Bestimmung von Calcium, Magnesium, Strontium, Kalium, Natrium, Lithium, Eisen, Mangan, Chrom, Nickel, Kupfer, Cobalt, Zink und Cadmium

Zusammenfassung Für 14 Elemente wird eine universelle Methode beschrieben. Durch Zusatz von Lanthan und Cäsium werden die physikalischen, chemischen und Ionisations-Störungen in der Flammen-AAS ausgeschaltet. Es wird gezeigt, daß diese Methode für sehr unterschiedliche Stoffe mit Erfolg angewendet werden kann, und gleichzeitig die Genauigkeit des Routinemeßverfahrens nicht beeinträchtigt wird. Nur in Ausnahmefällen muß die Additionsmethode benutzt werden.

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Determination of calcium, magnesium, strontium, potassium, sodium, lithium, iron, manganese, chromium, nickel, copper, cobalt, zinc and cadmium by flame AASA universal method for the analysis of waters, coals, ashes, ores, rocks, building materials, metals and similar samples

Summary A universal method is described for 14 elements. By addition of lanthanum and caesium the physical, chemical and ionization interferences in the flame AAS are eliminated. It is demonstrated that this method can be applied successfully for very different materials and simultaneously the precision of the standard measuring method is not affected. Only in exceptional cases the addition method has to be applied.

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Herrn Prof. Dr. W. Schuhknecht, dem langjährigen Leiter des Zentrallabors der Saarbergwerke AG (1948–1972) zum Gedenken

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Für die sorgfältige Durchführung von Säure- und Schmelzaufschlüssen sowie seine nützlichen Hinweise bei der Korrektur des Manuskriptes möchte ich Herrn Lothar Kiefer meinen besonderen Dank aussprechen.     

SYNTHESIS AND CRYSTAL STRUCTURE OF 5, 10, 15, 20, 22, 24-HEXAHYDRO-5, 5, 10, 10, 15, 15, 20, 20-OCTAMETHYL-PORPHINE

<正> The title com pound (HHOMP) has been synthesized with the pho-toinduced condensation of acetone and pyrrole in the presence of iodoaromatic hydrocarbons, and its molecular and crystal structures have been determined by X-ray analysis. C28H36N4, Mr = 428. 63, triclinic; space group P1; a =10. 165(3), b = 10. 185(2), c=13. 012(3)(?); α=85. 41(2), β=67. 84(2), γ= 89. 75(2)°; V = 1243 (?)3; Z = 2; D = 1. 145g. cm-3; μ= 0. 635cm-1; F (000) = 464. Although the HHOMP molecule twists, it is found that the four nitrogen atoms are still in a plane.     

Optimization of parameters for semiempirical methods. III Extension of PM3 to Be,Mg, Zn,Ga, Ge,As, Se,Cd, In,Sn, Sb,Te, Hg,Tl, Pb,and Bi

Using a recently developed procedure for optimizing parameters for semiempirical methods,¹ PM3 has been extended to a total of 28 elements. Average ΔH_f errors for the newly parameterized elements are Be: 8.6, Mg: 8.4, Zn: 5.8, Ga: 14.9, Ge: 11.4, As: 8.5, Se: 11.1, Cd: 2.6, In: 11.3, Sn: 9.0, Sb: 13.7, Te: 11.3, Hg: 6.8, Tl: 6.5, Pb: 7.4, and Bi: 10.9 kcal/mol. For some elements the paucity of data has resulted in a method, which, while highly accurate, is likely to be only poorly predictive.     

电感耦合等离子体质谱法(ICP-MS)测定稀土矿中钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥和钪量

通过用四酸与微波消解法溶解样品对比,建立了用硝酸、盐酸、氢氟酸、高氯酸分解样品,采用电感耦合等离子体质谱法(ICP-MS)测定稀土矿中16种元素含量。方法采用_¹⁰³Rh作为内标消除干扰,确定了最优测定条件,16种稀土元素检出限为0.0029-0.0099ng/mL,测定范围为0.0005-0.020%。精密度试验、加标回收试验及标准物质检测,结果验证了方法的可行性及准确性。该方法简单易操作,结果可靠,能满足实验分析要求。     

Sulfat-, Hydrogensulfat-, Pyrosulfat-, Peroxydisulfat-, Thiosulfat-, Dithionat-, Trithionat-, Tetrathionat- und Pentathionationen

Ohne Zusammenfassung     

Conjugate addition reactions of alpha-aminoalkylcuprates with alpha, beta-alkenyl-, alpha,beta-alkynyl-, alpha,beta-beta,gamma-allenyl-, and alpha,beta-gamma,delta-dienyl carboxylic acid derivatives, nitriles, and sulfoxides

alpha-Aminoalkylcuprates prepared from alpha-lithio carbamates and CuCN.2LiCl participate in 1,4-addition reactions with alpha, beta-unsaturated esters, thiol esters, imides, and nitriles in poor to excellent yields depending upon the electron-withdrawing substituent and the substitution pattern of the unsaturated substrate. These reagents also undergo conjugate addition reactions with alpha,beta-alkynyl esters, sulfoxides, and nitriles and with alpha,beta-beta,gamma-unsaturated allenyl esters. Excellent stereocontrol is achieved in the conjugate additions of alpha-aminoalkylcuprates to the allenyl esters, while poor stereoselectivity results in the conjugate additions to the alkynyl derivatives. Deprotection and cyclization of the alkynyl adducts affords pyrrolin-2-ones, while similar treatment of the allenyl adducts affords 4-alkylidine- pyrrolidin-2-ones and pyrrolizidinones.     

猪胰脏中铁钙镁铜铅锌镉锰钴镍的测定

采用硝酸－过氧化氢在自动回流消化仪中消化猪胰脏,火焰原子吸收光度法测定铁、钙、镁、铜、锌、铅、镉、锰、钴、镍的含量。,方法简便,快速,结果令人满意,并对猪胰脏食用价值进行了评价。     

1.1 Grundlagen,Methoden, Apparate,Reagentien, Automation,Datenverarbeitung

Analytical and Bioanalytical Chemistry -     

Bestimmung von As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, V und Zn in Kohlen, Additiven, Flugaschen und Impaktorfilterst?uben aus Kohlekraftwerken

Summary The analysis of coal, additives and combustion residues of coal-fired power plants is described. The selection of the best decomposition method has a special meaning for the type of sample (coal, additive etc.) as also for the elements to be determined in the different samples. There is no universal method which fits all the different samples and no universal determination system for this problem. Problems of the determination of chromium and arsenic are described and discussed due to the matrix and the decomposition technique. The determination with another independent method and the measurement of certified reference material is a good approach to the true value of the elements to be determined in the samples.     

KCl-NaCl(1:1mol)-RECl3熔体的电导率(RE=La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y、Ce族、Y族)

用交流电桥法测定了熔融KCl-NaCl(1:1摩尔)-RECl₃的电导。比电导的温度函数表达式如下: κ=A+B(t-700) κ:比电导(Ω^-1·cm^-1);t:温度(700—850℃); A、B:本文给出的常数。讨沦了实验值与计算值的偏差,当稀土氯化物在熔体中的浓度为10—50重量百分数时可能形成了络合物。     

Instrumental neutron activation determination of Pt, Ru, Ir, Sc, Cr, Fe, Co, La, Ce, Nd, Sm, Yb, Lu, Hf and Ta employing CIRUS reactor as a thermal neutron source

An accurate and simple method has been developed for the determination of Pt, Ru, Ir and other elements employing instrumental neutron activation analysis (INAA). Nondestructive analysis has been carried out for the determination of these elements in different rock samples such as Dolerite, Dyke Dolerite, Country Basalt, Hyaloclastite, Trachyte, Ijolite, Spillite, Diorite and Lamprophyre from various locations like Daman, Tapti, Murud, Talasari, Ranala and Bassein in Maharashtra state. High flux provided by the CIRUS reactor (1×10¹³ n cm^–2s^–1) has been used for thermal neutron bombardment followed by radioassaying of the (n,) products on a HPGe detector coupled to a PC-based MCA unit.     

Syntheses, structure, some band gaps, and electronic structures of CsLnZnTe3 (Ln=La, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Y)

Eleven new quaternary rare-earth tellurides, CsLnZnTe3 (Ln=La, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, and Y), were prepared from solid-state reactions at 1123 K. These isostructural materials crystallize in the layered KZrCuS3 structure type in the orthorhombic space group Cmcm. The structure is composed of LnTe6 octahedra and ZnTe4 tetrahedra that share edges to form [LnZnTe3] layers. These layers stack perpendicular to [010] and are separated by layers of face- and edge-sharing CsTe8 bicapped trigonal prisms. There are no Te-Te bonds in the structure of these CsLnZnTe3 compounds so the formal oxidation states of Cs/Ln/Zn/Te are 1+/3+/2+/2-. Optical band gaps of 2.13 eV for CsGdZnTe3 and 2.12 eV for CsTbZnTe3 were deduced from single-crystal optical absorption measurements. A first-principles calculation of the density of states and the frequency-dependent optical properties was performed on CsGdZnTe3. The calculated band gap of 2.1 eV is in good agreement with the experimental value. A quadratic fit for the lanthanide contraction of the Ln-Te distance is superior to a linear one if the closed-shell atom is included.     

1.1 Grundlagen, methoden, apparate, reagentien, automation, datenverarbeitung

Ohne Zusammenfassung