RESUMEN
Golden, Sunrise Solo and Tainung cultivars of papaya were found to release CS2 when submitted to experimental conditions of dithiocarbamate residue analysis. Three common analytical methods were used to quantitate CS2; one spectrophotometric method and two chromatographic methods. All three methods gave positive CS2 results for all three papaya varieties. Other endogenous compounds present in isooctane extracts of papaya fractions detected via gas chromatography (GC/ITD) using electron ionization (EI) were: carbonyl sulfide, dimethyl sulfide, carbon disulfide, 2-methylthiophene, 3-methylthiophene, 2-ethylthiophene, 3-ethylthiophene, benzylisothiocyanate, benzylthiocyanate and benzonitrile. Control samples were obtained from papaya plantations cultivated in experimental areas, in which no treatment with fungicides of the dithiocarbamate group was applied. Endogenous CS2 levels were compared with true dithiocarbamate residues measured in papaya samples from the field trials following applications of the mancozeb fungicide. Three days after application, true dithiocarbamate residues, measured by the procedure with isooctane partitioning and GC-ITD, were at the average level of 2 mg kg(-1).
Asunto(s)
Disulfuro de Carbono/química , Carica/química , Cromatografía de Gases/métodos , Fungicidas Industriales/análisisRESUMEN
A sensitive and robust analytical method for spectrophotometric determination of ethyl xanthate, CH(3)CH(2)OCS(2)(-) at trace concentrations in pulp solutions from froth flotation process is proposed. The analytical method is based on the decomposition of ethyl xanthate, EtX(-), with 2.0 mol L(-1) HCl generating ethanol and carbon disulfide, CS(2). A gas diffusion cell assures that only the volatile compounds diffuse through a PTFE membrane towards an acceptor stream of deionized water, thus avoiding the interferences of non-volatile compounds and suspended particles. The CS(2) is selectively detected by UV absorbance at 206 nm (epsilon=65,000 L mol(-1) cm(-1)). The measured absorbance is directly proportional to EtX(-) concentration present in the sample solutions. The Beer's law is obeyed in a 1x10(-6) to 2x10(-4) mol L(-1) concentration range of ethyl xanthate in the pulp with an excellent correlation coefficient (r=0.999) and a detection limit of 3.1x10(-7) mol L(-1), corresponding to 38 microg L(-1). At flow rates of 200 microL min(-1) of the donor stream and 100 microL min(-1) of the acceptor channel a sampling rate of 15 injections per hour could be achieved with RSD<2.3% (n=10, 300 microL injections of 1x10(-5) mol L(-1) EtX(-)). Two practical applications demonstrate the versatility of the FIA method: (i) evaluation the free EtX(-) concentration during a laboratory study of the EtX(-) adsorption capacity on pulverized sulfide ore (pyrite) and (ii) monitoring of EtX(-) at different stages (from starting load to washing effluents) of a flotation pilot plant processing a Cu-Zn sulfide ore.
Asunto(s)
Disulfuro de Carbono/análisis , Gases/química , Tionas/análisis , Disulfuro de Carbono/química , Difusión , Análisis de Inyección de Flujo/métodos , Espectrofotometría Ultravioleta/instrumentación , Espectrofotometría Ultravioleta/métodosRESUMEN
The sample decomposition of the carbon disulfide evolution method for the determination of dithiocarbamate residues was carried out in a closed vial in the presence of hexane. The evolved carbon disulfide was extracted by the organic solvent and injected in a flow system for its quantification as copper complex. The conditions for batch decomposition, flow injection determination, and association of both were investigated with sodium diethyldithiocarbamate as model substance. An one-channel flow system was employed where the carrier stream was the ethanolic ethylenediamine/copper solution. The determination range was of 0. 01-1.26 microg of CS(2), with a relative standard deviation of 0.06% (n = 10), with a sample throughput of 45 samples/h. The association of the batch decomposition with the flow system was carried out with the fungicide mancozeb and was applied to the analysis of its residue in potato, lettuce, cucumber, and green bean crops. The approach allowed the analysis of 11 samples in triplicate in 2 h, with recoveries between 85% and 92% and relative standard deviation about 2%.