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«Dissertation zur Erlangung des Grades “Doktor der Naturwissenschaften” Im Promotionsfach Geowissenschaften Am Fachbereich Chemie, Pharmazie und ...»

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Speciation of Metals in Agricultural Lime and

Contaminated Soil

Dissertation

zur Erlangung des Grades

“Doktor der Naturwissenschaften”

Im Promotionsfach Geowissenschaften

Am Fachbereich Chemie, Pharmazie und Geowissenschaften

der Johannes Gutenberg-Universität Mainz

Ka Hei Lui

Geboren in Hong Kong

Mainz, 2011

Dekan:

1. Berichterstatter:

2. Berichterstatter:

Tag der mündlichen Prüfung: 26.09.2011

A

Leader

Contents Contents…………………………………………………………………………………………………………………………………………….I List of tables…………………………………………………………………………………………………………………………………….VI List of figures………………………………………………………………………………………………………………………………….VIII List of abbreviations………………………………………………………………………………………………………………………….XI Zusammenfassung………………………………………………………………………………………………………………………….XIII Abstract…………………………………………………………………………………………………………………………………………XVII 1.0) Introduction…………………………………………………………………………………………………………………………………1 1.1.1) Introduction of arsenic…….……………………………………………………………………………………………1 1.1.2) Arsenic speciation and occurrences in natural environment………………………………….………3 1.1.3) Arsenic in minerals……………………………………………………………………………………………………..…6 1.1.4) Toxicity and mobility of arsenic..………………………………………………………………………………..…8 1.2.1) Introduction of copper………………………………………………………………………………………..………11 1.2.2) Copper concentrations in unpolluted soils………………………………………………………………....14 1.2.3) Copper concentrations in polluted soils………………………………………………………….…………..16 1.2.4) Copper in plant, micro-organisms, animal and the relevant toxicity……………….……………18 1.2.5) Existing guidelines of copper in soils and criteria in various media………………………………26 1.2.6) Copper speciation in soils………………………………………………………………………………..………….30 1.2.6.1) Properties of copper in soils………………………………………………………………..……….30 1.2.6.2) Importance of copper speciation in soils………………………………………………………33

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1.2.7) Introduction of thallium………………………………………………………………………………………………………….36 1.2.7.1) Occurrence and properties of thallium…………………………………………………………………..…38 1.2.7.2) Thallium exposure in vicinity of cement factories and safety regulations worldwide..40 2.0) Aim…………………………………………………………………………………………………………………………………………….42 2.1) Aim of arsenic project…………………………………………………………………………………….………………42 2.2) Aim of copper project………………………………………………………………………………………..…………..42 2.3) Aim of thallium project………………………………………………………………………………………………….42 3.0) Method………………………………………………………………………………………………………………………………………43 3.1) Sequential extraction technique…………………………………………………………………………………….43 3.2) Atomic absorption spectroscopy………………………………………………….…………………………………48 3.3) Flame atomic absorption spectroscopy (F-AAS)….………………………………………………………….50 3.4) Hydride generation atomic absorption spectroscopy (HG-AAS)..…………………………………….53 3.5) Nonlinearity in analytical calibration graphs…………………………………………………………………..58 3.6) X-ray fluorescence analysis (XRF)…………………………………………………………………….…………….59 3.7) Inductively coupled plasma mass spectrometry (ICP-MS)……………………………………………….62

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4.0) Materials and methods………………………………………………………………………………………………………………66 4.1) Site description, sample collection and morphology of arsenic and copper……….……………66 4.2) Instrumentation of arsenic…..…………………………………………………………………………….………….67 4.3) Sequential extraction procedure of arsenic…………………………………………………………………….68 4.4) Sample preparation for arsenic measurement in HG-AAS………………………………………………70 4.5) Instrumentation of copper………………………………………………………………………………….………….72 4.6) Sequential extraction procedure of copper………………………………………………………….…………72 4.7) Site description and extraction procedure of thallium……………………………………………………74 5.0) Results and discussions………………………………………………………………………………………………………………81 5.1) Matrix effect of arsenic………………………………………………………………………………………………….81 5.2) The sequential extraction of arsenic………………………………………………………………………………84 5.3) The sequential extraction of copper…………………………………………………………………….………..88 5.4) Thallium concentration profiles of top and sub soils at sampling location 1……………………92 5.5) Thallium concentration profiles of top and sub soils at sampling location 2……………….…105 6.0) Conclusions……………………………………………………………………………………………………………………………...113 6.1) Arsenic………………………………………………………………………………………………………………………..113 6.2) Copper………………………………………………………………………………………………………….…………….114 6.3) Thallium……………………………………………………………………………………………………………………….115 7.0) Acknowledgements…………………………………………………………………………………………………………………116

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8.0) References………………………………………………………………………………………………………………………………117 8.1) Arsenic……………………………………………………………………………………………………………..…………117 8.2) Copper…………………………………………………………………………………………………………………………126 8.3) Thallium……………………………………………………………………………………………………………………….137 9.0) Appendix…………………………………………………………………………………………………………………………………142 9.1) Appendix A………………………………………………………………………………………………………………….142 9.1.1) Arsenic (As)………………………………………………………………………………………….………142 9.1.2) Iron (Fe) in arsenic measurement…..……………………………………………………..………162 9.1.3) Manganese (Mn) in arsenic measurement……….……………………………………..…….176 9.1.4) XRF……………………………………………………………………………………………………………….190 9.1.5) Standard addition of samples with masking agent………………………………………..196 9.1.6) Copper (Cu)…………………………………………………………………………………………………..202 9.1.7) Iron (Fe) in copper measurement………………………………………………………………….205 9.1.8) Manganese (Mn) in copper measurement…………………………………………………….207 9.1.9) Calcium (Ca) in copper measurement……………………………………………….…………..209 9.1.10) Copper sequential extraction bar chart of six sub-samples………………………….212 9.1.11) Copper with sodium acetate/acetic acid in first extraction step……………….…216 9.1.12) Thallium sub-sample concentrations measured by ICP-MS……………….………..217 9.1.13) Thallium concentrations in minerals and soils…………………………………………..…218 9.1.14) Thallium sub-sampling points concentrations across the sample depth…….…219

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9.2) Appendix B…………………………………………………………………………………………………………………..225 9.2.1) As (standard addition graph plot)………………………………………………………………….225 9.2.2) As (standard addition graph plot with 1% cysteine)………………………………………245 9.2.3) As (standard addition graph plot with 1% cysteine) (average of 3 samples)…..255 9.3) Appendix C……………………………………………………………………………………………………………….….260 9.3.1) Instrumentation……………………………………………………………………………………………260 10.0) Curriculum vitae (CV)….………………………………………………………………………………………….….266

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List of tables Table (1) Table shows some observed As concentrations in different soils…………………4 Table (2) Table shows major As minerals in nature…………………………………………6 Table (3) Table shows worldwide emission of copper from natural sources…………...….11 Table (4) Table shows copper concentrations in igneous and sedimentary rocks (modified Cannon et al. 1978)……………………………………………………………....12 Table (5) Table shows typical copper intake values for the general Canadian population (CCME 1997)…………………………………………………………………….24 Table (6) Table shows environmental and human health guidelines of copper (CCME 1997)……………………………………………………………………………..28 Table (7) Table shows key factors affecting cation exchange capacity (CEC)…………….31 Table (8) Table shows general characteristics of sequential extraction fractions……….…35 Table (9) Table shows different phases that main element compounds can resident………44 Table (10) Table shows association between extractants and different soil solid phases...…45 Table (11) Table shows trace elements in different soil phases……………………..………47 Table (12) Table shows components of hydride generation atomic absorption (HGAAS) system…………………………………………………………………………....54 Table (13) Table shows sequential extraction procedure for Arsenic-bearing solid phases…68 Table (14) Table shows sequential extraction procedure for Copper-bearing solid phases…72 Table shows sampling location of the collected soils at location 1…………...…76 Table (15) Table shows sampling location of the collected soils at location 2…………...…78 Table (16)

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Table (17) Table shows average contents of As, Fe and Mn in the sequential extraction scheme……………………………………………………………………..……..84 Table (18) Table shows average contents of Cu, Fe and Mn in the sequential extraction scheme……………………………………………………………………………88 Table (19) Table shows soil thallium (Tl) concentrations extracted by ammonium nitrate and aqua regia total acid digestion at location 1.......... ……………………………....94 Table (20) Table shows soil thallium (Tl) concentrations extracted by ammonium nitrate and aqua regia total acid digestion at location 2.......... ……………………………..105

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