應用雷射剝蝕感應耦合電漿質譜儀偵測環境中水體及空氣懸浮微粒樣品

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研究生：	杜重未 Do, Trong Mui
論文名稱：	應用雷射剝蝕感應耦合電漿質譜儀偵測環境中水體及空氣懸浮微粒樣品 Laser ablation inductively coupled plasma mass spectrometry and its application in analysis of liquid and airborne particulate matter sample
指導教授：	王竹方
口試委員:	袁明程李振弘黃素珍李明禹
學位類別：	博士 Doctor
系所名稱：	原子科學院 - 生醫工程與環境科學系 Department of Biomedical Engineering and Environmental Sciences
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	100
中文關鍵詞：	雷射剝蝕感應耦合電漿質譜儀、空氣懸浮微粒、鹽水蜂炮、地表水、重金屬分析
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Laser ablation (LA) in analytical chemistry has grown rapidly over the past decade and is becoming a dominant technique for direct solid introduction into inductively coupled plasma mass spectrometry (ICP-MS) in analytical chemistry. The advantages of LA include direct characterization of solids, no chemical procedures for dissolution, reduced risk of contamination or sample loss, analysis of very small sample and determination of spatial distribution of elemental composition.
To exploit the possibilities of this technique in analysis of various types of environmental samples, in this study, we developed a dried-droplet method for laser ablation inductively coupled plasma mass spectrometry(LA-ICP-MS).The proposed method provides accurate and precise results when building calibration curves and determination of elements of interest in the liquid as well as airborne particulate matter samples. After placing just 1 L of a liquid standard solution onto the filter surface and then converting the solution into a very small, thin dry spot, the standard filter sample could be applied as an analytical subject for LA. To demonstrate the feasibility of this method, we used LA-ICP-MS to determine the levels of 13 elements ( Li, V, Mn, Co, Ni, Cu, Zn, As, Mo, Cd, Sb, Tl, and Pb) in five water samples and 16 elements (Na, Mg, Al, Si, K, Ca, V, Cr, Mn, Fe, Cu, Zn, As, Sr, Ba and Pb) in airborne particulate matter samples. The correlation coefficients obtained from the various calibration curves ranged from 0.9920 (205Tl) to 0.9998 (52V), sufficient to allow the determination of a wide range of elements in the samples. Quantitative elemental analysis using this LA-ICP-MS technique can be performed within a period short time. In comparison with the established sample introduction by nebulization, the developed method can bring several benefits: no matrix interference, no need for sample pretreatment (time-saving), and reduction of possibilities of sample contamination.

Table of Contents

Publications relevant to the scope of thesis                i
Abstract                                               ii
Acknowledgement                                         iii
Table of contents                                       iv
List of Table                                              vii
List of Figure                                             viii
List of abbreviations                                       ix
Chapter I.  Introduction                                1
I.1 General overview                                        1
I.2  Aims of study                                        3
I.3  The expected results that are needed to achieve in this study                                                         3
Chapter.  II  Literature review                                5
II.1. Metals in environment and their health effects         5
II.2. LA-ICP-MS systems                                        8
II.2.1 Interferences in ICP-MS                               10
II.2.2 Elemental fractionation                               11
II.2.3 Matrix modifier                                       12
II.3 Applications of LA-ICP-MS in analytical chemistry       14
II.4. Calibration strategies                               18
Chapter III. Material and methods                       22
III.1 Study approach                                       22
III.2 Apparatus                                               23
III.2.1 Laser ablation UP213 device                       23
III.2.2  ICP-MS 7500a system                               26
III.3 Reagent and materials                               28
III.4 Preparation of samples for LA-ICP-MS               28
III.4.1 Preparation of standards for LA-ICP-MS               28
III.4.2 Preparation of various Methylene Blue( MB) and NaCl concentrations                                               29
Chapter IV. Results and discussion                       31
IV.1 Selection and optimization of major operational parameters                                               31
IV.1.1 Laser energy level                               31
IV.1.2 Dwell time                                       32
IV.1.3 Defocus distance                                       33
IV.2 Sample analysis using LA-ICP-MS                       36
IV.3 Quality control of proposed method                       40
IV.3.1 External calibration                               40
IV.3.2 Standard addition calibration                       43
IV.4 Effects of MB and NaCl on signal intensity               45
IV.4.1 Effects of MB concentrations                       45
IV.4.2 Effects of NaCl on signal intensity               45
Chapter V. Applications                                       48
V.1 Determination of elements in water samples               48
V.1.1 Sample collection and analysis                       48
V.1.2 Results and discussion                               49
V.2 Investigation of metals present in the atmosphere before and after firework festival in Yanshui, Tainan, Taiwan       53
V.2.1 Aerosol sample collection and analysis               53
V.2.2 Results and discussion                               57
Chapter VI. Conclusion                                       72
References                                               74
Appendix                                               94




List of Tables
Table 4.1 Operating conditions for the LA-ICP-MS system.....................................................36
Table 4.2 Correlation coefficients (R2) and the lowest MDLs (ng mL−1) obtained using LA-ICP-MS and ICP-MS.....................................................41
Table 4.3 Recoveries of elemental analytes from the 5 ng mL−1 standard solution using LA-ICP-MS (n=3)………………………………………………………………………42
Table 4.4 Concentrations of elements determined in SRM 1643e………………………………………………………………………43
Table 5.1 Analyses of real samples using LA-ICP-MS and conventional ICP-MS (ng mL−1)………………………………………51
Table 5.2 ELPI specification ………………………………………55
Table 5.3 Sampling schedule and meteorological parameters during  fireworks festival in Yanshui, Tainan…………………56
Table 5.4 Element concentrations ( arithmetic mean±SD, in ng/m3) of nano, submicron, micron particles collected during the pre-fireworks period in Yanshui Township, Tainan County…………………………………………………………………… 58
Table 5.5 Element concentrations ( arithmetic mean±SD, in ng/m3) of nano, submicron,micron particles collected during the post-fireworks period in Yanshui Township, Tainan County…………………………………………………………………… 59
Table 5.6 Element concentrations in PM10(µg/m3) observed during various fireworks festivals from around the world… 63




List of Figures
Fig. 2.1. Schema of a laser ablation system, using ICP-OES and/or ICP-MS                                               9
Fig. 2.2. Fractionation versus wavelength               13
Fig. 2.3. C, Cu and Zn distribution in a cross section of rat brain sample (tumor tissue)                               15
Fig. 2.4. Application of LA-ICP-MS                         21
Fig. 3.1. Scheme of converting liquid droplet into dried droplet by evaporation of solvent                       23
Fig. 3.2. Photograph of laser ablation device 213       24
Fig. 3.3. View of changing defocus of crater size       26
Fig. 3.4. Photograph of ICP-MS 7500a system               27
Fig. 3.5. Photograph of standard solution on the filter medium                                                        29
Fig. 3.6. Scheme of preparing standard and real filter samples for LA-ICP-MS                                      30
Fig. 4.1. Effects of laser energy level on the ion intensity                                                  32
Fig. 4.2 Effects of dwell time on the ion intensities      33
Fig. 4.3. Effects of defocus distance on the ion intensity                                               35
Fig. 4.4. Still video images of LA of dried droplets (1µL) on the PTFE filter membrane                               37
Fig. 4.5. Transient signals obtained using LA-ICP-MS for the elements Mn, Co, Ni, Cu, As and Pb in the blake and 5 and 20 ngmL-1 standard solutions                               38
Fig. 4.6. Comparison of the signal intensities of 208Pb from the blank and the 50 ngmL-1 standard solution using LA-ICP- MS                                                         39
Fig. 4.7. Standard addition calibration curves of 63Cu and 65Zn in tap water with LA-ICP-MS (n=3)                     44
Fig. 4.8. Effects of MB concentration on the signal intensity of the various elements                          46
Fig. 4.9. Effect of NaCl concentration on the signal intensity of the various elements                          47
Fig. 5.1. Principle of preparing real filter sample and process of LA-ICP-MS                                       50
Fig. 5.2. Maps of the sampling site                        54
Fig. 5.3. Average element concentrations in (a) PM10 and (b) PM.2.5 (c) PM2.5-to- PM10 ratios during the pre- and post- fireworks display periods                                  61
Fig. 5.4. Mass concentration distributions of Na, Mg, Al, Si, Ca and Fe with respect to particle size in ambient air during the fireworks festival                              65
Fig. 5.5. Concentration distribution of K, V, Cr, Mn, Cu, Zn, As, Sr, Ba, and Pb elements with respect to particle size in ambient air during the fireworks festival          67
Fig. 5.6. Toxicity of different sized particles toward BEAS-2B cells after incubation for 24 h                    70


                                

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