張威

摘 要:以Al-水楊基熒光酮-聚乙烯醇-土溫-60為顯色體系,用分光光度法測定聚乙烯中的微量鋁。在實驗的過程中需要對測量的條件進行考察。實驗結果表明波長560 nm處產生最大吸收。鋁量1.0~5.0μg/25 mL符合比爾定律,摩爾吸光系數ε=0.845×105 L/(mol·cm),得線性回歸方程是A= 0.08126×106 C +0.008637(C的單位mo1/L)。樣品中存在多種微量元素,它們對聚乙烯中鋁的測定存在干擾。用檸檬酸三鈉作掩蔽劑,消除了干擾離子。人工合成樣品的回收率在100.2%~100.5%,它們的平均回收率為100.3%,相對偏差為0.3%。對聚乙烯中鋁含量進行測定回收率在96.1%~102.5%,平均加標回收率是100.1%,其相對偏差RSD為1.8%。本文所用的方法選擇性好、準確度好、靈敏度高、實用性強。它是一種快速、有效測定聚乙烯中微量鋁的方法并且在實際應用中具有一定的意義和價值。
關 鍵 詞:水楊基熒光酮; 分光光度法;聚乙烯;鋁
中圖分類號:O 657 文獻標識碼: A 文章編號: 1671-0460(2015)07-1614-04
Determination of Trace Aluminum in
Polyethylene by Salicyl Fluorone Spectrophotometry
ZHANG Wei
(PetroChina Fushun Petrochemical Company Synthetic Detergent Factory, Liaoning Fushun 113004,China)
Abstract:Aluminum-salicyl fluoronl-PVA-TWeen-60 coloured system was used to determine trace aluminum in polyethylene by spectrophotometry.In the course of the experiment,the measuring conditions were studied.The experiment results indicate that the absorbance of the complex at 560 nm is the maximum absorption wavelength.The molarabsorption coefficient is 0.845×105 L/(mol·cm),linear range is 1.0~5.0 μg/25 mL.The regression line equation is A= 0.08126×106 C +0.008637(C,mol/L).There are amount of trace elements in the samples , such as Ti4+、 Cr6+、Mn7+、Cu2+、Ni2+、Fe3+、Zn 2+ and V5+ ,which can interfere determination of aluminum in polyethyle.The sodium citrate can be used as masking agent to mask interfering ions during the course of determination.The recovery rate of synthetic sample is 100.2%~100.5%. The average recovery rate is 100.3%. The relative standard deviation is 0.3%.The recovery rate of samples of aluminum in polyethylene is 96.1%~102.5%. The average recovery rate is 100.1%.The relative standard deviation is 1.8%. This analysis method has the characteristics of high selectivity,accuracy and sensitivity. It is a rapid and efficient method to determine aluminum in polyethylene.
Keywords: salicyl fluorone;spectrophotometry; polyethylene; aluminum
聚乙烯是乙烯的聚合物,是乙烯耗量最大的石油化工產品。高純度的乙烯,在特定的溫度,壓力和引發劑或催化劑存在的條件下,發生聚合反應生成聚乙烯。聚乙烯工業化以有60來年的歷史,聚乙烯現在是世界上產量最大,品種繁多的重要的合成樹脂之一。合成樹脂及塑料是20世紀的新興材料,聚乙烯由于物化性能優異,成型加工簡易,價格相對便宜,其應用已深入到國民經濟的各個部門和人民的日常生活中,成為產量和需求量最大的一類合成樹脂[1]。聚乙烯產品在加工成型過程中采用一氯二乙基鋁作為助催化劑,因此在聚乙烯的成品中會引入微量的鋁元素。……