摘要
本文报道了荣光试剂3-苯基-5-苯甲酰基-2-疏代-4-噻唑啉酮(PBTT)的合成。产品经拉层桥提纯,用元素分析、IR、1HNMR和MS确证了其结构;研究了它的荧光性质。在PH5.6时,与痕量镜(Ⅲ)形成络合物。且在λex/λem=305nm/405nm产生强荧光。测定了人工合成样品中的铥,结果比较满意。
A new fluorescent reagent 3-phenyl-5-benzoyl-2-thioxo-4-thiazolinone (PBTT) had been prepared as follows. 0.014 mol 3-phenyl-2-thioxo-4-thiazolino (PTT) in ethanol solution was mixed with Ca (OH)2 and 0.02 mol benzoyl chloride, reacted for 3 h, then acidified. filtered and recrystallized, giving out the product. It was purified using coIumn adsorption chromatography. Its constitution has been confirmed by elemental analysis, IR, HNMR and MS. in potassium hydrogen phthalate-NaOH (pH = 5. 6) buffer solution, the reagent reacts with trace thulium (Ⅲ) to form a complex possessing an intensive florescence at λex/λem= 305 nm/405 nm. The fluorescence intensity has a linear relationship with the concentration of thulium(Ⅱ) in the range of 1.184×10-8-4. 72×10-7 mol/L with a detection limit of 2. 368×10-9 mol/L.Thulium in spiked sample was determined with good result.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
1996年第4期430-432,共3页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金
本校青年基金
关键词
荧光分析
苯基
苯甲酰基
硫代
噻唑啉酮
铥
PBTT
Fluorescence analysis, 3-phenyl-5-benzoyl-2-thioxo-4-thiazolinone,thulium,-reagent synthesis