Rapid,quantitative analysis of americium,curium and plutonium isotopes in Hanford samples using extraction chromatography and precipitation plating

Recently developed methods for the rapid, quantitative analysis of americium (Am), curium (Cm), and plutonium (Pu) isotopes in Hanford soil, sludge, and waste-tank samples are described. After dissolution, dilutions are made as necessary based on alpha-energy analysis of a small aliquot of the original solution. Isotopic tracers are then added and Am-Cm and Pu are separated by extraction chromatography, coprecipitated with neodymium fluoride, and counted. Examples of alpha spectra are given, and results obtained for Hanford sludge samples are presented.     

Spectrometric analysis of non-metals introduced from a graphite furnace into a microwave-induced plasma

A low-power helium microwave-induced plasma, sustained in a cylindrical TM(010) cavity, has been used with sample introduction from a graphite furnace. An end-on optical configuration was employed to monitor both atomic and ionic emission from Cl, I, S and P. The operating parameters were optimized with respect to the nature of the plasma background response, the limits of detection, and the shapes and linearity ranges of the log-log analytical working curves. Possible applications were evaluated by determining iodine in milk and analysing a multi-component mixture of sulphur compounds.     

Liquid-liquid extraction of transition and alkali metal cations by a new calixarene: Diphenylphosphino calix[4]arene methyl ether

The liquid-liquid extraction of various metal ions by a diphenylphosphino calix[4]arene (1) using picrate counter ion has been studied and compared with those ofp-tert-butyl-calix[4]arene methyl ether (2) and triphenylphosphine (3). The calixarene 1 shows strong binding ability to almost all metal cations examined, but calixarene 2 shows little ability to extract any of them. Based on the continuous variation method, calixarene 1 formed 1: 2 complexes with copper(II) ion.     

First Higher‐Order Photocycloaddition to a CN Bond: 1,3‐Diazepines from Maleimides

A light touch is all that is required to cleave a maleimide C? N bond to effect a [5+2] photocycloaddition with a sterically encumbered C?N moiety (see scheme).

     

Formation of mixed monolayers of silsesquioxanes and alkylsilanes on gold

The formation of mixed monolayers of hydridospherosilsesquioxane clusters (H(8)Si(8)O(12)) and alkylsilanes (H(2n+1)C(n)SiH(3)) on Au has been investigated using X-ray photoelectron and reflection-absorption infrared spectroscopies and scanning tunneling microscopy. All of the techniques indicate the displacement of the majority of the siloxane clusters from the surface in favor of the alkylsilane.     

Determination of ceruloplasmin in human serum by SEC-ICPMS

This paper describes an analytical method for the determination of ceruloplasmin (Cp) in human serum. The method uses immunoaffinity chromatography and size-exclusion chromatography (SEC) to “purify” the serum sample prior to analysis of ⁶³Cu and ⁶⁵Cu by inductively-coupled plasma mass spectrometry (ICPMS). By removing the six most abundant proteins from serum with immunoaffinity chromatography and by using SEC to separate Cu bound by Cp from any free Cu that might be present in the serum sample, we demonstrated that SEC-ICPMS can accurately and reproducibly measure Cp in the ERM DA470 reference serum. Cp identification is based on retention time match of the unknown in the serum sample with the Cp external standard and the presence of ⁶³Cu and ⁶⁵Cu at a ratio of 2.2±0.1. This method was used to analyze a reference serum certified for Cp, 47 serum samples from four different diseases and a set of normal controls. The reference serum and a serum sample from a patient with myocardial infarction, as well as a Cp standard, were also analyzed by electrospray mass spectrometry to confirm the presence of Cp in the SEC fraction known to contain ⁶³Cu.