Polarographic Determination of Cobalt and Nickel in Iron Meteorites

Abstract

Cobalt and nickel were determined in five iron meteorites by a polarographic method. The analyses gave good precision and are believed to be reliable. The nickel content ranged from 6.49% to 8.07%, and cobalt ranged from 0.40% to 0.49%. Atomic absorption measurements were made on the sample solutions for comparison.     

Triphenylamine derivatized phenylacetylene macrocycle with large two-photon absorption cross-section

A phenylacetylene macrocycle (PAM) derivative containing triphenylamine as the framework was synthesized in one-step Sonogashira coupling. The photophysical and electrochemical properties were investigated in details. This hexamer shows significant enhancement in two-photon absorption cross-section relative to reported PAM derivatives.     

Determination of Cadmium and Lead in Sea Water after Extraction Using Electrothermal Atomisation. Minimisation of Interferences from Co-Extracted Sea Salts

Abstract

Interferences from small amounts of sea salt in the determination of cadmium and lead were investigated. Test samples were made to mimic solutions obtained after extraction of sea water for trace metal analysis. Sea salt concentrations in the range 0–400 mg/l were investigated. Background absorption from this salt was high but easily minimised through the addition of nitric acid (2 % v/v). Sensitivity reductions due to the salt were considerable and varied from one graphite tube to the other. This problem was overcome by the addition of 1000 mg lanthanum per litre of sample. The positive effect of the lanthanum matrix modification is thought to be due to a change of the graphite tube surface.     

Determination of Iron in Calf Serum Using Bathophenanthroline and Thermal Lens Spectrometry

ABSTRACT

Thermal lens spectrometry has been used for the determination of iron in calf serum. The method is based on dissociation of Fe³⁺ from proteins, reduction of Fe³⁺ to Fe²⁺ and formation of a coloured complex between Fe²⁺ and bathophenanthroline. Contrary to the spectrophotometric method, it is shown that thermal lens spectrometry is less sensitive to scattering caused by the presence of small particles remaining in the test solution after the deproteinization step. The background signal is very small and the response is only slightly dependent on the amount of scattering particles. The method is reliable, sensitive and reproducible. The limit of detection for iron is 4 ppb and the relative standard deviation is around 2%. It is expected that the volume of serum sample necessary for an analysis can be reduced to less than 100 μl.     

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.     

Separation and Analysis of o.p'-DDD and its Lipophilic Metabolite,O.P'-DDE,in Tissue,Faeces and Plasma

Abstract

An analytical procedure based on electron capture gas chromatography for the determination of o,p′-DDD, a drug used for the treatment of Cushing′s syndrome, is presented. Detection of a metabolite, identified as o,p′-DDE, is also described.     

Transformation of macromonomers into ring‐opening polymerization macroinitiators: A detailed initiation efficiency study

In the present study, n‐butyl acrylate macromonomer (BAMM) (M_n = 1900 g mol^?1; PDI = 1.96) has been synthesized via a high‐temperature polymerization process. Subsequently, the olefinic termini of the BAMM have been transformed into a diol via a dihydroxylation process using KMnO₄ as an oxidizing agent. The OH‐terminated macroinitiator pBA(OH)₂ has subsequently been employed for the ring‐opening polymerization (ROP) of ε‐caprolactone via various catalytic systems, that is, organo‐(1,5,7‐triazabicyclo[4.4.0]dec‐5‐ene), metal (tin(II) 2‐ethylhexanoate), and enzymatic catalysis (Novozym® 435). The obtained pBA‐b‐pCL block copolymers and the initiation efficiency of the BAMM macroinitiator have been investigated via size exclusion chromatography (SEC), electrospray ionization–mass spectrometry (ESI‐MS) hyphenated with SEC and liquid chromatography at the critical conditions of both poly(ε‐caprolactone) (pCL) and pBA. The in vitro enzyme catalysis (eROP) approach proved to be the most efficient catalysis system due to minor transesterification side reactions during the polymerization process. However, side reactions such as transesterifications occur in each catalytic system and—while they cannot be suppressed—they can be minimized. The species generated during the eROP process include the desired block copolymer pBA‐b‐pCL as main species as well as pCL homopolymer and residual macroinitiator pBA(OH)₂. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

Abundant Intramolecular Ring Rearrangements of 1-(N-Benzyloxycarbonylamino)arylmethylphosphonate Phenyl monoesters Under Electrospray Ionization Conditions

Abstract

The mass spectrometric behavior of 1-(N-benzyloxycarbonylamino)arylmethyl-phosphonate phenyl monoesters was investigated under positive ion electrospray ionization conditions. All nitrogen-protonated title compounds undergo four- and/or six-membered ring rearrangements to yield nitrogen-containing fragment ions by consecutive or simultaneous loss of a carbon dioxide and phenyl hydrogen phosphonate or phenyl benzylphosphonate or an arylmethylimine. All oxygen-protonated title compounds undergo four- to six-membered ring rearrangements to produce fragment ions by loss of a carbon dioxide plus an arylmethylimine, or phenyl benzylphosphonate, by consecutive or simultaneous loss of benzyl phenyl ether and isocyanic acid. The fragmentation is obviously different from the corresponding methyl and ethyl monoesters, which show a tendency to undergo intramolecular four-membered ring rearrangements only.

GRAPHICAL ABSTRACT