给水排水
給水排水
급수배수
2015年
8期
9-14,15
,共7页
刘金明%徐斌%朱文倩%田富箱
劉金明%徐斌%硃文倩%田富箱
류금명%서빈%주문천%전부상
固相微萃取%碘代消毒副产物%萃取条件%解析条件
固相微萃取%碘代消毒副產物%萃取條件%解析條件
고상미췌취%전대소독부산물%췌취조건%해석조건
Solid phase microextraction (SPME)%Iodine disinfection by-products(I-DBPs)%Ex-traction conditions%Desorption conditions
碘代消毒副产物(I-DBPS)是饮用水消毒过程中发现的一类暂未受控的新兴高致毒性消毒副产物。为了便于对饮用水中 I-DBPS 进行研究,可采用固相微萃取(SPME)-气质(GC/MS)联用技术来检测分析,介绍了固相微萃取的装置、操作及萃取方法,着重论述了其工作条件的选择,得出最佳优化条件:以 DVB/CAR/PDMS 作为萃取膜,萃取温度为65℃,萃取时间为45 min,离子强度用25%(W/V)Na2 SO4调节,搅拌速率为250 r/min,并且在气相色谱中的解析温度为220℃,解析时间为30 s。同时进行重复性和再现性试验对方法的检测限、精确度与准确度进行了评价。结果表明,采用 SPME-GC/MS 方法,分析物的检测限在10~50 ng/L,可以用来检测 ng/L 级水平的痕量碘代三卤甲烷(I-THMS),且在分析物标准浓度为0.1μg/L 时,重复性试验的相关标准偏差(RSD)在0.4%~1.5%,再现性试验的 RSD 在4%~12.5%,这表明该方法应用于痕量 I-DBPS 的分析检测是精确可靠的。
碘代消毒副產物(I-DBPS)是飲用水消毒過程中髮現的一類暫未受控的新興高緻毒性消毒副產物。為瞭便于對飲用水中 I-DBPS 進行研究,可採用固相微萃取(SPME)-氣質(GC/MS)聯用技術來檢測分析,介紹瞭固相微萃取的裝置、操作及萃取方法,著重論述瞭其工作條件的選擇,得齣最佳優化條件:以 DVB/CAR/PDMS 作為萃取膜,萃取溫度為65℃,萃取時間為45 min,離子彊度用25%(W/V)Na2 SO4調節,攪拌速率為250 r/min,併且在氣相色譜中的解析溫度為220℃,解析時間為30 s。同時進行重複性和再現性試驗對方法的檢測限、精確度與準確度進行瞭評價。結果錶明,採用 SPME-GC/MS 方法,分析物的檢測限在10~50 ng/L,可以用來檢測 ng/L 級水平的痕量碘代三滷甲烷(I-THMS),且在分析物標準濃度為0.1μg/L 時,重複性試驗的相關標準偏差(RSD)在0.4%~1.5%,再現性試驗的 RSD 在4%~12.5%,這錶明該方法應用于痕量 I-DBPS 的分析檢測是精確可靠的。
전대소독부산물(I-DBPS)시음용수소독과정중발현적일류잠미수공적신흥고치독성소독부산물。위료편우대음용수중 I-DBPS 진행연구,가채용고상미췌취(SPME)-기질(GC/MS)련용기술래검측분석,개소료고상미췌취적장치、조작급췌취방법,착중논술료기공작조건적선택,득출최가우화조건:이 DVB/CAR/PDMS 작위췌취막,췌취온도위65℃,췌취시간위45 min,리자강도용25%(W/V)Na2 SO4조절,교반속솔위250 r/min,병차재기상색보중적해석온도위220℃,해석시간위30 s。동시진행중복성화재현성시험대방법적검측한、정학도여준학도진행료평개。결과표명,채용 SPME-GC/MS 방법,분석물적검측한재10~50 ng/L,가이용래검측 ng/L 급수평적흔량전대삼서갑완(I-THMS),차재분석물표준농도위0.1μg/L 시,중복성시험적상관표준편차(RSD)재0.4%~1.5%,재현성시험적 RSD 재4%~12.5%,저표명해방법응용우흔량 I-DBPS 적분석검측시정학가고적。
The iodine-disinfection by-products (I-DBPs)are a kind of disinfection by-products which were newly found in the process of drinking water disinfection.In this research,solid-phase micro extrac-tion(SPME)-GC/MS was used to study I-DBPs.Meanwhile,the installation and operation of SPME and the methods for extraction were also introduced in this paper.In addition,this paper also highlighted the choosing of working conditions for extraction and analysis.In the end,this paper proposed the most suit-able condition for extraction and analysis as follow:the DVB/CAR/PDMS should be used as extraction disks;the extraction temperature should be 65 ℃ and duration time 45 min,accordingly;the 25% (W/V) Na2 SO4 should be used to regulate the ionic strength;the mixing rate should be about 250 rmp;the tem-perature of desorption in gas chromatography might be 220 ℃ and the desorption should last for 30 s.In this paper,repeatability and reproducibility experiments were applied to test the detection limits,precision and accuracy of SPME-GC/ME.The results showed that if the detection limit of analysis was 10~50 ng/L,the SPME-GC/MS could be adopted to test the trace I-THMs at ng/L level;the standard concentration of analysis was 0.1 μg/L;the RSD of repeatability and reproducibility experiments were 0.4%~1.5%and 4%~12.5%,respectively.These data indicated that it would be accurate and reliable to use SPME-GC/MS to detect and analyze I-DBPs.