Investigations of a new sample compartment assembly for low-temperature and room-temperature solid substrate phosphorimetry.
Investigations of a new sample compartment assembly for low-temperature and room-temperature solid substrate phosphorimetry.
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研究用于低温和室温固体基质磷光测定的新型样品室组件。
DOI：
10.1021/ac00284a016
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发表时间：
1985
影响因子：
7.4
通讯作者：
Winefordner,JD
中科院分区：
文献类型：
--
作者：
Scharf,G;Smith,BW;Winefordner,JD
描述了一种新型样品室，用于对固定在固体基质中的样品进行室温（25℃）和低温（-65℃）磷光测定（和荧光测定）。为 Perkln-Elmer LS-5 荧光计设计的样品室组件包含四个样品和空白位置，可以方便地从样品光谱中减去空白。给出了在存在和不存在强碱和碘化物的情况下，几种固体基质（包括各种滤纸和薄层色谱板）的激发和发射磷光背景光谱和磷光寿命。对两种模型化合物 6-羧酸和对氨基苯甲酸进行了类似的研究。背景随着重原子的存在和低温而增加，并且背景可能是磷光体组合的结果。 6-屈甲酸 (6-CHRA) 和对氨基苯甲酸 (PABA) 的室温磷光 (RTP) 检测限为 0.2 ng，5 pg/mL 浓度的相对标准偏差百分比约为 10%，分析校准曲线呈线性。固体表面室温磷光 (RTP) 最近已发展为一种用于定量测定多种有机化合物的分析技术。 （1-23）。已经发表了几篇评论（24-29）。 Parker 等人(25, 26) 回顾了 RTP 的分析和物理方面。在最近出版的一本专着中，Vo-Dinh (29) 对 RTP 进行了广泛的调查。在多项研究 (4、9、12、30) 中，发现惰性、干燥的气氛对于在室温下产生强烈且稳定的磷光信号至关重要。每个样品报告的干燥时间在几分钟到 2 小时之间 (22)。因此，干燥阶段可能相当耗时。
A novel sample compartment for use in room-temperature (25 C) and in low-temperature (-65 C) phosphorimetry (and fluorometry) of samples held In solid substrates is described. The sample compartment assembly designed for the Perkln-Elmer LS-5 fluorometer contains four positions for samples and blank and allows convenient subtraction of the blank from the sample spectra. Excitation and emission phosphores-cence background spectra and phosphorescence lifetimes of several solid substrates, including various filter papers and a TLC plate, In the presence and absence of strong base and Iodide are given. Similar studies were performed with two model compounds 6-chrysenecarboxyllc acid and p-amlnobenzolc acid. The background Increased with the presence of heavy atom and at low temperatures, and the background Is likely a result of a combination of phosphors. The room-temperature phosphorescence (RTP) detection limits for 6-chrysenecarboxylic acid (6-CHRA) and p-amlnobenzoic acid (PABA) were 0.2 ng, the percent relative standard deviations for 5 pg/mL concentrations were about 10%, and the ana-lytical calibration curves were linear.Solid surface room-temperature phosphorescence (RTP) has recently been developed as an analytical technique for quantitative determination of a variety of organic compounds (1-23). Several reviews have been published (24-29). Parker et al.(25, 26) have reviewed the analytical and physical aspects of RTP. In a recently published monograph, Vo-Dinh (29) has given an extensive survey of RTP. In several studies (4, 9, 12, 30), it was found that an inert, dry atmosphere is essential for producing intense and stable phosphorescence signals at room temperature. The drying period reported for each sample was in the range of a few minutes to 2 h (22). Therefore, the drying stage can be fairly time-consuming.