火焰原子吸收法测定钡硅中钡铝钙

钡硅是在硅铁中增加钡元素的一种新型铁合金,主要作孕育剂用于铸造工业;采用化学分析方法测定钡铝钙三元素,只能单测,操怍繁琐费时。ICP-AES法需要贵重的进口仪器,在国产原子吸收分析仪上我们进行了试验测试,在同一份溶液中再经适当的稀释处理,加入消电离剂测定钡铝钙三元素,方法简便、快速、准确,能够满足分析要求。 1 试验部分 1.1 仪器与试剂 3300原子吸收分光光度计(上海分析仪器厂) WM-2A型无油气体压缩机(天津市医疗器械二厂) 氯化钾、氯化锶均为2％     

116例冠心病患者血清中钙镁钡铝锶含量的研究

测定１１６例冠心病患者血清中钙，镁，钡，铝和锶的含量并与正常值比较，常量元素钙，镁和微量元素锶降低，而微量元素钡和铝升高，它们之间的差异都有显著或高度显著性。Ｐ〈０．０５或Ｐ〈０．０１。     

二溴对甲基偶氮磺光度法测定硅钡镁合金中钡含量

硅钡镁铁合金是炼钢用无铝脱氧剂,是对钢液进行深脱氧脱硫最有效的高级复合合金,对于不要求酸溶铝的钢,在脱氧剂合金用量相同的条件下,对钢液进行深度脱氧脱硫,可使钢中的含氧量降低,氢化物减少,提高钢的纯度。目前,铁合金中钡的测定多采用重量法[1]或滴定法[2,3],这两种方法分析速度慢,分析准确性、可靠性差[4]。二溴对甲基偶氮磺是一种测定铅含量的显色剂[5],在磷酸介质中对钡有很好的灵敏度和选择性,在常温下迅速形成灵敏、稳定的蓝色配合物,能快速、准确地测定钡含量。在磷酸介质中钡与二溴对甲基偶氮磺形成蓝色配合物,最大吸收波长为62…     

EDTA容量法测定硅钡钙合金中钡

硅钡钙合金是一种在硅铁中加入钡和钙元素的新型合金,主要应用于铸造工业中作为孕育剂,目前还未制定出相应的国家标准和行业标准,对于其中测定钡元素的方法,文献报道有ICP-AES法和原子吸收法。而前法需贵重仪器,难以普及,只能测定低含量钡,后法由于在553.6nm处会发生氢氧化钙带背景吸收干扰,从而影响测定结果的准确度和精度。本文介绍一种采用EDTA容量法测定硅钡钙合金中钡元素的简便方法。     

示波极谱法测定硅锶钡铁合金中的锶和钡

Sr—Si—Fe合金中含1—5％的Sr,现有的化学分析方法是采用EDTA络合滴定。而在冶炼过程中尚需加入大致相等量的Ba,故此需Ba、Sr同时测定。其它方法分析如此含量的Ba、Sr总还存在一些困难。本文采用示波极谱法,以四甲基碘化铵为支持电解质,成功的测定了硅锶钡铁合金中的Sr和Ba。峰值电位Ba为-1.95V,Sr为-2.15V(vs SCE),Sr或Ba浓度在0.1—     

钡钙合金中钡和钙的快速测定

由于钡离子对乙二胺四乙酸(EDTA)滴定法测定钙存在较大干扰,排除困难,目前未见滴定法测定钡合金中钙离子较好的报道.通常硅钡合金、硅钡铝合金中钡的测定都采用硫酸钡重量法[1,2],但该方法需多次分离沉淀,手续繁杂操作不便.     

石墨炉原子吸收光谱法测定硅钡合金中钡和锶

硅钡合金作为炼钢工业的脱氧、脱硫、除磷、降铝的添加剂和铸造孕育剂已得到广泛应用。硅钡合金中钡的测定大多采用化学法[1-5],包括重量法和滴定法,操作繁琐,耗时长。由于钡与锶性质相近,试     

ICP-AES法测定硅铝钡钙合金

硅铝钡钙合金是炼钢常用的复合脱氧剂[1] ,它具有较强的脱氧能力和使夹杂物变质的能力 ,同时还能脱硫[2 ] 。硅铝钡钙合金目前既无国家标准分析方法 ,又无较成熟的化学分析方法 ,本文研究了用ＩＣＰ发射光谱仪测定硅铝钡钙合金的方法。本法采用基准物质配制标准系列绘制工作曲线 ,并用回收试验和试样精密度试验来证实方法的可靠性。1　试验部分1.1　仪器与试剂美国ＰＥ公司的ＯＰＴＩＭＡ330 0型全谱直读电感耦合等离子体发射光谱仪铝、钡、锶、锰、钙、磷、铁标准溶液 :用光谱纯金属氧化物或基准物质分别配置成 1ｍｇ·ｍｌ-1的储备液 ,使…     

高频燃烧-红外吸收光谱法测定钙铝合金球中碳的含量

<正>钙铝合金球是一种以钙、铝为主要元素的环保型脱氧剂,作为炼钢辅料,对改变钢液杂质形态、细化晶粒、改善钢的加工性能、提高钢材质量有明显作用^[1-2]。目前市场上的钙铝合金球都含有一定程度的杂质元素,而碳作为主要杂质元素,对钢材的强度、硬度、塑性和韧性都会有一定的影响,所以准确测定钙铝合金球中碳的含量对指导炼钢工艺及优化钢材性能具有重要意义^[3]。     

硅钡钙联合测定

硅钡钙是炼钢中很好的新型脱氧剂 ,并且有很好的脱硫、磷能力 ,对冶炼含硫、磷较低的钢种起着非常重要的作用 ,在特钢系统有着广阔的应用前景。本文提出了硅钡钙联合测定分析方法 ,该法快速、准确、简便、易掌握。1　试验部分1 .1　试剂混合熔剂 :无水碳酸钠 硼砂 过氧化钠 =2 0 1 0 3,硼砂在 350°C马弗炉中烘去结晶水分。NH4 CNS:50 g· L-1Ag NO3溶液 :1 0 g·L-1(NH4 ) 2 SO4 溶液 :1 0 0 g·L-1Ba Cl2 溶液 :1 0 0 g·L-1KOH溶液 :40 0 g·L-1EDTA标准溶液 :0 .0 2 mol· L-1,称取 EDTA基准试剂 7.4452 g溶于水中 ,用…     

Synthesis and structure of hydroxyisoxazolidines and derivatives of hydroxylamine and alkenals

The reactions of N-substituted hydroxylamines with alkenals serve as a method for the synthesis of the corresponding 2-substituted 3(5)-hydroxyisoxazolidines. The reaction pathway is determined by the nature of the substituent attached to the nitrogen atom. Ring-chain isomerism has been detected in these newly obtained compoundsTranslated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1270–1276, September, 1987.     

Synthesis and characterization of triazenide and triazene complexes of ruthenium and osmium

Triazenide [M(eta2-1,3-ArNNNAr)P4]BPh4 [M = Ru, Os; Ar = Ph, p-tolyl; P = P(OMe)3, P(OEt)3, PPh(OEt)2] complexes were prepared by allowing triflate [M(kappa2-OTf)P4]OTf species to react first with 1,3-ArN=NN(H)Ar triazene and then with an excess of triethylamine. Alternatively, ruthenium triazenide [Ru(eta2-1,3-ArNNNAr)P4]BPh4 derivatives were obtained by reacting hydride [RuH(eta2-H2)P4]+ and RuH(kappa1-OTf)P4 compounds with 1,3-diaryltriazene. The complexes were characterized by spectroscopy and X-ray crystallography of the [Ru(eta2-1,3-PhNNNPh){P(OEt)3}4]BPh4 derivative. Hydride triazene [OsH(eta1-1,3-ArN=NN(H)Ar)P4]BPh4 [P = P(OEt)3, PPh(OEt)2; Ar = Ph, p-tolyl] and [RuH{eta1-1,3-p-tolyl-N=NN(H)-p-tolyl}{PPh(OEt)2}4]BPh4 derivatives were prepared by allowing kappa1-triflate MH(kappa1-OTf)P4 to react with 1,3-diaryltriazene. The [Os(kappa1-OTf){eta1-1,3-PhN=NN(H)Ph}{P(OEt)3}4]BPh4 intermediate was also obtained. Variable-temperature NMR studies were carried out using 15N-labeled triazene complexes prepared from the 1,3-Ph15N=N15N(H)Ph ligand. Osmium dihydrogen [OsH(eta2-H2)P4]BPh4 complexes [P = P(OEt)3, PPh(OEt)2] react with 1,3-ArN=NN(H)Ar triazene to give the hydride-diazene [OsH(ArN=NH)P4]BPh4 derivatives. The X-ray crystal structure determination of the [OsH(PhN=NH){PPh(OEt)2}4]BPh4 complex is reported. A reaction path to explain the formation of the diazene complexes is also reported.     

Mass and NMR spectra of haplophyllidine and perforine and of their derivatives

Conclusions The mass and NMR spectra of haplophyllidine, perforine, and their derivatives have been studied. The influence of the open and cyclic forms of the molecular ion on the nature of the fragmentation has been discussed. The main routes of fragmentation of the compounds considered are due to the presence of substituents at C₈ and C₄.Khimiya Prirodnykh Soedinenii, Vol. 5, No. 4, pp. 273–279, 1969     

Crystal and molecular structure of aroyl- and acetylhydrazones of acet- and benzaldehydes

Aroyl- and acetylhydrazones of acet- (I) and benzaldehydes (IV) and benzoylhydrazones of acet- (II) and benzaldehydes (III) were studied by x-ray structural and quantum-chemical methods in order to establish their structures. Compund (I) was the EEZ structure in the crystal. Calculations and spectral data showed that the EEE form occurs in nonpolar solvents and in the gas phase. According to crystallographic data molecules (I)–(IV) are the E-isomers (relative to the N-N bond) and the hydrazone fragments are planar. Intermolecular N-H...O H-bonds from in the crystals. The data obtained suggest that the majority of acylhydrazones are conformationally rigid on dissolution although exceptions do occur. Apparently the reasons for the difference of acetyl- and benzoylhydrazones in electrocarboxylation reactions are electronic and not steric factors.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 1, pp. 75–81, January, 1991.     

Investigation of adhesion and mobility of polyurethane and epoxy-rubber glues and adhesives

The values of activation parameters in uncured and cured epoxy resins, rubbers, and blends thereof are investigated. The dependences of activation energy and adhesion strength of epoxy-rubber compositions on rubber content are determined. The correlation of adhesion and activation energy values for polyurethane rubber and epoxy-rubber compositions is shown.     

Preparation and characterization of diarylphosphazene and diarylphosphinohydrazide complexes of titanium, tungsten and ruthenium and phosphorylketimido complexes of rhenium

Reaction of the proligand Ph2PN(SiMe3)2 (L1) with WCl6 gives the oligomeric phosphazene complex [WCl4(NPPh2)]n, 1 and subsequent reaction with PMe2Ph or NBu4Cl gives [WCl4(NPPh2)(PMe2Ph)] (2) or [WCl5(NPPh2)][NBu4] (3), respectively. DF calculations on [WCl5(NPPh2)][NBu4] show a W=N double bond (1.756 A) and a P-N bond distance of 1.701 A, which combined with the geometry about the P atom suggests, there is no P-N multiple bonding. Reaction of L1 with [ReOX3(PPh3)2] in MeCN (X = Cl or Br) gives [ReX2(NC(CH3)P(O)Ph2)(MeCN)(PPh3)](X = Cl, 4, X = Br, 5) which contains the new phosphorylketimido ligand. It is bound to the rhenium centre with a virtually linear Re-N-C arrangement (Re-N-C angle = 176.6 degrees, when X = Cl) and there is multiple bonding between Re and N (Re-N = 1.809(7) A when X = Cl). The proligand Ph2PNHNMe2(L2H) reacts with [(C5H5)TiCl3] to give [(C5H5)TiCl2(Me2NNPPh2)] (6). An X-ray crystal structure of the complex shows the ligand (L2) is bound by both nitrogen atoms. Reaction of the proligands Ph2PNHNR2[R2 = Me2 (L2H), -(CH2CH2)2NCH3 (L3H), (CH2CH2)2CH2 (L4H)] with [{RuCl(mu-Cl)(eta6-p-MeC6H4iPr)}2] gave [RuCl2(eta6-p-MeC6H4iPr)L] {L = L2H (7), L3H (8), L4H (9)}. The X-ray crystal structures of 7-9 confirmed that the phosphinohydrazine ligand is neutral and bound via the phosphorus only. Reaction of complexes 7-9 with AgBF4 resulted in chloride ion abstraction and the formation of the cationic species [RuCl(6-p-MeC6H4iPr)(L)]+ BF4- {(L = L2H (10), L3H (11), L4H (12)}. Finally, reaction of complex 6 with [{RuCl(mu-Cl)(eta6-p-MeC6H4iPr)}2] gave the binuclear species [(eta6-p-MeC6H4iPr)Cl2Ru(mu2,eta3-Ph2PNNMe2)TiCl2(C5H5)], 13.     

Ti-V基储氢合金及其氢化物的物相结构与组分优化设计

Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB₅型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。