Optimization of digestion methods for sewage sludge using the Plackett-Burman saturated design

The Plackett-Burman saturated factorial design was used to select optimized dissolution conditions for sewage sludge samples. Three different digestion methods were applied: i) microwave oven digestion in a domestic oven with Parr-type reactors; ii) microwave oven digestion with controlled-pressure reactors; iii) pressure bomb reactor heated on a hot plate. The three methods were validated by statistically comparing the metal contents found with the certified ones of the sewage sludge sample (BCR 145R). No significant differences were obtained and the RSD values were lower than 3% in all cases. The metals were determined by flame-AAS. The variables studied were the following: microwave power; digestion time; predigestion; volume of hydrochloric acid; volume of hydrofluoric acid; volume of nitric acid. The operative advantages offered by microwave digestion with controlled-pressure reactors were also considered. Received: 23 July 1997 / Revised: 31 October 1997 / Accepted: 5 November 1997     

Comparison between Total Determination and Extractable Heavy Metals from River Sediments using Conventional and Microwave Accelerated Leaching Tests

Abstract

In the present study the concentration of heavy metals (Cu, Cr, Ni, Pb and Zn) in sediments collected from different sampling stations of the Leça river (Portugal) was determined, using Flame Atomic Absorption Spectrometry. In order to estimate the potential mobility of metals in these samples, the results of the total digestion were compared with those obtained by single extractions using EDTA and acetic acid as extractant solutions; in all samples studied, Cu and Zn were found to be the most mobile elements; Ni and Pb showed a smaller mobility in presence of either acidic medium and complexing ligands; Cr was found the least mobilizable element, given that the low extractability obtained with the two extractants tested in this work. In the single extraction tests, microwave energy was also employed to replace the conventional treatment and only in the case of the EDTA the results obtained were similar to those of the conventional procedure (recoveries between 90.16 and 98.76%); the precision (RSD, n=3) of the proposed microwave procedure for EDTA extractions was comparable to those of the conventional method with values always lower than 8% for all metals.     

Comparison between conventional and ultrasound accelerated Tessier sequential extraction schemes for metal fractionation in sewage sludge

Chemical sequential extraction for metal fractionation in sewage sludge using the Tessier method has been accelerated by ultrasound. The two sequential extraction schemes (conventional and ultrasound accelerated) were compared in terms of extraction efficiency, precision, treatment time and partitioning patterns of metals. Extractable contents of Cu, Cr, Ni, Pb and Zn were measured by flame atomic absorption spectrometry, and the analytical results obtained by the two procedures were statistically compared (P = 0.95). No significant differences were found in the two first fractions (i.e. exchangeable and carbonate-bound), however, in the third and fourth extracts (i.e. Fe-Mn oxides-bound and organic matter-bound) the extraction capability of the two methods differed significantly. Received: 15 June 1998 / Revised: 10 November 1998 / Accepted: 11 November 1998     

Comparison between conventional and ultrasound accelerated Tessier sequential extraction schemes for metal fractionation in sewage sludge

Chemical sequential extraction for metal fractionation in sewage sludge using the Tessier method has been accelerated by ultrasound. The two sequential extraction schemes (conventional and ultrasound accelerated) were compared in terms of extraction efficiency, precision, treatment time and partitioning patterns of metals. Extractable contents of Cu, Cr, Ni, Pb and Zn were measured by flame atomic absorption spectrometry, and the analytical results obtained by the two procedures were statistically compared (P = 0.95). No significant differences were found in the two first fractions (i.e. exchangeable and carbonate-bound), however, in the third and fourth extracts (i.e. Fe-Mn oxides-bound and organic matter-bound) the extraction capability of the two methods differed significantly. Received: 15 June 1998 / Revised: 10 November 1998 / Accepted: 11 November 1998     

Preconcentration of lead, cadmium and zinc on silica gel loaded with diethyldithiocarbamate prior to their determination by flame-atomic absorption spectrometry

A silica gel sorbent loaded with sodium diethyldithiocarbamate has been developed for the preconcentration of lead, cadmium and zinc prior to their determination by flameatomic absorption spectrometry (FAAS). The sorption and desorption of the metal ions was studied under both static and dynamic conditions. The metal ions were quantitatively retained on the silica gel sorbent based on an equilibrium time of less than 1 min. In case of the batch method, the effects of pH, shaking time, amount of sorbent, and desorption time were investigated. Among the desorption agents studied, only EDTA in ammonium chloride/ammonia buffer yielded quantitative recoveries. Freundlich's sorption isotherms determined for each metal show that sufficient sorption ability is obtained. The column method allows the preconcentration of metal ions from large sample volumes (e.g. 200 mL) using a flow rate of 5 mL min^–1. The influence of foreign ions present in natural waters and saline solutions was examined. The reproducibility of the total analytical method, expressed as relative standard deviation (RSD) is 1.8, 0.5 and 0.6%, for lead, cadmium and zinc, respectively.     

Optimization of digestion methods for sewage sludge using the Plackett-Burman saturated design

The Plackett-Burman saturated factorial design was used to select optimized dissolution conditions for sewage sludge samples. Three different digestion methods were applied: i) microwave oven digestion in a domestic oven with Parr-type reactors; ii) microwave oven digestion with controlled-pressure reactors; iii) pressure bomb reactor heated on a hot plate. The three methods were validated by statistically comparing the metal contents found with the certified ones of the sewage sludge sample (BCR 145R). No significant differences were obtained and the RSD values were lower than 3% in all cases. The metals were determined by flame-AAS. The variables studied were the following: microwave power; digestion time; predigestion; volume of hydrochloric acid; volume of hydrofluoric acid; volume of nitric acid. The operative advantages offered by microwave digestion with controlled-pressure reactors were also considered. Received: 23 July 1997 / Revised: 31 October 1997 / Accepted: 5 November 1997     

Speeding up of a three-stage sequential extraction method for metal speciation using focused ultrasound

The three-stage sequential extraction procedure, proposed by the European Community Bureau of Reference (BCR), has been applied for speciation of copper, chromium, nickel, lead and zinc in a sludge sample collected from an urban wastewater treatment plant. The conventional BCR sequential extraction method has been modified, in each stage, applying ultrasonic energy by means of a probe (handling at an adequate sonication power and time) in order to shorten the required operation time. Extractable metal contents obtained by both the conventional and the accelerated ultrasonic extraction method, were measured by Flame-Atomic Absorption Spectrometry. Results obtained in each fraction by both methods were statistically compared (P=0.95) for all the studied elements and no significant differences were found except for chromium and zinc in the third fraction (oxidisable). For all metals the extraction percentage was>95%. The proposed accelerated sequential extraction method could be a valid alternative to the conventional shaking with a much shorter operating time.