Swami K, Judd C D, Orsini J, Yang K X, Husain L
Wadsworth Center, New York State Department of Health, Albany, New York 12201-0509, USA.
Fresenius J Anal Chem. 2001 Jan 1;369(1):63-70. doi: 10.1007/s002160000575.
A microwave digestion method in a closed vessel was developed for the determination of trace metals in atmospheric aerosols using inductively coupled plasma mass spectrometry (ICP-MS). A recovery study for the elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, Sb, and Pb was conducted using multi-elemental standard solutions, NIST 1633b Trace Elements in Coal Fly Ash, and NIST 1648 Urban Particulate Matter. A simple digestion method using only HNO3/H2O2 gave good recoveries (90%-108%) for all elements except Cr in SRM 1648, but yielded low recoveries for SRM 1633b. A more robust method using HNO3/H2O2/HF/H3BO3 yielded higher recoveries (82%-103%) for the lighter elements (V-Zn) in SRM 1633b, and improved the Cr recovery in SRM 1648, but decreased the Se recovery in both SRMs. A comparative analysis of aerosol samples obtained at a remote mountain location Nathiagali, Pakistan (2.5 km above mean sea level), and Mayville, New York, downwind from the highly industrialized Midwestern United States, was carried out using Instrumental Neutron Activation Analysis (INAA) for the elements Cr, Mn, Fe, Co, Zn, As, Se, and Sb. The simple digestion method yielded excellent agreement for Cr, Fe, Zn, As, Se, and Sb, with slopes of the ICP-MS vs. INAA regressions of 0.90-1.00 and R2 values of 0.96-1.00. The regressions for Mn and Co had slopes of 0.82 and 0.84 with R2 values of 0.83 and 0.82, respectively. Addition of HF/H3BO3 did not improve the correlation for any of the elements and degraded the precision somewhat. The technique provides sensitivity and accuracy for trace elements in relatively small aerosol samples used in atmospheric chemistry studies related to SO2 oxidation in cloud droplets. The ability to determine concentrations of a very large number of elements from a single analysis will permit source apportionment of various trace pollutants and hence strategies to control the sources of air pollution. This is particularly important as the health effects of particulate matter are increasingly recognized.
开发了一种在密闭容器中的微波消解方法，用于使用电感耦合等离子体质谱法（ICP-MS）测定大气气溶胶中的痕量金属。使用多元素标准溶液、NIST 1633b煤灰中的痕量元素和NIST 1648城市颗粒物对V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Cd、Sb和Pb元素进行了回收率研究。仅使用HNO3/H2O2的简单消解方法对SRM 1648中除Cr以外的所有元素都有良好的回收率（90%-108%），但SRM 1633b的回收率较低。使用HNO3/H2O2/HF/H3BO3的更稳健方法对SRM 1633b中较轻的元素（V-Zn）产生了更高的回收率（82%-103%），并提高了SRM 1648中Cr的回收率，但降低了两种标准参考物质中Se的回收率。使用仪器中子活化分析（INAA）对在巴基斯坦偏远山区纳蒂亚加利（平均海拔2.5公里）和美国高度工业化的中西部地区下风处的纽约州梅维尔采集的气溶胶样品中的Cr、Mn、Fe、Co、Zn、As、Se和Sb元素进行了对比分析。简单消解方法对Cr、Fe、Zn、As、Se和Sb的结果一致性极佳，ICP-MS与INAA回归的斜率为0.90-1.00，R2值为0.96-1.00。Mn和Co的回归斜率分别为0.82和0.84，R2值分别为0.83和0.82。添加HF/H3BO3并没有改善任何元素的相关性，并且在一定程度上降低了精密度。该技术为与云滴中SO2氧化相关的大气化学研究中使用的相对较小的气溶胶样品中的痕量元素提供了灵敏度和准确性。一次分析就能测定大量元素浓度的能力将有助于对各种痕量污染物进行源解析，从而制定控制空气污染源头的策略。鉴于颗粒物对健康的影响越来越受到重视，这一点尤为重要。
