Charles R. Nony

Carcinogens and Analogs: Trace Analysis of Thirteen Compounds in Admixture in Wastewater and Human Urine

A gas chromatographic method is described for determining traces of 13 carcinogens and related compounds (aromatic amines and estrogens) in admixture in wastewater and human urine. This method was developed for use in toxicological research for monitoring the safe disposal of wastewater and to signal any accidental exposure of personnel to hazardous test substances. Salient elements of the procedure are: extraction of phenolic and neutral residues from the acidified sample, liquid--liquid partitioning cleanup and separation of neutral from phenolic residues at pH 14 and 10.2, acid hydrolysis of the neutral component, subsequent alkalinization of the sample and extraction of the basic residues as the free amines, conversion of all residues to the corresponding pentafluoropropionyl (PFP) derivatives and quantification by electron-capture gas chromatography. Residues were detectable in wastewater and urine at the 0.1 and 1 ppb levels, respectively. Additional information is provided concerning partition values for all PFP derivatives in five solvent systems, structure verification of the derivatives by mass spectrometry and the adaption of this method to the monitoring of surfaces and air in potentially contaminated work areas.

Removal of trace levels of 2-acetylaminofluorene (2-AAF) from wastewater

An adsorption system is described for the removal of part per billion levels of the chemical carcinogen, 2-acetylaminofluorene (2-AAF), from industrial wastewater. The system consists primarily of filters and activated carbon and non-ionic polymeric adsorbents arranged in tandem. It is highly efficient, operates at low cost, and requires minimal attention. The chemical monitoring of the raw and/or cleaned-up wastewater is based on a highly sensitive and specific spectrophotofluorometric method that allows acceptance or rejection of samples at the 0.2 part per billion level. The system is presented as a model for evaluating the removal of traces of organic chemicals from wastewater prior to recycling or discharging it into the environment. Results of laboratory evaluations of several other approaches to the purification of 2-AAF-containing wastewater are also presented.

Characterization, purification, and analysis of solvent yellow 33 and solvent green 3 dyes.

Thin-layer chromatography and high-performance liquid chromatography (HPLC) with linear photodiode array detection (LPDA) were used to separate impurities from two commercial dyes. Gravity flow liquid chromatography was used to purify reference standards of the dyes. Normal phase HPLC with LPDA detection was used to determine purities of submitted samples by comparing responses to those of the reference standards. Electron impact mass spectrometry and nuclear magnetic resonance were utilized to confirm structures of the dyes and their impurities.