光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
7期
1886-1889
,共4页
刘立柱%董发勤%孙仕勇%贺小春%王明翠
劉立柱%董髮勤%孫仕勇%賀小春%王明翠
류립주%동발근%손사용%하소춘%왕명취
羟自由基%石英粉%荧光光谱%定量检测%对苯二甲酸
羥自由基%石英粉%熒光光譜%定量檢測%對苯二甲痠
간자유기%석영분%형광광보%정량검측%대분이갑산
Hydroxyl radicals%Quartz power%Fluorescence spectrometry%Quantitative detection%Terephthalic acid
为了定量检测石英粉/磷酸盐缓冲溶液体系中极低浓度的羟自由基(· OH),依据对苯二甲酸(TA)在pH中性的缓冲溶液中与羟自由基反应生成唯一稳定且具有很强荧光特性的产物即2-羟基对苯二甲酸(HOTP),本文建立了滤液最大激发/发射波长EXmax/EMmax =316 nm/422 nm处的荧光强度与 HOTP浓度关系的标准曲线,通过检测石英粉与缓冲溶液作用之后滤液的荧光强度,从而间接测定了体系产生的· OH累积浓度。通过重复试验并分析五个不同实验条件下体系产生的· O H累积浓度,最小检出限达到1.59×10-10 mol · L -1,相对偏差为1.20%~7.89%,标准偏差为1.09×10-9~2.17×10-9 mol · L -1,相对标准偏差为3.5%~5.8%,说明该方法具有较高的精确度和较好的重复性。该方法可用于定量检测pH中性溶液中极低浓度的· OH ,与其他方法相比,具有明显的检测限低、成本低、灵敏度高、稳定性和重现性好等优势。
為瞭定量檢測石英粉/燐痠鹽緩遲溶液體繫中極低濃度的羥自由基(· OH),依據對苯二甲痠(TA)在pH中性的緩遲溶液中與羥自由基反應生成唯一穩定且具有很彊熒光特性的產物即2-羥基對苯二甲痠(HOTP),本文建立瞭濾液最大激髮/髮射波長EXmax/EMmax =316 nm/422 nm處的熒光彊度與 HOTP濃度關繫的標準麯線,通過檢測石英粉與緩遲溶液作用之後濾液的熒光彊度,從而間接測定瞭體繫產生的· OH纍積濃度。通過重複試驗併分析五箇不同實驗條件下體繫產生的· O H纍積濃度,最小檢齣限達到1.59×10-10 mol · L -1,相對偏差為1.20%~7.89%,標準偏差為1.09×10-9~2.17×10-9 mol · L -1,相對標準偏差為3.5%~5.8%,說明該方法具有較高的精確度和較好的重複性。該方法可用于定量檢測pH中性溶液中極低濃度的· OH ,與其他方法相比,具有明顯的檢測限低、成本低、靈敏度高、穩定性和重現性好等優勢。
위료정량검측석영분/린산염완충용액체계중겁저농도적간자유기(· OH),의거대분이갑산(TA)재pH중성적완충용액중여간자유기반응생성유일은정차구유흔강형광특성적산물즉2-간기대분이갑산(HOTP),본문건립료려액최대격발/발사파장EXmax/EMmax =316 nm/422 nm처적형광강도여 HOTP농도관계적표준곡선,통과검측석영분여완충용액작용지후려액적형광강도,종이간접측정료체계산생적· OH루적농도。통과중복시험병분석오개불동실험조건하체계산생적· O H루적농도,최소검출한체도1.59×10-10 mol · L -1,상대편차위1.20%~7.89%,표준편차위1.09×10-9~2.17×10-9 mol · L -1,상대표준편차위3.5%~5.8%,설명해방법구유교고적정학도화교호적중복성。해방법가용우정량검측pH중성용액중겁저농도적· OH ,여기타방법상비,구유명현적검측한저、성본저、령민도고、은정성화중현성호등우세。
Quartz powder would release radical hydroxyl in phosphate buffer solution .In order to detect the quantity of radical hydroxyl with a quite low concentration ,the present paper established a fluorescence method .According to the relationship be-tween the concentration of 2-hydroxyl of terephthalic acid (HOTP) and fluorescence intensity at the wavelength of EXmax/EMmax=316 nm/422 nm ,a working standard curve was constructed .Then through the filtrated fluorescence intensity obtained from the powder and solution system ,cumulative concentration of · OH can be measured indirectly .By repeating tests and analysis of five different experimental conditions of · OH cumulative concentration ,the minimum detection limit of the method reached 1.59 × 10-10 mol · L -1 ,with a relative deviation of 1.20% ~7.89% ,standard deviation was 1.09 × 10-9 ~2.17 × 10-9 mol · L -1 and the relative standard deviation was 3.5% ~5.8% .The method features high accuracy and good repeatability perform-ance .Compared to other quantitative studies ,this method might be applied to test radical hydroxy produced in pH neutral solu-tion systems .In addition ,it has apparent advantages such as low detection limit ,low cost ,higher sensitivity ,and better stabili-ty and reproducibility .That provides the means for the quantitative study of mixed systems consisting of quartz powder and phosphate buffered solution .