Fortschritte in der Auswertung von Markierungsversuchen an dynamischen Systemen

In einem dynamischen System vollziehen sich kontinuierlich ablaufende Stoffwandlungen, deren Ausgangsstoffe dem System ständig zufließen und deren Folgeprodukte das System kontinuierlich verlassen. Es wird das Verhalten eines solchen Systems mit drei Pools bei Markierungsexperimenten untersucht. Die Ergebnisse dieser mathematischen Untersuchungen werden auf die Erforschung des Stickstoffstoffwechsels laktierender Rinder mit Hilfe des stabilen Isotops ¹⁵N angewandt. In diesem Fall enthält das dynamische System zwei kleine stoffwechselaktive Pools und einen großen, niclit intensiv am Stoffwechsel beteiligten Körpereiweiβ-Pool.     

Beobachtung des Stickstoffstoffwechsels bei Leguminosen mittels 15N

Es war Ziel dieser Arbeit, zu ermitteln, welchen Einfluß höhere Dosen von Stickstoffdüngemitteln in Form von KNO₃ auf die Menge des in der Pflanze fixierten Luftstickstoffs haben. Als Versuchspflanze wählten wir Pferdebohnen (Vicia faba, Chlumetzer Abart) wegen ihrer vielseitigen Verwendung in der Landwirtschaft und ihrer besonderen experimentellen Eignung.     

Über den Einfluß von Isotopieeffekten auf die Verbreitung der Isotope in der Natur

Die Isotopenzusammensetzung der chemischen Elemente in ihren natürlichen Vorkommen wird von kernphysikalischen Vorgängen, vom Einfall extraterrestrischer Materie und, namentlich bei den leichten Elementen (etwa bis zum Chlor), von kinetischen und thermodynamischen Isotopieeffekten beeinfluβt. Deshalb ist die Kenntnis der in der Natur wirkenden Isotopieeffekte eine entscheidende Voraussetzung für das Verständnis der Gesetzmäβigkeiten der Verbreitung der Isotope in der Natur und für die Anwendung dieser Gesetzmäβigkeiten als Mittel der geo- und kosmoswissenschaftlichen Forschung und der Umweltforschung [1].     

Determination of Lead in Human Hair by High Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry with Microwave Digestion and Solid Sampling

The content of lead in human hair was measured by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) combined with microwave-assisted digestion (MAD) and direct solid sampling (DSS). Hair strands were washed, dried, and then cut into three parts (root, middle portion, and tip). For MAD-GFAAS assays, approximately 0.25 g of hair was completely digested using a mixture of concentrated nitric acid and hydrogen peroxide in a closed system. In the DSS-GFAAS assays, 0.1–0.2 mg of dried hair was directly introduced into a graphite furnace using a solid autosampler. The temperature programs were optimized and the effects of various added modifiers were compared. The results indicated that NH₄H₂PO₄ was the optimal modifier for analysis of Pb using GFAAS. Use of the optimal modifier and temperature program gave similar limits of detection for MAD-GFAAS and DSS-GFAAS of 1.16 ng/g and 0.82 ng/g, respectively. Both methods also produced satisfactory recoveries ranging from 98.69% to 103.14%. There was no significant difference observed between the Pb contents of hair strands determined by the MAD-GFAAS and DSS-GFAAS assays, which both indicated that the Pb levels increased along the hair strands. Comparison of the two methods revealed that DSS-GFAAS had several advantageous characteristics over MAD-GFAAS, including the need for much less sample material and having a less time-consuming procedure, lower sample blank absorbance, lower memory effect, and no risk of environmental pollution by digesting chemicals. The direct solid sampling technique can be employed as a good alternative to conventional wet digestion in AAS assays.     

Use of a Tensammetric Wave for the End-Point Detection in Chelatometry

Abstract

A new method for the end-point detection in complexometric titration using a tensammetric wave of organic reagents such as oxine and alizarin complexone (ALC) was studied. The tensammetric wave of these reagents disappears by their chelate formation and reappears by the liberation of free indicator during the exchange reaction between indicator chelate and EDTA. This mechanism is utilized for the end-point detection in complexometric titration of metals. Since the sensitivity of tensammetric wave is extremely high, very sharp end-point can be obtained for the titration of metals even in the concentration of 10^?5M.     

PbII 4,4,4-trifluoro-1-naphthyl-1,3-butanedione complexes of 1,10-phenanthroline and 2,2′-bipyridine ligands

Lead(II) 4,4,4-trifluoro-1-naphthyl-1,3-butanedione (Htfnb) complexes of 1,10-phenanthroline (phen) and 2,2′-bipyridine (bpy), [Pb₂(bpy)₂(tfnb)₂] (1) and [Pb₂(phen)₂(tfnb)₂] (2), have been synthesized and characterized by elemental analysis, IR, spectroscopy and X-ray crystallography. The self-assembly of 1 and 2 is likely to be caused by C–H ··· F–C, C–H ··· O and π–π stacking interactions.     

Lead(II) complexes of 2,2′-diamino-4,4′-bithiazole (DABTZ) including crystal structure of a novel 1D chain polymer, [PB(DABTZ)(μ-SCN)(μ-NO3)] n

Three new 2,2′-diamino-4,4′-bithiazole (DABTZ) lead(II) complexes were synthesized and characterized by elemental analyses, IR-, ¹H-NMR-, and ¹³C-NMR-spectroscopy. The single crystal X-ray structural analysis of [Pb(DABTZ)(μ-SCN)(μ-NO₃)] _n shows the complex to be a 1D chain polymer as a result of sequential thiocyanate and nitrate bridging. The Pb atoms are seven-coordinated by two nitrogen atoms of the 2,2′-diamino-4,4′-bithiazole, three nitrate and two thiocyanate ligands. The arrangement of the 2,2′-diamino-4,4′-bithiazole, nitrate and thiocyanate ligands does not suggest a gap in the coordination around the Pb^II ion, caused by a stereo-active lone pair of electrons on lead(II) where the coordination around the lead atoms is the less common holodirected.     

各色硝基铅笔漆中“可溶性”铅含量的测定

我们采用国家标准GB 9760[1]和GB9758.1[2]对各色硝基铅笔漆中"可溶性"铅含量进行了测定。本文对实验中酸萃取物的制备,样品的处理以及仪器最佳工作条件的选择等进行了研究。实验结果表明,只要根据样品实际情况,选择分离硝基漆中颜料效果最好的溶剂或混合溶剂,严格地遵守GB9760和CB9758.1实验步骤的全部细目等。就能得到足够的精密度,使实验获得成功。     

食用坚果中铅含量的分析

采用原子吸收光谱法对食用坚果中污染元素铅的含量进行了分析。铅在0.00～2.00 μg·mL-1范围内具有线性关系,r=0.999 1,测定铅的RSD≤4.64%,标准加入法测定铅的回收率94.0%～102.0%,方法简单,结果准确。