Zn—EDTA掩蔽Fe（Ⅲ）用CAS光度法测定硅铁中铝

络天青S(CAS)光度法早已应用于硅铁中铝的测定,但需用铜铁试剂沉淀分离铁、钒、钛、锡等干扰元素,不适合工厂快速分析。本文参考文献[2],采用不分离干扰元素,在弱酸性介质中用Zn-EDTA掩蔽Fe(Ⅲ),用CAS光度法测定硅铁中铝。分析结果能达到国家允许差的要求,方法简便、快速,可应用于各种牌号硅铁中铝的快速测定。     

二氧化钛中铝的分光光度测定

当有大量钛存在下测定铝,用通常方法需分离钛,文献指出,苦杏仁酸与钛(Ⅳ)有很强的络合能力,文献制订了以苦杏仁酸隐蔽钛,络合滴定法快速测定铝矾土中三氧化二铝。我们在文献的基础上,试验了用铬天青S测定铅时苦杏仁酸对钛的隐蔽性能,以及共存元素和溶样盐类的影响等。结果表明,苦杏仁酸对钛的隐蔽能力很强,0.06克苦杏仁酸可隐蔽     

石墨炉原子吸收光谱法测定铅钙锡铝合金中铝

铅钙锡铝合金广泛应用于全密封免维护铅蓄电池极板的生产。铅合金中铝的测定国标法采用络天青S比色法。试样用硝酸溶解,加入硫酸沉淀分离基体铅后进行比色测定。铅钙锡铝合金中含钙0．05％～0．12％,含锡0．1％～1．5％,含铝0．01％～0．04％,余量为铅。本文用石墨炉原子吸收光谱法测定铝,试样经硝酸溶解后,不加任何基体改进剂,直接测定,分析结果与国标法结果基本一致。     

ICP-AES法快速测定工业硅中杂质元素

我国是工业硅生产大国 ,每年都有大量出口任务。硅产品是重要的原材料 ,其杂质含量严重影响产品质量 ,影响出口。为了国家出口创汇 ,寻找工业硅中微量杂质元素的快速准确分析方法 ,是商检部门亟待解决的课题。GB/T1 484 9- 93标准中 ,铁、钙及铝分析采用容量法和吸光光度法 ,其操作复杂周期长 ,消耗试剂多。铁和钙元素有用原子吸收光谱法[1 ,2 ] ,其中磷元素质量分数小于 5× 1 0 - 3% ,是化学分析法和原子吸收光谱法均难以解决的。本文研究了用 ICP- AES法 ,在同一份溶液中同时测定磷、铁、钙、铝、铜、钒和钛杂质元素 ,其中磷的检出下…     

钛铁中钛铝的测定

目前钛铁合金中钛的测定,国家标准使用铝片还原,硫氰酸盐指示终点,硫酸高铁滴定.由于低价钛不稳定,在还原及滴定时须在氮气保护下进行,否则将造成一定误差且终点不易判别,操作极为不便.钛铁中铝的测定用8-羟基喹啉容量法.须经多次沉淀分离,测定流程较长.成本高.本文研究了铁、铝、钛、锰、铋与EDTA及过氧化氢之间的络合平衡关系,制定出在铁、铝、锰存在下测钛及锰存在下测铝的EDTA连续滴定方法.     

铬天青S分光光度法测定稀土氧化物中微量铝

关于微量铝的测定,目前以铬天青S分光光度法比较成熟,应用较广。与其他测定铝的显色剂比较,铬天青S具有灵敏度高、选择性好的优点。能否适用于稀土氧化物中微量铝的测定过去未见报导。为适应当时提取高纯氧化钇试验的需要,我们拟定了此方法。采用草酸沉淀分离大量稀土,然后用高氯酸冒烟破坏草酸,在pH5.7左右使铝和铬天青S生成红色络合物,用抗坏血酸还原铁(Ⅲ),用盐酸羟胺络合残余稀土,借此测定微量铝。 1.仪器:国产72型分光光度计。     

EDTA络合滴定法直接测定记忆合金中镍和钛

镍钛记忆合金是目前广泛用于医学上的一种功能材料,其中镍的质量分数为56％左右,钛的质量分数为44％左右。科研实践证明材料中的镍和钛的含量直接影响其应用性能。因此,快速、准确测定镍和钛的含量在生产过程中极为重要。传统的分析方法有镍一丁二肟重量法、丁二肟沉淀分离-EDTA络合滴定法,但这些方法操作都比较繁琐耗时,不能满足日常快速分析的需要。     

铬天青S分光光度法测定食品中铝

<正>铝是地壳中含量位居第三的元素,广泛分布于自然界中,在一些植物本底中含量很高~([1])。另外由于传统工艺的运用,某类食物中的铝含量也较高。纵观各种关于食品中铝毒性的报道可知,近几年开展的食品污染物风险监测选择膨化食品、面制食品、米粉和海蜇等进行铝的测定是非常及时和必要的。目前测定铝的方法有分光光度法、荧光光谱法、原子吸收光谱法和等离子体原子发射光谱法~([2])等。本工作采用微波消解处理食品样品,铬天青S     

铜铁试剂—氯仿萃取分离铬天青-S比色测定钢中铝

采用铜铁试剂-氯仿萃取分离钦、钒、铁、锆、铌、钽等干扰元素之后,用铬天青-S比色测定铝,提高了方法的选择性和准确度,操作简易快速。适用于铁基、镍基和钛基合金中铝的快速分析。 (一)主要试剂铬天青-S:(0.05％;5％乙醇溶液)。铝标准溶液:(1毫克铝/毫升)。称取光谱纯铝粉1.000克于250毫升烧杯中,加入30％氢氧化钠30毫升,加热溶解后,移入1000毫升容量瓶中,加水约     

碱分离-EDTA络合滴定法测定铝基钯催化剂中的氧化铝

采用碱分离-EDTA络合滴定法测定铝基钯催化剂中的氧化铝,考察了试样分解温度、EDTA的用量、煮沸时间、氟化钾用量、共存离子干扰等一系列条件对铝测定结果的影响。对标准样品定值的5个铝基钯催化剂的氧化铝进行测定,测定结果与参考值一致,测定范围是75%～95%,测定结果的相对标准偏差RSD(n=7)均小于1%。实验表明所拟定的铝基钯催化剂中铝的EDTA络合滴定法,测定结果准确可靠。     

Sc2MgGa2 and Y2MgGa2

Scandium magnesium gallide, Sc₂MgGa₂, and yttrium magnesium gallide, Y₂MgGa₂, were synthesized from the corresponding elements by heating under an argon atmosphere in an induction furnace. These intermetallic compounds crystallize in the tetragonal Mo₂FeB₂‐type structure. All three crystallographically unique atoms occupy special positions and the site symmetries of (Sc/Y, Ga) and Mg are m2m and 4/m, respectively. The coordinations around Sc/Y, Mg and Ga are pentagonal (Sc/Y), tetragonal (Mg) and triangular (Ga) prisms, with four (Mg) or three (Ga) additional capping atoms leading to the coordination numbers [10], [8+4] and [6+3], respectively. The crystal structure of Sc₂MgGa₂ was determined from single‐crystal diffraction intensities and the isostructural Y₂MgGa₂ was identified from powder diffraction data.     

Electrochemical study of (NEt4)2Cl2FeS2MoS2 and (NEt4)2Cl2FeS2MoS2FeCl2

Summary The ability of [MoS₄]^2–, anions to be used as ligands for transition metal ions has been widely demonstrated, especially with Fe²⁺. The present study has been restricted to linear complexes such as (NEt₄)₂ [Cl₂FeS₂MoS₂] and (NEt₄)₂[Cl₂FeS₂MoS₂FeCl₂]. Their electrochemical properties are described: upon electrochemical reduction, these compounds yield MoS₂, as a black precipitate, and an iron complex in solution, assumed to be [SFeCl₂]^2–. The electrochemical reduction goes through two electron transfers, coupled with the breakdown of the molecular skeleton: a DISPl and an ECE mechanism. Depending on the solvent, the following equilibrium may be observed: [Cl₄Fe₂MoS₄]^2–[Cl₂FeMoS₄]^2–+FeCl₂. The equilibrium constant, K_D, was evaluated by differential pulse polarography. K_D is tightly related to the donor number of the solvent.     

The alkali hypophosphites KH2PO2, RbH2PO2 and CsH2PO2

The structures of the hypophosphites KH₂PO₂ (potassium hypophosphite), RbH₂PO₂ (rubidium hypophosphite) and CsH₂PO₂ (caesium hypophosphite) have been determined by single‐crystal X‐ray diffraction. The structures consist of layers of alkali cations and hypophosphite anions, with the latter bridging four cations within the same layer. The Rb and Cs hypophosphites are isomorphous.     

Zur Kenntnis der Dialkalimetalldichalkogenide β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 und Rb2Te2

On Dialkali Metal Dichalcogenides β-Na₂S₂, K₂S₂, α-Rb₂S₂, β-Rb₂S₂, K₂Se₂, Rb₂Se₂, α-K₂Te₂, β-K₂Te₂ and Rb₂Te₂ The first presentation of pure samples of α- and β-Rb₂S₂, α- and β-K₂Te₂, and Rb₂Te₂ is described. Using single crystals of K₂S₂ and K₂Se₂, received by ammonothermal synthesis, the structure of the Na₂O₂ type and by using single crystals of β-Na₂S₂ and β-K₂Te₂ the Li₂O₂ type structure will be refined. By combined investigations with temperature-dependent Guinier-, neutron diffraction-, thermal analysis, and Raman-spectroscopy the nature of the monotropic phase transition from the Na₂O₂ type to the Li₂O₂ type will be explained by means of the examples α-/β-Na₂S₂ and α-/β-K₂Te₂. A further case of dimorphic condition as well as the monotropic phase transition of α- and β-Rb₂S₂ is presented. The existing areas of the structure fields of the dialkali metal dichalcogenides are limited by the model of the polar covalence.     

Formal [(2+2)+2] and [(2+2)+(2+2)] nonconjugated dienediyne cascade cycloadditions

[reaction: see text] Fluoranthene 2 and heptacycle 3 are easily accessible from the reaction of diyne 1 and norbornadiene (NBD) in the presence of the rhodium catalyst. The unusual [(2+2)+(2+2)] adduct 3 was confirmed by the X-ray crystal structure analysis.     

Crystal Structures of [Bu2Sn(O2PPh2)2], [Ph2Sn(O2PPh2)2], and [PhClSn(O2PPh2)OMe]2. Raman Spectra of [Ph2Sn(O2PPh2)2] and [PhClSn(O2PPh2)OMe]2

[(n‐Bu)₂Sn(O₂PPh₂)₂] ( 1 ), and [Ph₂Sn(O₂PPh₂)₂] ( 2 ) have been synthesized by the reactions of R₂SnCl₂ (R=n‐Bu, Ph) with HO₂PPh₂ in Methanol. From the reaction of Ph₂SnCl₂ with diphenylphosphinic acid a third product [PhClSn(O₂PPh₂)OMe]₂ ( 3 ) could be isolated. X‐ray diffraction studies show 1 to crystallize in the monoclinic space group P2₁/c with a = 1303.7(1) pm, b = 2286.9(2) pm, c = 1063.1(1) pm, β = 94.383(6)°, and Z = 4. 2 crystallizes triclinic in the space group , the cell parameters being a = 1293.2(2) pm, b = 1478.5(4) pm, c = 1507.2(3) pm, α = 98.86(3)°, β = 109.63(2)°, γ = 114.88(2)°, and Z = 2. Both compounds form arrays of eight‐membered rings (SnOPO)₂ linked at the tin atoms to form chains of infinite length. The dimer 3 consists of a like ring, in which the tin atoms are bridged by methoxo groups. It crystallizes triclinic in space group with a = 946.4(1) pm, b = 963.7(1) pm, c = 1174.2(1) pm, α = 82.495(6)°, β = 66.451(6)°, γ = 74.922(6)°, and Z = 1 for the dimer. The Raman spectra of 2 and 3 are given and discussed.     

Die Photoionenspektren von SCl2, S2Cl2 und S2Br2

Photoionization Mass Spectra of SCl₂, S₂Cl₂, and S₂Br₂ Photoionization mass spectra of SCl₂, S₂Cl₂, and S₂Br₂ have been measured. Heats of formation, bond energies, and ionization potentials of fragments have been calculated from appearance potentials.