O gesso agrícola (CaSO4.2H2O) destaca-se como fonte eficiente de cálcio e enxofre e na redução da saturação de alumínio no solo. O 34S como traçador isotópico pode elucidar aspectos importantes no ciclo do enxofre. Para tanto o Ca34SO4.2H2O foi obtido por reação química entre o Ca(OH)2 e solução de H2(34)SO4, realizada sob agitação lenta. O ácido foi produzido por cromatografia de troca iônica, utilizando resina catiônica Dowex 50WX8 e solução eluente de Na2(34)SO4. Após a precipitação foi separado o precipitado e realizada a secagem em estufa ventilada à temperatura de 60ºC. Nos testes, a partir de 2,2 L de H2SO4 0,2 mol L-1 e 33,6 g de Ca(OH)2, foram produzidos em média 73,7 ± 0,6 g de Ca34SO4.2H2O representando um rendimento médio de 94,6 ± 0,8%, com pureza de 98%. A partir do Ca34SO4.2H2O na presença de NaPO3, em linha de alto vácuo, obteve-se o gás 34SO2 utilizado para a determinação isotópica do S no espectrômetro de massas ATLAS-MAT modelo CH-4.

Agricultural gypsum (CaSO4.2H2O) stands out as an effective source of calcium and sulfur, and to control aluminum saturation in the soil. Labeled as 34S it can elucidate important aspects of the sulfur cycle. Ca34SO4.2H2O was obtained by chemical reaction between Ca(OH)2 and H2(34)SO4, performed under slow agitation. The acid was produced by ion exchange chromatography using the Dowex 50WX8 cation exchange resin and a Na2(34)SO4 eluting solution. After precipitation, the precipitate was separated and dried in a ventilated oven at 60ºC. From 2.2 L H2SO4 0.2 mol L-1 and 33.6 g Ca(OH)2, 73.7 ± 0.6 g Ca34SO4.2H2O were produced on average in the tests, representing a mean yield of 94.6 ± 0.8%, with 98% purity. The 34SO2 gas was obtained from Ca34SO4.2H2O in the presence of NaPO3 in a high vacuum line and was used for the isotopic determination of S in an ATLAS-MAT model CH-4 mass spectrometer.

A system for disposal and recovery of the main effluents and chemical waist from isotope separation plants and enriched compounds-15N and 34S production has been carried out at the Stable Isotope Laboratory (LIE) of the CENA/USP. Around four hundred thousand liters of effluents has been recovered yearly. Among the recovered chemical wastes, the more relevant are: ammonia; brome; ammonium and sodium sulfate; sodium hydroxide; sulfur dioxide; and hydrochloric acid. Chemical wastes containg recoverable heavy metals (Ag, Cr and Cu) and solvents (methanol, ethanol and acetone) are processed and recovered. Gaseous emissions, mainly H2S are used for recovery of heavy metals solutions. The minimization of the residues waters, as well the reduction of electric energy consume was established using a water deionization system. A cost/effect balance of the process is reported.

A simple procedure for recovering Ag, generated as residual solutions, from three different analytical methods, is presented. Based on the rate of the total Ag mass recovered, to the initial one in the initial residual solutions, efficiency as high as 97,9 ± 2,9% was obtained in the process. The purity of Ag, as Ag2O, was verified by employing this reagent in the determination of S in plant tissue. This leads to the generation of a solid metallic Ag as waste. In this situation, an 88,7 ± 0,6% Ag recovery was acquired, when a HNO3 solution was employed as solvent.

No Brasil, a aquamônia vem sendo utilizada como fertilizante nitrogenado, especialmente na cultura de cana de açúcar. Entre os fatores que influenciam a produtividade das culturas agrícolas, está a eficiência de utilização de fertilizantes nitrogenados (EUF), sendo a técnica isotópica com 15N empregada em investigações dessa natureza. Este trabalho procurou estabelecer métodos de produção de amônia anidra (15NH3) e aquosa (15NH3aq), enriquecidas em 15N, em um único sistema, a partir do sulfato de amônio previamente enriquecido no mesmo isótopo. O processo de produção de 15NH3 e 15NH3aq foi avaliado em função dos fatores: temperatura (60, 70 e 75ºC) e tempo de reação (90, 120, 150, 165, 210 e 255 minutos), fluxo de gás de arraste (140; 180 e 220 mL min-1 de N2) e massa de sulfato de amônio utilizada na reação (40; 72,6; 106; 132 e 200 g). As melhores condições com relação à produção de 15NH3 e 15NH3aq foram proporcionadas pela temperatura de 70ºC, fluxo de gás de arraste de 180 mL min-1 de N2 e tempo de reação de 210 minutos. O teor de N na 15NH3aq variou de 15 a 20% (m/m) e o sistema apresentou capacidade de produção de aproximadamente 280 mL de 15NH3aq com concentração de 15% (m/m) por batelada. O processo global apresentou rendimento na faixa de 91 a 99%, em função da massa de (15NH4)2SO4 utilizada, sendo as perdas de 15N desprezíveis.

In Brazil aqua ammonia is an important fertilizer for soil fertilization of the sugarcane crop. The efficiency of the use of nitrogen fertilizers (EUF) by crops is a factor that has influence on agricultural productivity. The isotope technique of 15N labeled fertilizer is used for EUF determinations. In this paper the methods for production, in a same system, of anhydrous ammonia (15NH3) and aqua ammonia (15NH3aq), both enriched in the heavy stable isotope of nitrogen, using ammonium sulfate (AS) labeled with 15N [(15NH4)2SO4 ] as raw material, are presented. The parameters evaluated in the processes were: temperature (60, 70 e 75°C); reaction time (90, 120, 150, 165, 210 e 255 minutes), flow of N2 carrier gas (140, 180 e 220 mL min-1) and mass of AS (40, 72.6, 106, 132 e 200 g). The best conditions related to the production of the 15NH3 e 15NH3aq, were obtained at a temperature of 70°C, flow of N2 carrier gas of 180 mL min-1 and a reaction time of 210 minutes. The N concentration of the 15NH3aq was between 15-20% (w/w), with the 15NH3aq production of 280 mL with concentrations around 15% (w/w) for each batch. The overall yield of the process ranged from 91 to 99% and was directly related to the mass of AS. The unrecovered 15NH3 was very low.

Isotopic and elemental analysis of N, C and S in liquid and solid samples has been simplified with the advent of automated systems. The simplest method of automation for this kind of analysis involves an elemental analyzer interfaced directly to the ion source of an IRMS (Isotope Ratio Mass Spectrometry). In the analyzer reduction system, an expressive amount of oxidized copper is generated as solid residue. This material is normally imported and the price is very high. A methodology was proposed for the recovery of metallic copper in order to recycle this reagent in the reduction system of a GC-IRMS, using the hydrogen gas in the vacuum line. Results show that it is possible to obtain a recycle of about 95 % of the initial metallic copper used in the reduction system.