Wink O, Schack F
Clariant GmbH, Werk Cassella-Offenbach, Analytical and Physical Department, Frankfurt am Main, Germany.
Analyst. 2000 Oct;125(10):1745-50. doi: 10.1039/b001950j.
Superabsorbent polyacrylates (SAPs) have been used in the hygiene industry for many years. A derivatization and analytical method was developed for routine analysis of trace levels of SAP dust in workplace atmospheres. In comparison with existing methods, which are based on the sodium content or the ion exchange properties of the polymer, this method is more specific. It has the advantage of not being influenced by any sodium containing contaminants. Air samples are collected on Teflon filters using air monitoring sampling cassettes. The filters are subsequently placed in quartz vials and a reaction mixture containing hydrochloric acid in ethanol is added. The hydrochloric acid-ethanol solution, when heated, converts the carboxylic acid groups on the backbone of the insoluble polyacrylate into ethyl esters. After reaction, the excess of ethanol and hydrochloric acid is completely removed under vacuum. The sample is then treated with aqueous sodium hydroxide at 80 degrees C to release the bound ethanol. The solution is analyzed by HPLC on an anion exclusion stationary phase using dilute perchloric acid as mobile phase. Ethanol is identified and quantified with a pulsed electrochemical detector. Several environmental samples in addition to laboratory spiked samples were successfully analyzed with this technique. Recoveries averaged > 85% for spiked blank filters at levels from 5 to 50 micrograms per filter with relative standard deviations up to 7%. The instrument's limit of detection (LOD) for ethanol was 0.1 mg l-1. The LOD for derivatization and analysis corresponds to 3 micrograms of SAP per filter (assuming an esterification factor of 0.30 microgram of ethanol per microgram of SAP).
高吸水性聚丙烯酸盐(SAPs)已在卫生行业中使用多年。开发了一种衍生化和分析方法,用于对工作场所空气中痕量水平的SAP粉尘进行常规分析。与基于聚合物钠含量或离子交换特性的现有方法相比,该方法更具特异性。它具有不受任何含钠污染物影响的优点。使用空气监测采样盒在聚四氟乙烯滤膜上采集空气样品。随后将滤膜置于石英小瓶中,并加入含有盐酸乙醇溶液的反应混合物。加热时,盐酸乙醇溶液将不溶性聚丙烯酸酯主链上的羧酸基团转化为乙酯。反应后,在真空下完全除去过量的乙醇和盐酸。然后将样品在80℃下用氢氧化钠水溶液处理,以释放结合的乙醇。使用稀高氯酸作为流动相,在阴离子排斥固定相上通过HPLC对溶液进行分析。用脉冲电化学检测器对乙醇进行鉴定和定量。除实验室加标样品外,还使用该技术成功分析了几个环境样品。对于每片滤膜添加量为5至50微克的加标空白滤膜,回收率平均> 85%,相对标准偏差高达7%。仪器对乙醇的检测限(LOD)为0.1 mg l-1。衍生化和分析的LOD相当于每片滤膜3微克的SAP(假设酯化系数为每微克SAP 0.30微克乙醇)。