光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
11期
3109-3112
,共4页
张六一%付川%杨复沫%杨季冬%黄怡民%张强%吴炳煜
張六一%付川%楊複沫%楊季鼕%黃怡民%張彊%吳炳煜
장륙일%부천%양복말%양계동%황이민%장강%오병욱
微波消解%ICP-OES%细颗粒物%检出限%回收
微波消解%ICP-OES%細顆粒物%檢齣限%迴收
미파소해%ICP-OES%세과립물%검출한%회수
Microwave digestion%ICP-OES%Fine particulate matter%Detection limit%Recovery
重金属具有不可降解性,细颗粒物(PM2.5)中重金属可随呼吸进入体内,对人体构成潜在的威胁。因此,有必要针对颗粒物中重金属元素的测定方法进行研究。用玻璃纤维滤膜采样、密闭微波消解进行前处理,建立了电感耦合等离子体发射光谱仪(ICP-OES)测定PM2.5中铅、锌、铜、镉、铬的分析方法。考察了微波消解体系,通过信噪比选取了铅、锌、铜、镉、铬的最佳分析谱线和最优仪器测试条件,其结果为:(1) HNO3-H2 O2消解体系比HNO3-HCl和 HNO3-H2 SO4消解体系更稳定、更彻底;(2)铅、锌、铜、镉、铬的最佳分析线分别为220.353,213.857,327.393,228.802,267.716 nm ;(3)仪器最优测试条件为射频功率1300W ,蠕动泵流速1.5mL·min-1,冷却气流量15L·min-1,载气流速0.8L·min-1。本方法元素的检出限为2.02×10-3~8.20×10-3μg · mL -1,滤膜样品测定的相对标准偏差(RSD , n=6)为1.86%~2.82%,加标回收率为91.6%~103.7%。对重庆市中科院万州监测点细颗粒物中铅、锌、铜、镉、铬的含量进行了分析,结果表明:万州城区细颗粒物没有受到镉和铬的污染,细颗粒物中铅处于潜在污染水平,锌和铜处于轻度污染水平。
重金屬具有不可降解性,細顆粒物(PM2.5)中重金屬可隨呼吸進入體內,對人體構成潛在的威脅。因此,有必要針對顆粒物中重金屬元素的測定方法進行研究。用玻璃纖維濾膜採樣、密閉微波消解進行前處理,建立瞭電感耦閤等離子體髮射光譜儀(ICP-OES)測定PM2.5中鉛、鋅、銅、鎘、鉻的分析方法。攷察瞭微波消解體繫,通過信譟比選取瞭鉛、鋅、銅、鎘、鉻的最佳分析譜線和最優儀器測試條件,其結果為:(1) HNO3-H2 O2消解體繫比HNO3-HCl和 HNO3-H2 SO4消解體繫更穩定、更徹底;(2)鉛、鋅、銅、鎘、鉻的最佳分析線分彆為220.353,213.857,327.393,228.802,267.716 nm ;(3)儀器最優測試條件為射頻功率1300W ,蠕動泵流速1.5mL·min-1,冷卻氣流量15L·min-1,載氣流速0.8L·min-1。本方法元素的檢齣限為2.02×10-3~8.20×10-3μg · mL -1,濾膜樣品測定的相對標準偏差(RSD , n=6)為1.86%~2.82%,加標迴收率為91.6%~103.7%。對重慶市中科院萬州鑑測點細顆粒物中鉛、鋅、銅、鎘、鉻的含量進行瞭分析,結果錶明:萬州城區細顆粒物沒有受到鎘和鉻的汙染,細顆粒物中鉛處于潛在汙染水平,鋅和銅處于輕度汙染水平。
중금속구유불가강해성,세과립물(PM2.5)중중금속가수호흡진입체내,대인체구성잠재적위협。인차,유필요침대과립물중중금속원소적측정방법진행연구。용파리섬유려막채양、밀폐미파소해진행전처리,건립료전감우합등리자체발사광보의(ICP-OES)측정PM2.5중연、자、동、력、락적분석방법。고찰료미파소해체계,통과신조비선취료연、자、동、력、락적최가분석보선화최우의기측시조건,기결과위:(1) HNO3-H2 O2소해체계비HNO3-HCl화 HNO3-H2 SO4소해체계경은정、경철저;(2)연、자、동、력、락적최가분석선분별위220.353,213.857,327.393,228.802,267.716 nm ;(3)의기최우측시조건위사빈공솔1300W ,연동빙류속1.5mL·min-1,냉각기류량15L·min-1,재기류속0.8L·min-1。본방법원소적검출한위2.02×10-3~8.20×10-3μg · mL -1,려막양품측정적상대표준편차(RSD , n=6)위1.86%~2.82%,가표회수솔위91.6%~103.7%。대중경시중과원만주감측점세과립물중연、자、동、력、락적함량진행료분석,결과표명:만주성구세과립물몰유수도력화락적오염,세과립물중연처우잠재오염수평,자화동처우경도오염수평。
In the present work ,a method was developed for determining lead ,zinc ,copper ,cadmium ,znd chromium in PM2.5 by inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis with microwave digestion and glass fibre filter collection of samples .The microwave digestion systems were investigated and the experimental conditions were optimized .The results show that (1) HNO3-H2 O2 digestion system is more stable and complete than HNO3-HCl and HNO3-H2 SO4 digestion systems ;(2) The most sensitive emission wave length of lead ,zinc ,copper ,cadmium ,and chromium are 220.353 ,213.857 , 327.393 ,228.802 ,and 267.716 nm ,respectively ;(3) The highest signal-to-noise ratios were observed under the conditions :RF power of 1 300 W ,peristaltic pump flow rate of 1.5 mL · min-1 ,cooling gas flow rate of 15 L · min-1 ,and carrier gas flow rate of 0.8 L · min-1 .In addition ,the detection limit for these elements ranged between 2.02 × 10-3 and 8.20 × 10-3 μg · mL -1 ,the relative standard deviations (RSD ,n=6) for the samples were in the range of 1.86% ~2.82% ,and the recovery for the elements determined was from 91.6% to 103.7% .The proposed method was used for determination of the above five ele-ments in atmospheric fine particulate matter at Wanzhou Monitoring Site of Chongqing Institute of Green and Intelligent Technol-ogy .The results revealed that the atmospheric fine particulate matter at this monitoring site was not polluted by cadmium and chromium ,lead was at the level of potential contamination ,while zinc and copper were at the level of slight pollution .