BiPbSbSrCaCuO的超导电性

据报,在BiPbSrCaCuO中加Sb形成BiPbSbSrCaCuO体系的T_c可达130K。但其组成、结构、性质等均未见详细报道。我们合成了一系列BiPbSbSrCaCuO,发现了一个具有2212相结构、但T_c却为～110K的超导相。 试样制备包括将Bi_2O_3,PbO,Sb_2O_3,SrCO_3,CaO和CuO(AR级)混匀、碾磨、于     

用水合五氧化二锑分离放射性母子体的研究─—一个新的~(201)Pb—~(201)T1发生器的制备

本文研究了无机离子交换剂—水合五氧化二锑（Sb2O5·nH2O）的制备，并用它分离了放射性母子体，制备了一个新的201Pb—201Tl放射性发生器。结果表明，末发生器具有高效、快速、简便的特点，此外还讨论了离子交换反应的机理。     

固固相反应合成牛磺酸水杨醛钾与锑、铋的配合物

合成了牛磺酸水杨醛钾,并采用室温固固相反应法合成了牛磺酸水杨醛钾与三氯化锑和三氯化铋的配合物,其组成为:K2MC18H20O8N2S2 (M = Sb, Bi)。两种配合物的晶体结构均属于单斜晶系,锑配合物的晶胞参数为:a = 1.2869 nm, b = 1.7636 nm, c = 1.9917 nm, β= 93.79埃活榕浜衔锏木О问篴 = 1.4770 nm, b = 2.0334 nm, c = 2.0149 nm, β= 94.05。红外光谱表明N、Cl原子参与了配位,中心离子的配位数为5。     

固固反应合成三碘化锑、三碘化铋与硫脲配合物

通过三碘化锑和三碘化铋与硫脲间的室温固固反应合成了三碘化锑、三碘化铋的硫脲配合物 ,其组成为 :M[CS( NH2 ) 2 ]3 I3 ( M=Sb,Bi)。两种配合物的晶体结构均属于单斜晶系 ,锑配合物 Sb[CS( NH2 ) 2 ]3 I3 的晶胞参数为 :a=1 .4 772 nm,b=1 .6 5 82 nm,c=2 .0 6 74 nm,β=90 .81°,铋配合物 Bi[CS( NH2 ) 2 ]3 I3 的晶胞参数为 :a=1 .4 0 1 0 nm,b=2 .0 1 6 8nm,c=2 .0 397nm,β=90 .84°。远红外光谱表明硫脲中的 N原子而非硫原子参与了配位     

甲基绿－萃取光度法测定锑

本文用Ｃｅ（ＳＯ＿４）＿２作氧化剂，在６ｍｏｌ／Ｌ　ＨＣｌ溶液中将Ｓｂ（Ⅲ）氧化为Ｓｂ（Ⅴ），过量的氧化剂用盐酸羟胺还原，生成的［ＳｂＣｌ＿６］￣－与甲基绿形成离子缔合物，在２ｍｏｌ／ＬＨＣｌ溶液中被ＣＨＣｌ＿３萃取。Ｔｌ、Ｉｎ、Ｇａ、Ａｕ等２０种离子共存时不干扰测定，用于金属镉及废水中测定微量锑，结果满意。     

联萘衍生物的磺化反应研究

研究了1-和2-苯基萘, 1, 1'-和2, 2'-联萘, 2, 2-二羟基-, 2, 2'-二甲氧基和-2, 2'-甲基磺酰氧基-1, 1'-联萘等七种萘衍生物和三氧化硫的磺化反应。1-苯基萘和1, 1'-联萘的磺化先发生在4位上, 第二取代位置为6和7位。2-苯基萘和2, 2'-联萘均首先得到8位磺酸取代物, 进一步磺化得到8, 4'-和8, 8'-二磺酸取代物。2, 2'-二甲氧基-1, 1'-联萘以13:87的比例得到3位和6位磺酸取代物。2, 2'-二甲磺酰氧基-1, 1'-联萘以58:42的比例得到5位和6位磺酸取代物。2, 2'-二羟基-1, 1'-联萘的等摩尔磺化得到比例为35:65的5位和6位磺酸取代物, 和大于6摩尔的SO~3反应则以62:38的比例得到5位和6位磺酸取代物。     

Study of isomorphism in fluorine-containing antimony(III) complexes

The mutual influence of the atoms on the composition of solid fluorine-containing antimony(iii) complexes formed in aqueous solutions in the (MF) _x −(M′F) _n−x −SbF₃ (M, M′=Na, K, Rb, Cs, and NH₄;n=1, 2;x=0 to 2), (KNO₂) _n −(KY) _n −SbF₃ (Y=F, Cl, SO₄;n=0.5, 1), and K₂SbF₅−K₂SbCl₅ systems was investigated by elemental, X-ray, and thermogravimetric analyses and by IR and^121,123Sb NQR spectroscopy. The isomorphism conditions for fluorine-containing antimony(iii) compounds resulting in the formation of complexes NaM′SbF₅·1.5H₂O (M′=K and Rb), K₂SbF₅·1.5H₂O, NaCs₃Sb₄F₁₆·H₂O, KsbF₃Cl, K₂SbF₂Cl₃ with constant compositions, continuous M _x M′_2−x SbF₅ (0<x<2) and limited M _x M′_1−x SbF₄ (0.25<x<0.75; M, M′=K, Rb, Cs, and NH₄) solid solutions or LiF+MSbF₄ (M=Na, K, Rb, and Cs), M₂SbF₅+Cs₂SbF₅ (M=Na and K) and MSbF₄+NaSbF₄ (M=Rb and NH₄) mechanical mixtures were determined. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 103–108, January, 1999.     

Effect of medium on the rate constant of decomposition of di(tert-butyl)trioxide

It was found that the medium affects the rate constant of the thermal decomposition of di(tert-butyl)trioxide. In all solvents studied, the decomposition occurred according to the first-order law. The effect of the solvent on the rate constant was analyzed within the framework of the Koppel-Palm equation.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1167–1168, June, 1995.The authors are grateful to O. N. Makarova for help in this work.This study was financially supported by the Russian Foundation for Basic Research (Grant No. 93-03-5231).     

Trifluoroethylxanthate as an Analytical Reagent: AAS of Zinc,Antimony and Lead After Coprecipitation of Their Trifluoroethylxanthates onto Microcyrstalline Naphthalene

Abstract

A sensitive method has been developed for the direct atomic absorption spectrometric determination of zinc, antimony and lead after coprecipitation of their trifluoroethylxanthates onto microcrystalline naphthalene. The metal xanthates are quantitatively coprecipitated over the pH ranges: Zn, 5.9–8.4; Sb, 4.0–6.0 and Pb, 4.0–11.0. The solid mass consisting of the metal complex and naphthalene is dissolved in DMF. This solution is aspirated into an air-acetylene flame at 213.9, 217.6 and 217.0nm for Zn, Sb and Pb, respectively. Beer's law is obeyed in the concentration range 2–50, 3–90 and 5–60 μg of Zn, Sb and Pb, respectively in 10ml of the final DMF solution. RSDs are at the ± (0.5–0.6)% level (n=10). The concentration for 1% absorption is 0.019, 0.035 and 0.060μg/ml for Zn, Sb and Pb, respectively. The method is suitable for the preconcentration of the metals from a larger volume of the aqueous phase, and has been employed for their determination in standard reference materials. It may be employed for the simultaneous determination of Zn, Pb and Sb in a solution by pH control.     

Solid-state chemiluminescence assay for ultrasensitive detection of antimony using on-vial immobilization of CdSe quantum dots combined with liquid–liquid–liquid microextraction

On-vial immobilized CdSe quantum dots (QDs) are applied for the first time as chemiluminescent probes for the detection of trace metal ions. Among 17 metal ions tested, inhibition of the chemiluminescence when CdSe QDs are oxidized by H₂O₂ was observed for Sb, Se and Cu. Liquid–liquid–liquid microextraction was implemented in order to improve the selectivity and sensitivity of the chemiluminescent assay.