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Improved Purge-Trap and GC/MS/MS Techniques for the Trace-Level Determination of 1,4-Dioxane in Water 改进的吹扫捕集器和GC/MS/MS技术测定水中痕量1,4-二恶烷
发布日期: 2002-11-01
1,4-二恶烷通常存在于处理过的废水和垃圾填埋场中 由于广泛使用1,4-二氧六环作为垃圾处理的稳定剂而产生的渗滤液 氯化溶剂,如1,1,1-三氯乙烷(TCA)和 除草剂中某些表面活性剂化合物中的污染物。也是 各种个人护理产品,如洗发水、液体肥皂、, 含有防晒霜、保湿乳液、婴儿乳液和护发液 1,4-二氧六环,含量在百万分之3到100之间。更多 据报道,1,4-二恶烷的出现和分布在几个国家 包括加利福尼亚州在内的各州都对可靠和快速的分析系统感兴趣 检测亚ppb水平1,4-二恶烷的方法有所增加。 最近,美国环境保护局(USEPA)将1,4-二恶烷列为一种可能的化合物 人类致癌物,已在特定的地面和表面检测到 水域。水系统中1,4-二恶烷的发现促使 需要对饮用水中的化合物进行广泛监测。但是 目前可用的方法具有10至50 ug/L的高检测限。高可报告检测限是提取不良的结果 化合物的效率和挥发性。 Orange County Water District(OCWD)实验室已审查 目前可用的同位素稀释方法和吹扫捕集器技术 使用GC/MS。大多数实验室都采用同位素稀释法 方法,但同位素稀释法涉及劳动密集型液体- 对每个样品进行液体萃取和100-200毫升二氯甲烷。 由于1,4的净化效率低,水溶性无限大- 二恶烷,净化捕集器技术的检测限高出100倍 比美国环保局方法524的其他可净化化合物。 2.最新进展 OCWD实验室已开始对吹扫捕集器进行一系列修改 美国环保局方法524.2的提取和仪器化,以提高 测定水中1,4-二氧六环的灵敏度和再现性。 为了提高吹扫效率,吹扫时间已增加到20分钟 从11分钟增加到10分钟,而不是将吹扫流量增加到40分钟 毫升/分钟,以防止重基质样品起泡。也是 不同类型的捕集器含有更多的carbopack(TM),可以提高效率 1,4-二氧六环峰的形状和响应。对于 在仪器方面,GC/MS/MS已被用于回收离子 从GC/MS中去除背景离子以帮助 从废水样本中识别低ppb水平的1,4-二恶烷。 改进后的方法检测限为0.2 ppb 无需人工,仅使用25毫升的 样品与同位素稀释提取的1000 ml样品进行比较 方法吹扫捕集器与同位素稀释法的分离试验 对饮用水和废水表现出良好的相关性 样品。改进的吹扫捕集器和GC/MS/MS技术将 节省劳动力,100%无溶剂萃取,快速 周转时间长,精度高,对同位素的灵敏度相当 稀释法。 包括6个参考文献、表格。
1,4-dioxane is commonly found in treated wastewater effluent and landfill leachate due to the extensive use of 1,4-dioxane as a stabilizer for chlorinated solvents such as 1,1,1-trichloroethane (TCA) and a contaminant in some surfactant compounds used in herbicides. Also a variety of personal care products such as shampoo, liquid soaps, sunscreens, moisturing lotions, baby lotions, and hair lotions contained 1,4-dioxane with levels ranging from 3 to 100 parts per million. As more occurrences and distributions of 1,4-dioxane were reported in several states including California, the interest in a reliable and fast analytical method to detect sub ppb levels 1,4-dioxane has increased. Recently, 1,4-dioxane, which the US Environmental Protection Agency (USEPA) classifies as a B2 probable human carcinogen, has been detected in the specific ground and surface waters. The findings of 1,4-dioxane in the water systems prompted the need of extensive monitoring of the compound in the drinking water. But the currently available methods have high detection limits of 10 to 50 ug/L. The high reportable detection limits are the results of poor extraction efficiency and volatile nature of the compound. The Orange County Water District (OCWD) Laboratory has reviewed currently available isotope dilution methods and purge-trap techniques using the GC/MS. Most laboratories are applying the isotope dilution method, but the isotope dilution method involves labor-intensive liquid- liquid extraction and 100-200 ml of methylene chloride for each sample. Due to the poor purging efficiency and infinite water solubility of 1,4- dioxane, the detection limit of purge-trap techniques is 100 times higher than the other purgeable compounds with USEPA method 524.2. The OCWD lab has initiated a series of modifications for the purge-trap extraction and instrumentation of USEPA method 524.2 to improve the sensitivity and reproducibility for the determination of 1,4-dioxane in water. To improve purging efficiency, the purge time has been increased to 20 minutes from 11 minutes instead of increasing the purge flow of 40 ml/minute to prevent foaming of the heavy matrix samples. Also a different type of trap, which contains more carbopack(TM), could improve the response and the shape of 1,4-dioxane peak. For the instrumentation, the GC/MS/MS has been applied to retrieve the ions from GC/MS, which removed the background ions to help the identification of low ppb levels of 1,4-dioxane from wastewater samples. The improved method generated the method detection limit of 0.2 ppb and very reproducible data without manual labor and using only 25 ml of sample compared to the 1000 ml-sample extraction of the isotope dilution method. The split test between purge-trap and isotope dilution method showed the excellent correlation for drinking water and wastewater samples. The improved purge-trap and GC/MS/MS techniques will be very resourceful in saving labor and 100% solvent less extraction with fast turn-around time, high precision, and comparable sensitivity to the isotope dilution method. Includes 6 references, tables.
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发布单位或类别: 美国-美国给水工程协会
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