06%,精密度小于15%,回收率为90.0%~110.0%,适合于大批量钛及钛合金样品中杂质元素的同时检测。 相似文献
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电感耦合等离子体发射光谱法同时测定钒钛磁铁矿中铁钛钒 总被引：6，自引：3，他引：3
样品采用HCl-HF-HNO3-HClO4四酸溶矿、H2SO4-HF-HNO3三酸溶矿、KOH碱熔3种分解方法进行处理,电感耦合等离子体发射光谱法(ICP-AES)测定钒钛磁铁矿中的铁、钛、钒。结果表明,3种样品处理方法应用于ICP-AES测定是可行的。KOH碱熔适用于方法比对,三酸溶矿适用于样品内检分析,四酸溶矿适用于大批量样品测定。对铁、钛、钒三元素选择适合的分析谱线,以冶金行业钒钛磁铁矿标准样品制备的溶液绘制标准曲线,可消除试液基体和介质不一致对测定结果的影响。样品试液中主要共存离子对选择的分析线干扰小。采用四酸溶矿ICP-AES测定铁、钛、钒的方法检出限分别为0.0032%、0.0024%、0.0003%,方法精密度(RSD,n=12)为0.43%～5.06%。经实验室间比对和批量样品方法比对实验,测定值无明显系统偏差。建立的方法具有样品分解完全、测定含量范围宽、分析简便快速、结果准确等优点,适用于钒钛磁铁矿样品中铁、钛、钒的测定。 相似文献
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为探讨不同碳氮源对培养基中铀酰离子的络合形态及荧光假单胞菌对铀吸附和还原作用的影响,本文以查氏培养基为基础,将蔗糖替换为葡萄糖或将硝酸钠替代为氯化铵,采用Visual MINTEQ分析研究铀酰离子络合形态。研究结果表明,碳氮源的种类对微生物生长无影响。U(Ⅵ)浓度为10 mg/L时,3种培养基中铀酰离子的主要络合形态均为UO2PO-4。U(Ⅵ)浓度为50~200 mg/L,查氏和葡萄糖碳源培养基中铀酰离子主要络合形态均为UO2(SO4)2-2。氯化铵氮源培养基中,U(Ⅵ)浓度为50 mg/L时铀酰离子的主要络合形态为UO2HPO4(aq),浓度为100~200 mg/L时主要是UO2Cl2(aq)。荧光假单胞菌对U(Ⅵ)耐受浓度高达100 mg/L,当U(Ⅵ)浓度达到200 mg/L时,菌体失活。荧光假单胞菌为活体时,对U(Ⅵ)的吸附率为84.02%~92.59%,还原率为3.32%~10.94%,不同碳氮源对铀吸附和还原的影响较小。荧光假单胞菌为死体时,对铀的吸附率为24.33%~39.05%;非葡萄糖碳源培养基中,对铀的还原率为37.50%~44.58%,含还原性葡萄糖的培养基条件下U(Ⅵ)的还原率为53.12%。还原性葡萄糖与荧光假单胞菌对铀的还原为协同作用。荧光假单胞菌为活体时,培养基成分被微生物充分利用,两者协同作用不明显。 相似文献
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M. N. Taran M. Andrut E. V. Polshin S. S. Matsyuk 《Physics and Chemistry of Minerals》1999,27(1):59-69
Over thirty samples of natural Ti-bearing amphiboles with Ti- and Fe-contents ranging from 0.111 to 0.729 atom per formula unit (a.p.f.u.) and from 0.479 to 2.045 a.p.f.u., respectively, were studied by means of optical absorption spectroscopy and microprobe analysis. Thirteen samples were also studied by Mössbauer spectroscopy. A strong pleochroic absorption edge, causing the dark brown colours of Ti-bearing amphiboles, is attributed to ligand-metal and metal-metal charge transfer transitions involving both iron and titanium ions (O2?→ Fe3+, Fe2+, O2?→ Ti4+ and Fe2+ + Ti4+→ Fe3+ + Ti3+). A broad intense Y-polarized band ～22?000?cm?1 (ν1/2?≈?3700?cm?1) in spectra of two low iron amphiboles with a relatively low Fe3+/Fetotal ratio, both from eclogite-like rocks in kimberlite xenoliths, was attributed to electronic Fe2+(M3) + Ti4+(M2)→Fe3+(M3)+Ti3+(M2) IVCT transitions. The IVCT bands of other possible ion pairs, involving Ti4+ and Fe2+ in M2 and M1, M4 sites, respectively, are presumed to be at higher energies, being obscured by the absorption edge. 相似文献
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蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇 总被引：1，自引：1，他引：0
建立了蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇的分析方法。进行了蒸馏温度和时间、氧化剂、吸收液等条件的选择,消除了等离子体质谱法测定钌和锇的干扰。样品用过氧化钠熔融,酸化后以高锰酸钾-过硫酸钾-氯化钠作为同时蒸馏钌和锇的氧化剂,采用20 mL 50 g/L水合肼溶液同时吸收从混合物中分离出来的痕量钌和锇,用电感耦合等离子体质谱法测定。方法的检出限Ru为0.020 ng/g,Os为0.015 ng/g;方法加标回收率Ru为94.0%~102.7%,Os为96.0%~102.4%;精密度为4.72%~9.58%(n=12)。方法经国家一级标准物质验证,钌和锇的测定结果与标准值相符。 相似文献
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L. Z. Reznitsky E. V. Sklyarov T. Armbruster L. F. Suvorova Z. F. Uschapovskaya S. V. Kanakin 《Geology of Ore Deposits》2013,55(8):676-685
Kyzylkumite has been found in Cr-V-bearing metamorphic rocks of the Sludyanka Complex, Southern Baikal region; it has been identified by X-ray powder diffraction method. This is a late secondary mineral developed after Ti-V-oxides (schreyerite, berdesinskiite) and V-bearing rutile and titanite. Kyzylkumite represents a new structural type with composition Ti4V 2 3+ O10(OH)2 corresponding to octahedral coordination of Ti4+ and V3+. Its unit-cell dimensions are: a = 8.4787(1), b = 4.5624(1), c = 10.0330(1) Å, β = 93.174(1)°. The ideal formula of kyzylkumite Ti4V 2 3+ O10(OH)2 corresponds to composition, wt %: 65.56 TiO2, 30.75 V2O3, 3.69 H2O. Indeed, the contents (wt %) of these constituents range from 62 to 70 TiO2 and from 23 to 33 V2O3. Variations in contents and the Ti/V value are caused by partial substitution V3+ for V4+, isovalent substitutions Ti4+ and V3+ for V4+ and Cr3+, respectively, and coupled substitution V3+ + OH? ? Ti4+ + O2?. Smyslova et al. (1981)—the discovereres of kyzylkumite—assumed its composition to be the same as for schreyerite V 2 3+ Ti3O9 that principally different from kyzylkumite from the Sludyanka Complex. Therefore, re-examination of the kyzylkumite holotype or cotype from its type locality is needed. 相似文献
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We investigated a natural Brazilian Fe–Ti-containing andalusite and its thermal behavior by polarized infrared and optical spectroscopy. Polarized infrared spectra of the Brazilian andalusite and their evolution at thermal annealing in air clearly evidence that there are several types of OH-groups in the structure. Optical spectra and their evolution with temperature indicate that the incorporated iron (about 0.43 wt% calculated as FeO) is in the ferrous and ferric state. Incorporation of ferrous iron in the Al-sites of andalusite is discussed as a possible incorporation mechanism for hydrogen. The weakening and disappearance of the Fe2+/Ti4+ IVCT band in the andalusite spectra under annealing in air is caused by oxidization of Fe2+ to Fe3+ in Fe2+/Ti4+ IVCT pairs. The process of oxidation is accompanied by a rearrangement of the hydroxyl groups and dehydration of the sample, especially vivid at the final stage of the thermal annealing at 1,200 °C. During thermal annealing, structural hydroxyls of different types apparently transform into each other: the most distinct are the hydroxyls causing the doublet at 3,516 and 3,527 cm?1 (i.e., H bonded to O1) which seem to transform into the hydroxyls causing the line at 3,461 cm?1 (i.e., H bonded to O2). The infrared spectra scanned across differently colored zones of the crystal clearly show that some amount of hydroxyls is related to Fe2+/Ti4+ IVCT pairs which are the cause of the red-to-black coloration of the sample in E||c-polarized illumination: it is evident that in a part of the hydroxyl groups, OH-vector changes orientation aligning directly along crystallographic a-axis due to some kind of interaction with Fe2+/Ti4+ IVCT pairs. 相似文献
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Examination of schorlomite from ijolite at Magnet Cove (USA) and silicocarbonatite at Afrikanda (Russia), using electron-microprobe and hydrogen analyses, X-ray diffraction and Mössbauer spectroscopy, shows the complexity of substitution mechanisms operating in Ti-rich garnets. These substitutions involve incorporation of Na in the eightfold-coordinated X site, Fe2+ and Mg in the octahedrally coordinated Y site, and Fe3+, Al and Fe2+ in the tetrahedrally coordinated Z site. Substitutions Ti4+Fe3+Fe3+–1Si–1 and Ti4+Al3+Fe3+–1Si–1 are of major significance to the crystal chemistry of schorlomite, whereas Fe2+ enters the Z site in relatively minor quantities (<3% Fe). There is no evidence (either structural or indirect, such as discrepancies between the measured and calculated Fe2+ contents) for the presence of [6]Ti3+ or [4]Ti4+ in schorlomite. The simplified general formula of schorlomite can be written as Ca3Ti4+2[Si3-x(Fe3+,Al,Fe2+)xO12], keeping in mind that the notion of end-member composition is inapplicable to this mineral. In the published analyses of schorlomite with low to moderate Zr contents, x ranges from 0.6 to 1.0, i.e. Ti4+ in the Y site is <2 and accompanied by appreciable amounts of lower-charged cations (in particular, Fe3+, Fe2+ and Mg). For classification purposes, the mole percentage of schorlomite can be determined as the amount of [6]Ti4+, balanced by substitutions in the Z site, relative to the total occupancy in the Y site: ([6]Ti4+–[6]Fe2+–[6]Mg2+– [8]Na+)/2. In addition to the predominant schorlomite component, the crystals examined in this work contain significant (>15 mol.%) proportions of andradite (Ca3Fe3+2Si3O12), morimotoite (Ca3Fe2+TiSi3O12), and Ca3MgTiSi3O12. The importance of accurate quantitative determination and assignment of Fe, Ti and other cations to the crystallographic sites for petrogenetic studies is discussed.
相似文献
| A. R. ChakhmouradianEmail: Phone: +1-204-4747278Fax: +1-204-4747623 |
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Angela Ullrich Ronald Miletich Tonci Balic-Zunic Lars Olsen Fabrizio Nestola Manfred Wildner Haruo Ohashi 《Physics and Chemistry of Minerals》2010,37(1):25-43
A compressional study of (Na,Ca)(Ti3+,Mg)Si2O6-clinopyroxenes was carried out at high pressures between 10−4 and 10.2 GPa using in situ single-crystal X-ray diffraction, Raman spectroscopy and optical absorption spectroscopy. Compressional
discontinuities accompanied by structural changes, in particular, the appearance of two distinct Ti3+–Ti3+ distances within the octahedral chains at 4.37 GPa, provide evidence for the occurrence of a phase transition in NaTi3+Si2O6. Equation-of-state parameters are K
0 = 115.9(7) GPa with K′ = −0.9(3) and K
0 = 102.7(8) GPa with K′ = 4.08(5) for the low- and high-pressure range, respectively. The transition involves a C2/c–P
[`1] \overline{1} symmetry change, which can be confirmed by the occurrence of new modes in Raman spectra. Since no significant discontinuity
in the evolution of the unit-cell volume with pressure has been observed, the transition appears to be second-order in character.
The influence of the coupled substitution Na+Ti3+↔Ca2+Mg2+ on the static compression behavior and the structural stability has been investigated using a sample of the intermediate
composition (Na0.54Ca0.46)(Mg0.46Ti0.54)Si2O6. No evidence for a deviation from continuous compression behavior has been found, neither in lattice parameter nor in structural
data and the fit of a third-order Birch–Murnaghan equation-of-state to the pressure–volume data yields a bulk modulus of K
0 = 109.1(5) GPa and K′ = 5.02(13). Raman and polarized absorption spectra have been compared to NaTiSi2O6 and reveal major similarities. The main driving force for the phase transition in NaTi3+Si2O6 is the localization of the Ti3+
d-electron and the accompanying distortion, which is suppressed in the (Na,Ca)(Ti3+,Mg)Si2O6-clinopyroxene. 相似文献
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Valence state of titanium in the Wark-Lovering rim of a Leoville CAI as a record of progressive oxidation in the early Solar Nebula 总被引：1，自引：0，他引：1
Simon et al. (2005) reported low Ti3+/Ti4+ values in Ti-rich pyroxenes in the Wark-Lovering rim (WL) of a Leoville CAI (144A) as compared to the interior of the inclusion. These electron microprobe analyses were interpreted as evidence that the growth of the WL rim is the manifestation of an evolution to a more oxidizing environment. Further work by Simon et al. (2007) used XANES analyses to argue for higher Ti3+ abundances and interpreted the data of Simon et al. (2005) as the result of X-ray contamination by neighboring phases, specifically spinel. Late-stage alteration was also included as a possible explanation.To investigate further the oxidation state of Ti in WL rims, we re-analyzed Leoville 144A to obtain a more complete data set of Ti3+/Ti4+ values in the Wark-Lovering rims. We conducted experiments on spinel-mixing to determine whether this was a plausible explanation for the observed paucity of Ti3+ in WL rims. While we found a wider range of Ti3+/Ti4+ in these WL rim data than in our original study, our new data show that the original conclusion that rims are lower in Ti3+/Ti4+ than interiors remains valid. We conclusively rule out spinel-mixing as an explanation for our data, and we see no clear inconsistency between our electron microprobe data and the XANES data. The WL rim of CAI Ef3 was also analyzed by EMPA and compared to the results of Leoville 144A.To predict compositional consequences of this hypothesis, we constructed a reaction space between Ti-rich pyroxene in the WL rim, perovskite, Mg(g), Ca(g), O2(g), and SiO(g). We find the oxidation of Ti3+, coupled with Ti loss via perovskite formation, explains many features of WL rim EMPA analyses. We maintain that the WL rim pyroxenes are compositionally distinct from those in the interior, and are evidence of a more oxidizing environment during WL rim formation. 相似文献