分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2010年
2期
219-224
,共6页
徐思琦%谢周清%刘崴%杨红霞%李冰
徐思琦%謝週清%劉崴%楊紅霞%李冰
서사기%사주청%류외%양홍하%리빙
气溶胶%溴%碘%形态%高效液相色谱-电感耦合等离子体质谱
氣溶膠%溴%碘%形態%高效液相色譜-電感耦閤等離子體質譜
기용효%추%전%형태%고효액상색보-전감우합등리자체질보
Atmospheric aerosol%Iodine and bromine species%High performance liquid chromatography-inductively) coupled plasma mass spectrometry
比较了超声纯水提取不同时间和多种密封提取条件下大气气溶胶样品滤膜中溴、碘形态稳定性和提取率.结果表明:密封提取方法的提取率高于超声提取方法,但有可能破坏了某种未知的有机碘形态;在长时间纯水超声条件下,醋酸纤维(CF)空白滤膜加标回收中I~-形态不稳定.因此,纯水超声提取5 min为最佳提取条件.对比醋酸纤维(CF)和玻璃纤维(GF)空白滤膜加标回收实验发现,各种提取条件下GF材质对样品中溴、碘形态稳定性的干扰比CF材质小.在优化大气气溶胶溴、碘形态提取方法的基础上,建立了HPLC-ICP-MS测定大气气溶胶中BrO_3~-、Br~-、IO_3~-和I~-的方法,并对合肥地区气溶胶样品中溴、碘总量及形态进行测定.合肥地区气溶胶中溴和碘总量浓度分别为883和231 pmol/m~3.其中,Br~-占总溴的69%,BrO_3~-未检出;70%的碘为未知形态,包括可溶性有机碘和不可溶性碘.
比較瞭超聲純水提取不同時間和多種密封提取條件下大氣氣溶膠樣品濾膜中溴、碘形態穩定性和提取率.結果錶明:密封提取方法的提取率高于超聲提取方法,但有可能破壞瞭某種未知的有機碘形態;在長時間純水超聲條件下,醋痠纖維(CF)空白濾膜加標迴收中I~-形態不穩定.因此,純水超聲提取5 min為最佳提取條件.對比醋痠纖維(CF)和玻璃纖維(GF)空白濾膜加標迴收實驗髮現,各種提取條件下GF材質對樣品中溴、碘形態穩定性的榦擾比CF材質小.在優化大氣氣溶膠溴、碘形態提取方法的基礎上,建立瞭HPLC-ICP-MS測定大氣氣溶膠中BrO_3~-、Br~-、IO_3~-和I~-的方法,併對閤肥地區氣溶膠樣品中溴、碘總量及形態進行測定.閤肥地區氣溶膠中溴和碘總量濃度分彆為883和231 pmol/m~3.其中,Br~-佔總溴的69%,BrO_3~-未檢齣;70%的碘為未知形態,包括可溶性有機碘和不可溶性碘.
비교료초성순수제취불동시간화다충밀봉제취조건하대기기용효양품려막중추、전형태은정성화제취솔.결과표명:밀봉제취방법적제취솔고우초성제취방법,단유가능파배료모충미지적유궤전형태;재장시간순수초성조건하,작산섬유(CF)공백려막가표회수중I~-형태불은정.인차,순수초성제취5 min위최가제취조건.대비작산섬유(CF)화파리섬유(GF)공백려막가표회수실험발현,각충제취조건하GF재질대양품중추、전형태은정성적간우비CF재질소.재우화대기기용효추、전형태제취방법적기출상,건립료HPLC-ICP-MS측정대기기용효중BrO_3~-、Br~-、IO_3~-화I~-적방법,병대합비지구기용효양품중추、전총량급형태진행측정.합비지구기용효중추화전총량농도분별위883화231 pmol/m~3.기중,Br~-점총추적69%,BrO_3~-미검출;70%적전위미지형태,포괄가용성유궤전화불가용성전.
The species of bromine and iodine in aerosol samples were extracted using ultra-pure water-ultrasonic method with different time in-length and pressurizing decomposition with dilute ammonia, respectively. The efficiency of extraction and the stability of bromine and iodine species were compared under different extraction) conditions. Results showed that(1) the efficiency of extraction using pressurizing decomposition, which might destroy some unknown form of organic iodine, was relatively higher than the one by ultrasonic method;(2) I~- was unstable in added standard cellular blank filter during ultrasonic assisted extraction for long time;(3) The optimum condition was ultra-pure water-ultrasonic assisted extraction for 5 min. Moreover), the suitability of glass microfiber filter(GF) and cellular filter(CF) during extraction for bromine and iodine) species in aerosol was also compared, which indicated that GF is favorable for species analysis than CF under different kinds of extraction conditions. Based upon the extraction results, HPLC-ICP-MS approach was developed to analyze bromine and iodine) species in atmospheric aerosol. The total iodine, bromine and species in the aerosol samples collected in Hefei were then determined accordingly. The levels of total bromine and iodine) in Hefei aerosols were 883 and 231 pmol/m~3, respectively. Br~- was found to be dominant species with 68%, while BrO_3~- was undetectable. 70% of total iodine occurred as unidentified forms including soluble organic) iodine and insoluble iodine.