大气颗粒物中溴和碘的浓度特征及来源
摘要
针对大气颗粒物化学成分的研究是大气气溶胶化学中的基础研究领域,其研究成果可以为大气颗粒物的源解析以及大气气溶胶界面上的多相反应等方面的研究提供支持。溴、碘作为大气中重要的活性物种,参与了大气中的多种化学过程,对臭氧的损耗有重要影响,同时影响众多重要物种的源和汇,对大气化学过程起到重要的作用,研究活性卤素化学已成为近年来大气化学研究领域的热点问题。本论文从研究大气颗粒物中溴和碘的分析方法入手,研究了大气颗粒物中溴和碘的浓度特征及其来源,测定了大气颗粒物中碘的物种,研究了大气颗粒物源尘中溴和碘的含量、以及大气颗粒物中的主要人为源——煤燃烧过程中溴和碘的释放行为,得到以下研究结论。
1、微波消解ICP-MS同时测定大气颗粒物和煤样中溴和碘。(1)煤样的消解介质为7-8mLHNO3、1-2mLHF、2mLH2O2,颗粒物样品的消解介质为5mLHNO3、2mLH2O2和2滴HF。(2)测试液中硝酸介质浓度为5%。(3)氧化剂Na2S2O8的用量为1mL20%Na2S2O8溶液；加入1滴0.1%AgNO3溶液,将不同价态Br、I氧化至统一高价态。(4)溴、碘的检测限分别为5 ng/mL和0.15ng/mL。(5)Br的加标回收率为80-110%,I的加标回收率为80-120%,符合ISO 5725标准中一般接受范围70-130%的要求。(6)本方法的测试结果符合土壤标样的标准值。
2、上海市大气颗粒物(TSP和PMlo)中溴和碘的浓度特征。(1)采样期间,TSP中总溴和总碘含量的均值分别为163.6±108.7μg/g和55.6±37.μg/g;PM10中总溴和总碘的含量均值分别为230.4±137.0μg/g和78.4±44.3 gg/g。(2)采样期间,TSP中总溴和总碘的体积浓度均值分别为27±20 ng/m3和9.4±5.6ng/m3, PM10中总溴和总碘的体积浓度均值分别为22±14 ng/m3和8.0±4.6 ng/m3。(3)TSP和PMlo中总溴体积浓度的季节变化规律表现为秋季>春季>冬季>夏季；TSP和PM10中总碘体积浓度的季节变化规律表现为冬季>春季>秋季>夏季；TSP和PMlo中水溶性和酸溶性溴和碘的季节变化规律与总溴和总碘的规律基本一致。(4)TSP中Br/I的比值和PM1o中Br/I的比值分别为7.0±16.5和5.3±9.6。(5)TSP中水溶性溴和碘占总溴和总碘的比例分别为34±18%和32±19%,PM1o中水溶性溴和碘占总溴和总碘的比例分别为31±18%和32±15%；与水溶性溴、碘相比,PM1o中溴、碘溶出量增加了22.5%和18.4%。
3、大气颗粒物源尘中溴和碘以及煤燃烧过程中溴和碘的释放行为。(1)煤炭中溴含量约10-30μg/g,碘含量约1-10μg/g。(2)燃烧过程中,Br、I的释放率随温度升高而增加,在1000℃处形成平台；强氧化性燃烧气氛对溴、碘的释放行为有抑制作用。(3)煤燃烧过程中,痕量元素I则几乎全部分布在气相中,而Br主要分布于气相中,在底渣和颗粒相中也有分布。(4)固体添加剂可以在燃烧过程中对溴和碘进行有效捕集。
4、上海市大气颗粒物中溴和碘的来源及其影响因素。(1)PM10中Br的富集因子(Efs)在0.3-3.0之间,均值为1.0±0.7；I的Efs在154-791之间,均值为426±169,碘的富集因子远远大于溴的富集因子。PMlo中的溴主要来源于海洋气溶胶,但同时存在溴的损失,尤其表现在春季和冬季；颗粒物中的碘主要来源于海洋气溶胶和受气粒转化的作用。(2)风向为向岸流时,大气颗粒物TSP、PM10中溴、碘的浓度均低于离岸流时的浓度,风向对大气中颗粒物中溴、碘浓度有显著影响。影响颗粒物中溴的主要气象因素为大气气压,而影响颗粒物中碘的主要气象因素为大气气压和温度。(3)当大气中SO2、NO2浓度上升时,大气颗粒物中Br、I的浓度呈现出不同程度的上升趋势；大气颗粒物中总碘的浓度与SO2及NO2呈显著正相关,总溴的相关性不显著；颗粒物中溶解性溴和碘与S02的相关性较高,与N02的相关性较弱。(4)随着城市大气污染程度的增加,大气颗粒物中Br/I在减小。颗粒物中Br/I比值与空气中主要污染物SO2、NO2呈现负相关,且PM10中Br/I比值与S02负相关达到显著水平。
5、大气颗粒物中碘的物种。(1)在昼间,PMlo中碘酸根、碘离子和可溶性有机碘含量分别为1.32±0.82μg/g、16.75±±9.43μg/g和18.23±±11.061μg/g；在夜间,PM1o中碘酸根、碘离子和可溶性有机碘含量分别为2.87±2.06μg/g、16.75±9.96gg/g和24.21±11.46μg/g。(2)在昼间,PM10中碘酸根、碘离子和可溶性有机碘的浓度分别为0.24±0.22 ng/m3、3.36±2.21 ng/m3和3.67±2.67 ng/m3；在夜间,碘酸根、碘离子和可溶性有机碘的浓度分别为0.244±0.22 ng/m3、3.11±±2.21 ng/m3和2.97±±2.77 ng/m3。(3)在昼间,PM1o中碘酸根、碘离子和可溶性有机碘离子占溶解性碘的比例分别为3.1±1.3%、47.1±2.4%和49.4±2.5%；在夜间,PMlo中碘酸根、碘离子和可溶性有机碘离子占溶解性碘的比例分别为3.9±3.7%、53.4±8.7%和42.7±11.5%。
Study on chemical composition of aerosols, which can provide basic data for source apportionment of atmosphric particulate and heterogeneous reaction on particulate, is the basic research area. Bromine and Iodine are important reactive halogen species in the atmosphere, which can participate in many atmospheric chemical processes, play important role in the ozone depletion, affect sources and sinks of many important compounds. Reactive halogen chemistry is an important frontier research field in the atmospheric chemistry. Therefore, the aim of this dissertation is to develop a analytical method of iodine and bromine in coal and atmospheric particles, research concentration characteristics and sources of bromine and iodine in aerosols, and behavior of the trace elements bromine and iodine during coal combustion process.
1. Determination of iodine and bromine in coal and atmospheric particles by inductively coupled plasma mass spectrometry. (1) 7-8 mL of nitric acid,1-2 mL of hydrofluoric acid, and 2 mL of hydrogen peroxide were used as digestion solution for coal, and for atmospheric particles,5 mL of nitric acid,2 drops of hydrofluoric acid, and 2 mL of hydrogen peroxide were used as digestion solution. (2) 5%(V/V) of nitric acid in determination solution was employed in this analytical method. (3) 1mL of NaS2O8(20% solution) and one drop of 0.1% AgNO3 solution were introduced in determination solution for oxidizing Br and I to the same valence. (4) The detection limits (DL) of Br and I were 5 ng/mL and 0.15 ng/mL, respectively. (5) The recoveries of Br and I ranged from 80% to 110% and from 80% to 120%, respectively. The accuracy of the method was well within the generally accepted range of 70-130% indicated in ISO 5725. (6) The determined contents of Br and I in soil certified reference materials by this method were accurate with comparison of certified value.
2. Concentration characteristics of bromine and iodine in aerosols in Shanghai. (1) The contents of total Br and total I are 163.6±108.7μg/g and 55.6±37.7μg/g for TSP, and 230.4±137.0μg/g and 78.4±44.3μg/g for PM10, in sampling period, respectively. (2) The concentrations of total Br and total I are 27±20 ng/m3 and 9.4±5.6 ng/m3 for TSP, and 22±14 ng/m3 and 8.0±4.6 ng/m3 for PM10, in sampling period, respectively. (3) The seasonal variations of total Br concentrations in TSP and PM10 were Autumn> Spring> Winter> Summer. For total I, the seasonal variations in TSP and PM10 were Winter> Spring> Autumn > Summer. (4) The Br/I ratios are 7.0±16.5 and 5.3±9.6 for TSP and PM10, respectively. (5) For TSP, watersoluble Br and I accounted for 34±18% and 32±19% of the total Br and total I, while for PM10, water-soluble Br and I accounted for 31±18% and 32±15%, respectively. Soluble Br and I in PM10 extracted by acid increased by 22% and 18% respectively, compared with water-soluble Br and I.
3. The contents of Br and I in source dust of aerosols, and the behavior of bromine and iodine during coal combustion process. (1) The contents of Br and I in different coal are ranged from 10 to 30μg/g, and from 1 to 10μg/g, respectively. (2) The release of bromine and iodine increased with an increase in temperature, decreased with the increase of oxygen concentration. (3) At the given experimental condition, iodine was observed almost entirely in the vapor phase, but bromine was observed dominantly in the vapor phase, as well as in residue and particulate matter, respectively. (4) Solid additives could capture bromine and iodine effectively during coal combustion process.
4. The sources and effect factors of Br and I in aerosols in Shanghai. (1) The sea water enrichment factor for Br ranged from 0.3 to 3.0, with a mean of 1.0±0.7, whilst for I, it ranged from 154 to 791, with a mean of 426±169 for PM10. It indicated that I concentrations were essentially affected by marine aerosol concentrations and the gas-to-particle reactions in the production of I aerosols. The major part of aerosols bromine originated from marine sources, and the bromine depletion on particulate surface was very high in summer and autumn. (2) When the wind flowed to the shore, the concentrations of particulate bromine and particulate iodine were lower than the values in the offshore flow. The wind direction, air pressure and air temperature were the major factors in influencing the concentration of Br and I in aerosols. (3) The concentrations of Br and I in aerosols increased with the concentrations of SO2 and NO2 increasing. Iodine in aerosols showed a highly positive correlation with SO2 and NO2, whereas for Br, it only weakly correlated with these pollutants. (4) When the air quality deteriorated, the Br/I ratio decreased. The Br/I ratio in aerosols showed a highly negative correlation with SO2 and NO2 in air.
5. Iodine speciation in PM10. (1) The contents of iodate, iodide and soluble organic iodine(SOI) are 1.32±0.82μg/g,16.75±9.43μg/g and 18.23±11.06μg/g for PM10, during the day, respectively. The contents of iodate, iodide and SOI are 2.87±2.06μg/g,16.75±9.96μg/g and 24.21±11.46μg/g for PM10 during the night, respectively. (2) The concentrations of iodate, iodide and SOI are 0.24±0.22 ng/m3,3.36±2.21 ng/m3 and 3.67±2.67 ng/m3 for PM10, during the day, respectively. The concentrations of iodate, iodide and SOI are 0.24±0.22 ng/m3, 3.11±2.21 ng/m3 and 2.97±2.77 ng/m3 for PM10, during the night, respectively. (3) SOI and iodide are the most abundant fraction, accounting for 49.4±2.5%,47.1±2.4% during the day, and 42.7±11.5%,53.4±8.7% during the night, respectively.
1、微波消解ICP-MS同时测定大气颗粒物和煤样中溴和碘。(1)煤样的消解介质为7-8mLHNO3、1-2mLHF、2mLH2O2,颗粒物样品的消解介质为5mLHNO3、2mLH2O2和2滴HF。(2)测试液中硝酸介质浓度为5%。(3)氧化剂Na2S2O8的用量为1mL20%Na2S2O8溶液；加入1滴0.1%AgNO3溶液,将不同价态Br、I氧化至统一高价态。(4)溴、碘的检测限分别为5 ng/mL和0.15ng/mL。(5)Br的加标回收率为80-110%,I的加标回收率为80-120%,符合ISO 5725标准中一般接受范围70-130%的要求。(6)本方法的测试结果符合土壤标样的标准值。
2、上海市大气颗粒物(TSP和PMlo)中溴和碘的浓度特征。(1)采样期间,TSP中总溴和总碘含量的均值分别为163.6±108.7μg/g和55.6±37.μg/g;PM10中总溴和总碘的含量均值分别为230.4±137.0μg/g和78.4±44.3 gg/g。(2)采样期间,TSP中总溴和总碘的体积浓度均值分别为27±20 ng/m3和9.4±5.6ng/m3, PM10中总溴和总碘的体积浓度均值分别为22±14 ng/m3和8.0±4.6 ng/m3。(3)TSP和PMlo中总溴体积浓度的季节变化规律表现为秋季>春季>冬季>夏季；TSP和PM10中总碘体积浓度的季节变化规律表现为冬季>春季>秋季>夏季；TSP和PMlo中水溶性和酸溶性溴和碘的季节变化规律与总溴和总碘的规律基本一致。(4)TSP中Br/I的比值和PM1o中Br/I的比值分别为7.0±16.5和5.3±9.6。(5)TSP中水溶性溴和碘占总溴和总碘的比例分别为34±18%和32±19%,PM1o中水溶性溴和碘占总溴和总碘的比例分别为31±18%和32±15%；与水溶性溴、碘相比,PM1o中溴、碘溶出量增加了22.5%和18.4%。
3、大气颗粒物源尘中溴和碘以及煤燃烧过程中溴和碘的释放行为。(1)煤炭中溴含量约10-30μg/g,碘含量约1-10μg/g。(2)燃烧过程中,Br、I的释放率随温度升高而增加,在1000℃处形成平台；强氧化性燃烧气氛对溴、碘的释放行为有抑制作用。(3)煤燃烧过程中,痕量元素I则几乎全部分布在气相中,而Br主要分布于气相中,在底渣和颗粒相中也有分布。(4)固体添加剂可以在燃烧过程中对溴和碘进行有效捕集。
4、上海市大气颗粒物中溴和碘的来源及其影响因素。(1)PM10中Br的富集因子(Efs)在0.3-3.0之间,均值为1.0±0.7；I的Efs在154-791之间,均值为426±169,碘的富集因子远远大于溴的富集因子。PMlo中的溴主要来源于海洋气溶胶,但同时存在溴的损失,尤其表现在春季和冬季；颗粒物中的碘主要来源于海洋气溶胶和受气粒转化的作用。(2)风向为向岸流时,大气颗粒物TSP、PM10中溴、碘的浓度均低于离岸流时的浓度,风向对大气中颗粒物中溴、碘浓度有显著影响。影响颗粒物中溴的主要气象因素为大气气压,而影响颗粒物中碘的主要气象因素为大气气压和温度。(3)当大气中SO2、NO2浓度上升时,大气颗粒物中Br、I的浓度呈现出不同程度的上升趋势；大气颗粒物中总碘的浓度与SO2及NO2呈显著正相关,总溴的相关性不显著；颗粒物中溶解性溴和碘与S02的相关性较高,与N02的相关性较弱。(4)随着城市大气污染程度的增加,大气颗粒物中Br/I在减小。颗粒物中Br/I比值与空气中主要污染物SO2、NO2呈现负相关,且PM10中Br/I比值与S02负相关达到显著水平。
5、大气颗粒物中碘的物种。(1)在昼间,PMlo中碘酸根、碘离子和可溶性有机碘含量分别为1.32±0.82μg/g、16.75±±9.43μg/g和18.23±±11.061μg/g；在夜间,PM1o中碘酸根、碘离子和可溶性有机碘含量分别为2.87±2.06μg/g、16.75±9.96gg/g和24.21±11.46μg/g。(2)在昼间,PM10中碘酸根、碘离子和可溶性有机碘的浓度分别为0.24±0.22 ng/m3、3.36±2.21 ng/m3和3.67±2.67 ng/m3；在夜间,碘酸根、碘离子和可溶性有机碘的浓度分别为0.244±0.22 ng/m3、3.11±±2.21 ng/m3和2.97±±2.77 ng/m3。(3)在昼间,PM1o中碘酸根、碘离子和可溶性有机碘离子占溶解性碘的比例分别为3.1±1.3%、47.1±2.4%和49.4±2.5%；在夜间,PMlo中碘酸根、碘离子和可溶性有机碘离子占溶解性碘的比例分别为3.9±3.7%、53.4±8.7%和42.7±11.5%。
Study on chemical composition of aerosols, which can provide basic data for source apportionment of atmosphric particulate and heterogeneous reaction on particulate, is the basic research area. Bromine and Iodine are important reactive halogen species in the atmosphere, which can participate in many atmospheric chemical processes, play important role in the ozone depletion, affect sources and sinks of many important compounds. Reactive halogen chemistry is an important frontier research field in the atmospheric chemistry. Therefore, the aim of this dissertation is to develop a analytical method of iodine and bromine in coal and atmospheric particles, research concentration characteristics and sources of bromine and iodine in aerosols, and behavior of the trace elements bromine and iodine during coal combustion process.
1. Determination of iodine and bromine in coal and atmospheric particles by inductively coupled plasma mass spectrometry. (1) 7-8 mL of nitric acid,1-2 mL of hydrofluoric acid, and 2 mL of hydrogen peroxide were used as digestion solution for coal, and for atmospheric particles,5 mL of nitric acid,2 drops of hydrofluoric acid, and 2 mL of hydrogen peroxide were used as digestion solution. (2) 5%(V/V) of nitric acid in determination solution was employed in this analytical method. (3) 1mL of NaS2O8(20% solution) and one drop of 0.1% AgNO3 solution were introduced in determination solution for oxidizing Br and I to the same valence. (4) The detection limits (DL) of Br and I were 5 ng/mL and 0.15 ng/mL, respectively. (5) The recoveries of Br and I ranged from 80% to 110% and from 80% to 120%, respectively. The accuracy of the method was well within the generally accepted range of 70-130% indicated in ISO 5725. (6) The determined contents of Br and I in soil certified reference materials by this method were accurate with comparison of certified value.
2. Concentration characteristics of bromine and iodine in aerosols in Shanghai. (1) The contents of total Br and total I are 163.6±108.7μg/g and 55.6±37.7μg/g for TSP, and 230.4±137.0μg/g and 78.4±44.3μg/g for PM10, in sampling period, respectively. (2) The concentrations of total Br and total I are 27±20 ng/m3 and 9.4±5.6 ng/m3 for TSP, and 22±14 ng/m3 and 8.0±4.6 ng/m3 for PM10, in sampling period, respectively. (3) The seasonal variations of total Br concentrations in TSP and PM10 were Autumn> Spring> Winter> Summer. For total I, the seasonal variations in TSP and PM10 were Winter> Spring> Autumn > Summer. (4) The Br/I ratios are 7.0±16.5 and 5.3±9.6 for TSP and PM10, respectively. (5) For TSP, watersoluble Br and I accounted for 34±18% and 32±19% of the total Br and total I, while for PM10, water-soluble Br and I accounted for 31±18% and 32±15%, respectively. Soluble Br and I in PM10 extracted by acid increased by 22% and 18% respectively, compared with water-soluble Br and I.
3. The contents of Br and I in source dust of aerosols, and the behavior of bromine and iodine during coal combustion process. (1) The contents of Br and I in different coal are ranged from 10 to 30μg/g, and from 1 to 10μg/g, respectively. (2) The release of bromine and iodine increased with an increase in temperature, decreased with the increase of oxygen concentration. (3) At the given experimental condition, iodine was observed almost entirely in the vapor phase, but bromine was observed dominantly in the vapor phase, as well as in residue and particulate matter, respectively. (4) Solid additives could capture bromine and iodine effectively during coal combustion process.
4. The sources and effect factors of Br and I in aerosols in Shanghai. (1) The sea water enrichment factor for Br ranged from 0.3 to 3.0, with a mean of 1.0±0.7, whilst for I, it ranged from 154 to 791, with a mean of 426±169 for PM10. It indicated that I concentrations were essentially affected by marine aerosol concentrations and the gas-to-particle reactions in the production of I aerosols. The major part of aerosols bromine originated from marine sources, and the bromine depletion on particulate surface was very high in summer and autumn. (2) When the wind flowed to the shore, the concentrations of particulate bromine and particulate iodine were lower than the values in the offshore flow. The wind direction, air pressure and air temperature were the major factors in influencing the concentration of Br and I in aerosols. (3) The concentrations of Br and I in aerosols increased with the concentrations of SO2 and NO2 increasing. Iodine in aerosols showed a highly positive correlation with SO2 and NO2, whereas for Br, it only weakly correlated with these pollutants. (4) When the air quality deteriorated, the Br/I ratio decreased. The Br/I ratio in aerosols showed a highly negative correlation with SO2 and NO2 in air.
5. Iodine speciation in PM10. (1) The contents of iodate, iodide and soluble organic iodine(SOI) are 1.32±0.82μg/g,16.75±9.43μg/g and 18.23±11.06μg/g for PM10, during the day, respectively. The contents of iodate, iodide and SOI are 2.87±2.06μg/g,16.75±9.96μg/g and 24.21±11.46μg/g for PM10 during the night, respectively. (2) The concentrations of iodate, iodide and SOI are 0.24±0.22 ng/m3,3.36±2.21 ng/m3 and 3.67±2.67 ng/m3 for PM10, during the day, respectively. The concentrations of iodate, iodide and SOI are 0.24±0.22 ng/m3, 3.11±2.21 ng/m3 and 2.97±2.77 ng/m3 for PM10, during the night, respectively. (3) SOI and iodide are the most abundant fraction, accounting for 49.4±2.5%,47.1±2.4% during the day, and 42.7±11.5%,53.4±8.7% during the night, respectively.
引文
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