冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2015年
6期
53-56
,共4页
荧光光度法%钪%钙黄绿素%Triton X-100%粉煤灰
熒光光度法%鈧%鈣黃綠素%Triton X-100%粉煤灰
형광광도법%항%개황록소%Triton X-100%분매회
fluorescence spectrophotometry%scandium%calcein%Triton X-100%fly ash
研究了钙黄绿素与钪Ⅲ的荧光反应。实验表明,在pH 8.5 NH3·H2 O-NH4 Cl缓冲溶液和表面活性剂Triton X-100的存在下,痕量钪Ⅲ能和钙黄绿素反应生成络合物,使体系的荧光强度显著增强,激发波长和发射波长分别为495 nm和520 nm,钪Ⅲ的质量浓度在0.021~1.80μg/mL范围内与荧光强度差值(ΔF )的线性关系良好,线性回归方程为:ΔF=3.431+2.473ρ(μg/mL),相关系数r=0.9981,检出限为0.021μg/mL。干扰试验表明:粉煤灰样品中的钪经1-苯基-3-甲基-4-苯甲酰-5-砒唑酮(PMBP)-甲苯萃取分离后,大多数常见离子不干扰测定。方法应用于粉煤灰中痕量钪的测定,结果与电感耦合等离子体原子发射光谱法( ICP-AES)相符,相对标准偏差(RSD,n=6)为0.57%~1.0%,加标回收率在98%~105%之间。
研究瞭鈣黃綠素與鈧Ⅲ的熒光反應。實驗錶明,在pH 8.5 NH3·H2 O-NH4 Cl緩遲溶液和錶麵活性劑Triton X-100的存在下,痕量鈧Ⅲ能和鈣黃綠素反應生成絡閤物,使體繫的熒光彊度顯著增彊,激髮波長和髮射波長分彆為495 nm和520 nm,鈧Ⅲ的質量濃度在0.021~1.80μg/mL範圍內與熒光彊度差值(ΔF )的線性關繫良好,線性迴歸方程為:ΔF=3.431+2.473ρ(μg/mL),相關繫數r=0.9981,檢齣限為0.021μg/mL。榦擾試驗錶明:粉煤灰樣品中的鈧經1-苯基-3-甲基-4-苯甲酰-5-砒唑酮(PMBP)-甲苯萃取分離後,大多數常見離子不榦擾測定。方法應用于粉煤灰中痕量鈧的測定,結果與電感耦閤等離子體原子髮射光譜法( ICP-AES)相符,相對標準偏差(RSD,n=6)為0.57%~1.0%,加標迴收率在98%~105%之間。
연구료개황록소여항Ⅲ적형광반응。실험표명,재pH 8.5 NH3·H2 O-NH4 Cl완충용액화표면활성제Triton X-100적존재하,흔량항Ⅲ능화개황록소반응생성락합물,사체계적형광강도현저증강,격발파장화발사파장분별위495 nm화520 nm,항Ⅲ적질량농도재0.021~1.80μg/mL범위내여형광강도차치(ΔF )적선성관계량호,선성회귀방정위:ΔF=3.431+2.473ρ(μg/mL),상관계수r=0.9981,검출한위0.021μg/mL。간우시험표명:분매회양품중적항경1-분기-3-갑기-4-분갑선-5-비서동(PMBP)-갑분췌취분리후,대다수상견리자불간우측정。방법응용우분매회중흔량항적측정,결과여전감우합등리자체원자발사광보법( ICP-AES)상부,상대표준편차(RSD,n=6)위0.57%~1.0%,가표회수솔재98%~105%지간。
The fluorescence reaction between calcein and scandiumⅢ was studied. The results showed that trace scandiumⅢ ions could react with calcein to form complex in NH3 ·H2 O-NH4 Cl buffer solution at pH 8. 5 in pres-ence of surfactant Triton X-100, and the fluorescence intensity of this system was enhanced significantly. The exci-tation wavelength and emission wavelength was 495 nm and 520 nm, respectively. The content of scandiumⅢ in range of 0. 021-1. 80 μg/mL exhibited good linearity to its fluorescence intensity difference (ΔF). The equation of linear regression wasΔF=3. 431+2. 473ρ(μg/mL) with correlation coefficient of r=0. 998 1. The detection limit was 0. 021 μg/mL. The interference tests indicated that most common ions did not interfere with the determination after scandium in fly ash sample was extracted and separated with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP)-methylbenzene. The proposed method was applied to determination of trace scandium in fly ash samples. The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry ( ICP-AES). The relative standard deviation (RSD, n=6) was 0. 57%-1. 0%. The recoveries were between 98% and 105%.