The rapid and accurate determination of the relative stereochemistry of some postulated chlorinated polycyclodiene pesticide metabolites without excessive dependence on chemical methods is described. Proton assignments were made employing the new nuclear magnetic resonance (n.m.r.) shift reagent, Eu(DPM),, which effected the separation of superimposed signals in these systems. The assignments based on coupling constant information and requiring spin decoupling equipment are in good agreement with those obtained from the Eu(DPM), studies. The data presented establishes the relative stereochemistry of these biologically important compounds and demonstrates the utility of one or both approaches in elucidating their overall structures.On d6crit une m6thode rapide et pr6cise de determiner sans d6pendre d'une facon excessive sur des m6thodes chimiques la stCr6ochimie relative de quelques mktabolites postul6s de pesticides de polycyclodienes chlor6s. On a assign6 les diff6rents protons en utilisant, en r.m.n., le r6actif Eu(DPM), qui permet de s6parer les signaux qui seraient par ailleurs superpos6s dans ce systeme. Les attributions faites en se basant sur des constantes de couplage ou n6cessitant I'utilisation d'equipement pour le d6couplage des spins sont en bon accord avec celles d6coulant des Ctudes faites avec Eu(DPM),. Les donn6es pr6sentCes permettent d'6tablir la stkrkochimie relative de ces compos6s biologiquement importants et d6montrent I'utilitC de chacune des mkthodes dans 1'6lucidation des structures.

The high resolution nuclear magnetic resonance spectra of 35 carbamate pesticides and a major metabolite of one pesticide are discussed. The chemical shifts and coupling constants are tabulated and reproductions of the more complex or unusual spectra are included. A concentration and solvent dependence of both the NH-proton and the NCH3-proton resonances of an N-monosubstituted carbamate is discussed. Hindered rotation is observed in the N,N-dimethylcarbamates, the thiolcarbamates and the dithiocarbamates, but not in the N-methylcarbamates.

Publications from 1969 through 1974 reporting organic and spark source mass spectrometric studies on environmental samples have been compiled. Emphasis is placed on pollutants identified, but some methods and techniques are discussed. The 396 reports cited vary from those reporting hundreds of identified pollutants to those describing the analysis of only one sample containing one or a few pollutants. Reports concerning forensic, synthetic and standard samples, and analyses for drug residues. metabolites and degradation products are not included

The high resolution nuclear magnetic resonance spectra of the DDT class of pesticides and related compounds are discussed, including a study of the resonances of the aromatic protons as they are affected by various substiluents. The CCl3 moiety on the α-carbon strongly deshields the ortho protons on the aromatic rings, and this deshielding effect is greatly enhanced by substitution of a chlorine ortho rather than para on the aromatic ring. These deshielding effects are explained by a consideration of the electronegativity of the substituents and the stereochemistry of the molecule. The chemical shifts and coupling constants are tabulated.

The 1975 publications reporting organic and spark source mass spectrometric studies on environmental samples were compiled. Emphasis was placed on pollutants identified rather than methods and techniques used, and reports that did not incorporate data obtained by a technique's application were not included. The 272 reports cited vary from those reporting hundreds of identified pollutants to those describing the analysis of only one sample containing one or a few pollutants. The following sample types were not considered to be environmental samples: forensic samples, synthetic or 'standard' samples, and samples analyzed for drug residues.