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Esta pesquisa teve o objetivo de avaliar a eficiência de uma zona alagadiça (wertland) que ocorre nas dependências de uma usina situada em Santo Amaro da Purificação, Bahia, como medida de controle da contaminação proveniente de um barramento de escória contaminada por metais pesados. Inicialmente, foi proposto um levantamento anual com amostragens semanais das águas pluviais e superficiais da zona alagadiça, com o intuito de avaliar a eficiência da zona alagadiça, por meio do levantamento das concentrações dos metais oriundos dos processos de lixiviação e/ou solubilização da escória nos seus pontos de entrada e saída do sistema alagado e, concentrações e potencial disponibilidade dos metais retidos nos sedimentos da zona alagadiça. Foram selecionados os seguintes parâmetros: para as águas pluviais o pH e o volume da chuva; para as águas superficiais as concentrações dos metais Chumbo (Pb), Cádmio (Cd), Zinco (Zn), Cobre (Cu), Alumínio (Al), Manganês (Mn), Ferro (Fe), Magnésio (Mg) e Cálcio (Ca) e os parâmetros de suporte pH, Eh, condutividade, Oxigênio Dissolvido (OD) e temperatura. Para o solo e sedimento da zona alagadiça as concentrações dos metais Pb, Cd, Zn e Cu e, determinação por análise por extração seqüencial do total removido pelo sistema nas suas diversas fases e a potencial disponibilidade dos metais pesados. Todavia, uma modificação da estratégia de pesquisa teve que ser feita em função de uma decisão judicial que determinou o recobrimento da escória e do ponto de entrada da zona alagadiça. Em função do ocorrido, a pesquisa foi dividida em três etapas considerando os levantamentos efetuados antes, durante e depois do recobrimento. Os dados levantados nos cinco meses antes do recobrimento mostraram que os metais cádmio, chumbo, cobre e zinco estão sendo retidos pela zona alagadiça e, que este sistema foi eficiência de 100% para os metais cobre e zinco, 82% para o chumbo e 73% para o cádmio. Os parâmetros de suporte que influenciam a remoção destes metais foram o pH, entre neutro a alcalino, e Eh, na faixa de oxidação das águas superficiais, além da alta capacidade de troca catiônica da montmorilonita presente no sedimento. Quanto ao potencial de disponibilidade dos metais, cádmio, chumbo e zinco apresentam valores elevados, enquanto o cobre encontra-se preferencialmente concentrado na fase residual. A segunda etapa do levantamento realizada durante o recobrimento da escória demonstrou que ocorreu pouca migração dos metais da zona alagadiça, embora a empresa não tenha obedecido as normas técnicas para o recobrimento da escória. Na terceira etapa foi realizado levantamento na saída da zona alagadiça e da drenagem próxima ao rio Subaé. As análises levantadas demonstraram a grande disponibilidade do cádmio no sistema alagado, este mecanismo foi acionado a partir da erosão do solo contaminado disposto sobre a escória e a grande solubilidade do cádmio. Desta forma pode-se conclui que as zonas alagadiças estão sendo eficientes na retenção dos metais. A redução de sua área é indesejável, pois tende a diminuir sua eficiência, como sistema de controle da poluição das águas superficiais, recomenda-se a construção de nova zona alagadiça a jusante da existem. / A lead ore smaller which operated from 1960 to 1993 in Santo Amaro da Purificação, Bahia State, disposed of 490,000 tons of slag in a landfill situated in the situated in the industrial site. Earthworks formed a man-made wetland downstream of the slag landfill, which acted as a metal retaining systems, thus preventing further water pollution. This research aimed at investigating the efficiency of this wetland as a water pollution control system. The research plan scheduled weekly samplings of rainfall, rainwater pH and water runoff in two points corresponding to the input and the output of the wetland for determination of metals concentration (Pb, Cd, Cu, Zn, Al, Mn, Fe, Mg, Ca), as well as water pH, Eh, conductivity, temperature and dissolved oxygen (OD). In addition, soil and sediment in the wetland were sampled and analyzed for Pb, Cd, Zn and Cu by sequential extraction methods. However, a Court ruling following a lawsuit for environmental damage led to the slag being covered by clayish soil weeks after sampling began. As a consequence, the point where waters entered the wetlands has been covered. Hence, sampling in this point has been discontinued and a new sampling point was established downstream of the wetland, at a point where its waters flow into a river. Results showed that before cover-up, Pb, Cd, Cu and Zn were being retained in the wetland at rates reaching 100% for Cu and Zn, 82% for Pb and 73% for Cd. After cover-up, Cd was being released into the waters. Sequential extraction showed that only Cu is not available for leaching, since it is mostly concentrated in the insoluble phase. On the other hand, Pb, Cd and Zn are potentially available, thus could re-enter other media if wetland is disturbed. The wetland acts as an efficient device for retaining metals because of near neutral water pH, oxidizing water Eh, and the existence of montmorillonite clay in the sediments, which features high cationic exchange capacity. It is concluded that this involuntary wetland has been working, as an efficient system for water pollution control. The reduction in its size, due to the cover-up activities, is undesirable. Hence, a new constructed wetland is proposed downstream of the existing one. Then, we can end that the wetland of Plumbum this being efficient in the control of the metals, from when interferences anthropogenetic that maximize the capacity of support of this system don’t happen.

Heavy metal ions, such as cadmium and lead, should be removed from wastewaters to prevent bioaccumulation. Among many other separation processes, one of the alternatives is ion exchange involving a low cost packing material, clinoptilolite. Clinoptilolite is a natural zeolite and contains exchangeable cations such as Na+, K+, Mg2+, and Ca2+ in its structure. Aim of this study is to determine binary and multicomponent ion exchange behaviors of sodium enriched form of G&ouml / rdes clinoptilolite for lead and cadmium ions. For this purpose, Pb+2 &ndash / Na+, Cd+2 &ndash / Na+ binary and Pb+2 &ndash / Cd+2 &ndash / Na+ ternary systems were investigated in column operations for concentrations between 0.005 to 0.02 N and flow rates between 5 to 20 mL/min at 25 &amp / #730 / C. For determination of optimum particle size, 5/6, 8/10, 14/18, 20/30, 35/60, and 70/140 ASTM E-11 standard mesh ranges were tested and the optimum particle size, under the experimental conditions was found as 35/60. Furthermore, although the clinoptilolite has a theoretical ion exchange capacity of 2.14 meq/g based on its aluminum content, under experimental conditions maximum exchange level was determined as 1.08 meq/g. For binary and ternary experiments, it is observed that the clinoptilolite has affinity for both Pb2+ and Cd2+ ions. However, clinoptilolite has greater affinity to Pb2+ than Cd2+ ion. Therefore, selectivity sequence was determined as Pb2+&gt / Cd2+&gt / Na+. Additionally, for column studies, flow rates less than 10 mL/min and influent concentrations up to 0.01 N, sodium enriched form of G&ouml / rdes clinoptilolite holds great potential to remove Pb2+ and Cd2+ ions from wastewaters.

In this thesis, a facile methodology for the synthesis of CdS and PbS particles using novel thiobisphthalimide (D1) and dithiobisphthalimide (D2) organic sulfur precursors is proposed. A slightly different approach was followed for the synthesis of CuS particles. The effect on the size and morphology of the particles of a variety of reaction parameters such as the nature of sulfur precursor, the reducing agent concentration, the metal-to-sulfur ratio and the reaction temperature was investigated. The phase and composition identifications of the CdS and PbS particles were done by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) techniques. The transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques were employed to determine the morphologies of the particles. The optical properties of the CdS, PbS and CuS particles were examined by UV-Vis and fluorescence spectroscopy techniques. The phase identification results showed that pure cubic CdS and PbS, and hexagonal CuS particles were successfully synthesized with both D1 and D2 precursors. The synthesized CdS and PbS particles possess various morphologies depending on the precursor type and the reaction parameters mentioned previously. Control of the size of the PbS particles in one dimension in a quantum confinement regime was possible, whereas the CdS particles exhibited faster growth and 3D morphologies. The CuS particles, on the other hand, were produced with high monodispersity in a surfactantless environment.

Esta pesquisa teve o objetivo de avaliar a eficiência de uma zona alagadiça (wertland) que ocorre nas dependências de uma usina situada em Santo Amaro da Purificação, Bahia, como medida de controle da contaminação proveniente de um barramento de escória contaminada por metais pesados. Inicialmente, foi proposto um levantamento anual com amostragens semanais das águas pluviais e superficiais da zona alagadiça, com o intuito de avaliar a eficiência da zona alagadiça, por meio do levantamento das concentrações dos metais oriundos dos processos de lixiviação e/ou solubilização da escória nos seus pontos de entrada e saída do sistema alagado e, concentrações e potencial disponibilidade dos metais retidos nos sedimentos da zona alagadiça. Foram selecionados os seguintes parâmetros: para as águas pluviais o pH e o volume da chuva; para as águas superficiais as concentrações dos metais Chumbo (Pb), Cádmio (Cd), Zinco (Zn), Cobre (Cu), Alumínio (Al), Manganês (Mn), Ferro (Fe), Magnésio (Mg) e Cálcio (Ca) e os parâmetros de suporte pH, Eh, condutividade, Oxigênio Dissolvido (OD) e temperatura. Para o solo e sedimento da zona alagadiça as concentrações dos metais Pb, Cd, Zn e Cu e, determinação por análise por extração seqüencial do total removido pelo sistema nas suas diversas fases e a potencial disponibilidade dos metais pesados. Todavia, uma modificação da estratégia de pesquisa teve que ser feita em função de uma decisão judicial que determinou o recobrimento da escória e do ponto de entrada da zona alagadiça. Em função do ocorrido, a pesquisa foi dividida em três etapas considerando os levantamentos efetuados antes, durante e depois do recobrimento. Os dados levantados nos cinco meses antes do recobrimento mostraram que os metais cádmio, chumbo, cobre e zinco estão sendo retidos pela zona alagadiça e, que este sistema foi eficiência de 100% para os metais cobre e zinco, 82% para o chumbo e 73% para o cádmio. Os parâmetros de suporte que influenciam a remoção destes metais foram o pH, entre neutro a alcalino, e Eh, na faixa de oxidação das águas superficiais, além da alta capacidade de troca catiônica da montmorilonita presente no sedimento. Quanto ao potencial de disponibilidade dos metais, cádmio, chumbo e zinco apresentam valores elevados, enquanto o cobre encontra-se preferencialmente concentrado na fase residual. A segunda etapa do levantamento realizada durante o recobrimento da escória demonstrou que ocorreu pouca migração dos metais da zona alagadiça, embora a empresa não tenha obedecido as normas técnicas para o recobrimento da escória. Na terceira etapa foi realizado levantamento na saída da zona alagadiça e da drenagem próxima ao rio Subaé. As análises levantadas demonstraram a grande disponibilidade do cádmio no sistema alagado, este mecanismo foi acionado a partir da erosão do solo contaminado disposto sobre a escória e a grande solubilidade do cádmio. Desta forma pode-se conclui que as zonas alagadiças estão sendo eficientes na retenção dos metais. A redução de sua área é indesejável, pois tende a diminuir sua eficiência, como sistema de controle da poluição das águas superficiais, recomenda-se a construção de nova zona alagadiça a jusante da existem. / A lead ore smaller which operated from 1960 to 1993 in Santo Amaro da Purificação, Bahia State, disposed of 490,000 tons of slag in a landfill situated in the situated in the industrial site. Earthworks formed a man-made wetland downstream of the slag landfill, which acted as a metal retaining systems, thus preventing further water pollution. This research aimed at investigating the efficiency of this wetland as a water pollution control system. The research plan scheduled weekly samplings of rainfall, rainwater pH and water runoff in two points corresponding to the input and the output of the wetland for determination of metals concentration (Pb, Cd, Cu, Zn, Al, Mn, Fe, Mg, Ca), as well as water pH, Eh, conductivity, temperature and dissolved oxygen (OD). In addition, soil and sediment in the wetland were sampled and analyzed for Pb, Cd, Zn and Cu by sequential extraction methods. However, a Court ruling following a lawsuit for environmental damage led to the slag being covered by clayish soil weeks after sampling began. As a consequence, the point where waters entered the wetlands has been covered. Hence, sampling in this point has been discontinued and a new sampling point was established downstream of the wetland, at a point where its waters flow into a river. Results showed that before cover-up, Pb, Cd, Cu and Zn were being retained in the wetland at rates reaching 100% for Cu and Zn, 82% for Pb and 73% for Cd. After cover-up, Cd was being released into the waters. Sequential extraction showed that only Cu is not available for leaching, since it is mostly concentrated in the insoluble phase. On the other hand, Pb, Cd and Zn are potentially available, thus could re-enter other media if wetland is disturbed. The wetland acts as an efficient device for retaining metals because of near neutral water pH, oxidizing water Eh, and the existence of montmorillonite clay in the sediments, which features high cationic exchange capacity. It is concluded that this involuntary wetland has been working, as an efficient system for water pollution control. The reduction in its size, due to the cover-up activities, is undesirable. Hence, a new constructed wetland is proposed downstream of the existing one. Then, we can end that the wetland of Plumbum this being efficient in the control of the metals, from when interferences anthropogenetic that maximize the capacity of support of this system don’t happen.

<p><strong>Apstrakt je obrađen tehnologijama za optičko prepoznavanje teksta (OCR).</strong></p><p>Razvojem novih tehnika, odnosno metoda potenciometrijske striping analize (PSA), značajno je povećana osetljivost određivanja osnovne modifikacije PSA sa kiseonikom kao oksidansom. Definisane su metode za određivanje olova i kadmijuma u standardnoj elektrohemijskoj ćeliji, tankoslojnoj protočnoj ćeliji i tubulamom protočnom sistemu.<br />Ostvarena je granica osetljivosti od 50 ng/dm³, uz reproduktivnost od oko 15%, izraženom kao koeficijent varijacije. Tačnost novih tehnika je potvrđena dobrim slaganjem rezultata analiza uzoraka pijaće vode sa rezultatima uporednih analiza izvedenih primenom osnovne modifikacije PSA, kao referentne metode.<br />Sve analize su izvedene uz primenu kompjuterizovanog striping analizatora domaće konstrukcije i proizvodnje (Tehnolo&scaron;ki fakultet, Novi Sad &mdash; &rdquo;Elektrouniverzal&rdquo;, Leskovac).</p> / <p><strong>Abstract was processed by technology for Optical character recognition (OCR).</strong></p><p>А new and high sensitive techniques (methods) of the potentiometric stripping analysis аге developed. Methods for lead and cadmium determination in conventional electrochemical cell, are defined. The detection limit of 50 ng/dm3 is obtanied, by the reproducibility about 15% (CV). The ассuracу of the new techniques is confirmed by good agreements of the results of the tap water analyses, with the results obtanied from the same samples analysed by conventional PSA, as reference method. All analyses аге carried by a computerized stripping analyzer constructed and made by the Faculty of Technology, Novi Sad and &rdquo;Elektrouniverzal&rdquo;, Leskovac.</p>

Tato dizertační práce zkoumá vývoj techniky difúzního gradientu v tenkém filmu (DGT) pro stanovení rtuti (Hg) a dalších stopových kovů a dále rozšířené možnosti použití této techniky. Technika DGT je v této práci vyvinuta pro stanovení Hg a dalších stopových prvků v různých kapalných médiích. Dvě rozdílná sorpční média specifická pro rtuť byla testována pro použití v technice DGT – Purolite S924 a cysteinem modifikovaná aminopropyl silika (CAPS). Purolite S924 je komerčně dostupný chelatační iontoměnič, CAPS byla připravena v laboratorních podmínkách imobilizací cysteinu na 3-aminopropyl funkcionalizovanou siliku pomocí glutaraladehydu. Obě testovaná sorpční média ukázala slibný aplikační potenciál pro užití v technice DGT díky funkčnosti v roztocích o širokém rozsahu pH i iontové síly. Funkčnost DGT s novými sorpčními médii byla porovnána s technikami DGT s běžně používanými sorbenty Chelex-100 a 3-merkaptopropylfunkcionalizovanou silikou. Hlavní výhodou sorpčních médií Purolite S924 a CAPS je schopnost současného stanovení Hg a dalších stopových kovů (Cd, Pb, Co, Ni, Cu). Vzhledem k odlišným požadavkům na sorpční média používaná v technice DGT nebylo dosud současné kvantitativní stanovení Hg a dalších stopových kovů možné. Doposud byly zapotřebí dvě samostatné techniky DGT – jedna pro Hg a druhá pro další stopové kovy, což zvyšuje množství vzorků pro analýzu a množství použitého spotřebního materiálu. Technika DGT s CAPS byla použita pro stanovení koncentrací kovů v námořních přístavech v Oostende a Zeebrugge na belgickém pobřeží Severního moře. Přestože byla technika DGT původně představena pro použití v analytické chemii životního prostředí, byla v této práci zkoumáno i použití této techniky v analýze potravin. V prostředí rybí omáčky byla ověřena funkčnost techniky DGT a stanoveny difúzní koeficienty Hg a dalších stopových prvků. Technika DGT byla následně použita pro stanovení koncentrace rtuti a dalších stopových kovů v různých komerčně dostupných vzorcích rybí omáčky. Výsledky nově navrhnutého analytického postupu s použitím techniky DGT byly porovnány s výsledky přímé analýzy atomovou absorpční spektroskopií s termální dekompozicí a amalgamací zlatem (TD-AAS) a po mikrovlnném rozkladu vzorků omáčky také s výsledky sektorové hmotnostní spektrometrie s indukčně vázanou plazmou (SF-ICP-MS). Díky předkoncentrační schopnosti techniky DGT byly dosaženy nižší detekční limity ve srovnání s TD-AAS nebo SF-ICP-MS. Technika DGT díky schopnosti oddělení analytů z komplexní matrice rybí omáčky rovněž snížila opotřebení a koroze kovových částí použitých instrumentálních technik.

Hair is an excellent matrix for monitoring trace elements and minerals in the body. To long-term changes in concentration of elements in the body are reflected in their value in her hair, so the assessment of the organism from the mineral analysis of hair is a very suitable method. This method is widely used in toxicological testing and forensics. This work deals with the analysis of Mg, K, Fe, Zn, Mn, Se, As, Cd and Pb in 100 samples by ICP-MS. It is a male hair samples with the age range 19 – 74 years. Analysis of hair revealed that concentrations of individual elements are moving in a narrow range of values. Values of older age category are in some case significantly deflective.

The newly planned lead recycling zone in Dong Mai village has been operating with primary treatment systems using lime to neutralize acid in wastewater is a good sign for the local environment, yet the real problem that needs further attention and proper solutions is the accumulation of heavy metals typically lead (Pb) and cadmium (Cd) in agricultural land near the old Pb recycling area. In this context, 27 soil samples were collected and analyzed by AAS method to assess the situation and the quality of the agricultural soil. The results showed that the levels of Cd in the soil were still in acceptable level according to National Regulation. However, the lead contents in all of the soil samples exceeded National Regulation. The level of Pb pollution in soil was inversely proportional to the distance with old lead melting zone. The lead content in the soil sample collected at the distance of 50 m radius to the old melting zone reached 7070 ppm, which was 100 times higher than the allowable value of National Regulation. / Khu tái chế chì mới tại thôn Đông Mai đã được quy hoạch và đi vào hoạt động cùng hệ thống xử lý sơ bộ với vôi bột là một tín hiệu đáng mừng cho môi trường nơi đây, nhưng vấn đề cần quan tâm và giải quyết triệt để là sự tích lũy một lượng lớn kim loại nặng điển hình là chì (Pb) và cađimi (Cd) trong đất nông nghiệp gần những khu tái chế chì cũ. 27 mẫu đất đã được thu thập và phân tích bằng phương pháp AAS để đánh giá tình trạng, chất lượng đất nông nghiệp tại đây. Kết quả cho thấy hàm lượng Cd trong đất vẫn trong mức độ cho phép theo Quy chuẩn quốc gia. Tuy nhiên, 100% các mẫu đất đều có hàm lượng chì vượt quá mức cho phép theo Quy chuẩn quốc gia. Mức độ ô nhiễm Pb trong đất tỷ lệ nghịch với khoảng cách tới khu lò nấu chì cũ. Mẫu đất cách 50 m so với khu vực lò cũ có hàm lượng chì lên tới 7070 ppm, gấp hơn 100 lần so với Quy chuẩn quốc gia.

Two plant species including Polygonum hydropiper L. and Hymenachne acutigluma (Steud.) Gilliland were investigated in their resistance to lead (Pb) and cadmium (Cd) pollution in the soil. Lead-contaminated soil samples were collected from the lead recycling village Dong Mai, Chi Dao commune, Van Lam district, Hung Yen province, Vietnam that had Pb level up to 192,185 mg.kg-1, dry weight (DW). Cadmium-contaminated soil samples were due to supplement of CdCl2.21/2H2O to alluvial soil. Results showed that both species were highly resistant to Pb, however P.hydropiper was better. Similarly, the Cd resistance was higher for P.hydropiper than for H.acutigluma. No morpho-abnormalities of P.hydropiper regarding the impact of lead were recorded, whereas for H.acutigluma, the young leaves had white colour after two months of planting in soil containing lead levels of 192,185 mg.kg-1. The response of both species with Cd in soils included yellowing leaves, withering branches and even dying after 5-15 days exposed to Cd. Lead contents accumulated in above-ground parts of both plants were up to 4,650 and 3,161 mg.kg-1, DW, corresponding to P.hydropiper and H.acutigluma. From the research results on lead resistance and accumulation of two plant species studied, it is suggested that the two species are lead hyperaccumulators can be used for phytoremediation technology to clean contaminated soil. / Hai loài thực vật gồm nghể răm Polygonum hydropiper L. và bấc nhọn Hymenachne acutigluma (Steud.) Gilliland được nghiên cứu về khả năng chống chịu ô nhiễm chì (Pb) và cadmi (Cd) trong đất. Mẫu đất ô nhiễm chì được thu từ làng nghề tái chế chì Đông Mai, xã Chỉ Đạo, huyện Văn Lâm, tỉnh Hưng Yên, Việt Nam có hàm lượng chì lên đến 192.185 mg.kg-1, tính theo trọng lượng khô (DW). Mẫu đất ô nhiễm Cd là do được bổ sung CdCl2.21/2H2O vào đất phù sa. Kết quả cho thấy cả hai loài đều có sức chống chịu chì rất cao, tuy nhiên nghể răm có khả năng tốt hơn. Tương tự như vậy, sức chống chịu Cd của nghể răm cũng cao hơn của bấc nhọn. Không có dấu hiệu bất thường nào của nghể răm đối với tác động của chì được ghi nhận, trong khi ở bấc nhọn thì lá non có màu trắng sau hai tháng trồng trên đất có hàm lượng chì 192.185 mg.kg-1. Phản ứng của cả hai loài thực vật với Cd trong đất gồm có hiện tượng vàng lá, héo ngọn và thậm chí chết sau 5-15 ngày phơi nhiễm với Cd. Hàm lượng chì được tích lũy cao trong phần trên mặt đất của cả hai loài thực vật lên tới 4.650 và 3.161 mg.kg-1, DW, tương ứng cho loài P.hydropiper và H.acutigluma. Từ kết quả nghiên cứu về khả năng chống chịu và tích lũy chì của hai loài thực vật nghiên cứu, có thể đề xuất đây là hai loài siêu tích lũy chì có thể sử dụng trong công nghệ làm sạch đất ô nhiễm.