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测定干漆酸提取物中铅的现场浊度法。

Field turbidity method for the determination of lead in acid extracts of dried paint.

作者信息

Studabaker William B, McCombs Michelle, Sorrell Kristen, Salmons Cynthia, Brown G Gordon, Binstock David, Gutknecht William F, Harper Sharon L

机构信息

RTI International, P.O. Box 12194, Research Triangle Park, NC 27709, USA.

出版信息

J Environ Monit. 2010 Jul 8;12(7):1393-403. doi: 10.1039/c000888e. Epub 2010 Apr 16.

Abstract

Lead, which can be found in old paint, soil, and dust, has been clearly shown to have adverse health effects on the neurological systems of both children and adults. As part of an ongoing effort to reduce childhood lead poisoning, the US Environmental Protection Agency promulgated the Lead Renovation, Repair, and Painting Program (RRP) rule requiring that paint in target housing built prior to 1978 be tested for lead before any renovation, repair, or painting activities are initiated. This rule has led to a need for a rapid, relatively easy, and an inexpensive method for measuring lead in paint. This paper presents a new method for measuring lead extracted from paint that is based on turbidimetry. This method is applicable to paint that has been collected from a surface and extracted into 25% (v/v) of nitric acid. An aliquot of the filtered extract is mixed with an aliquot of solid potassium molybdate in 1 M ammonium acetate to form a turbid suspension of lead molybdate. The lead concentration is determined using a portable turbidity meter. This turbidimetric method has a response of approximately 0.9 NTU per microg lead per mL extract, with a range of 1-1000 Nephelometric Turbidity Units (NTUs). Precision at a concentration corresponding to the EPA-mandated decision point of 1 mg of lead per cm(2) is <2%. This method is insensitive to the presence of other metals common to paint, including Ba(2+), Ca(2+), Mg(2+), Fe(3+), Co(2+), Cu(2+), and Cd(2+), at concentrations of 10 mg mL(-1) or to Zn(2+) at 50 mg mL(-1). Analysis of 14 samples from six reference materials with lead concentrations near 1 mg cm(-2) yielded a correlation to inductively coupled plasma-atomic emission spectroscopy (ICP-AES) analysis of 0.97, with an average bias of 2.8%. Twenty-four sets of either 6 or 10 paint samples each were collected from different locations in old houses, a hospital, tobacco factory, and power station. Half of each set was analyzed using rotor/stator-25% (v/v) nitric acid extraction with measurement using the new turbidimetric method, and the other half was analyzed using microwave extraction and measurement by ICP-AES. The average relative percent difference between the turbidimetric method and the ICP-AES method for the 24 sets measured as milligrams of lead per cm(2) is -0.63 +/- 32.5%; the mean difference is -2.1 +/- 7.0 mg lead per cm(2). Non-parametric and parametric statistical tests on these data showed no difference in the results for the two procedures. At the federal regulated level of 1 mg of lead per cm(2) paint, this turbidimetric method meets the performance requirements for EPA's National Lead Laboratory Accreditation Program (NLLAP) of accuracy within +/-20% and has the potential to meet the performance specifications of EPA's RRP rule.

摘要

旧油漆、土壤和灰尘中含有的铅已被明确证实会对儿童和成人的神经系统产生不良健康影响。作为减少儿童铅中毒持续努力的一部分,美国环境保护局颁布了《铅翻新、修复和涂漆计划》(RRP)规则,要求在1978年以前建造的目标房屋中,在开始任何翻新、修复或涂漆活动之前对油漆进行铅含量检测。该规则导致需要一种快速、相对简便且廉价的油漆铅含量测量方法。本文介绍了一种基于比浊法测量从油漆中提取的铅的新方法。该方法适用于从表面收集并萃取到25%(v/v)硝酸中的油漆。将过滤后的萃取液的一份等分试样与1M醋酸铵中的固体钼酸钾的一份等分试样混合,形成钼酸铅的浑浊悬浮液。使用便携式浊度计测定铅浓度。这种比浊法的响应约为每毫升萃取液中每微克铅0.9 NTU,范围为1 - 1000 Nephelometric Turbidity Units(NTU)。在对应于美国环境保护局规定的决策点每平方厘米1毫克铅的浓度下,精密度小于2%。该方法对油漆中常见的其他金属(包括浓度为10 mg mL⁻¹的Ba²⁺、Ca²⁺、Mg²⁺、Fe³⁺、Co²⁺、Cu²⁺和Cd²⁺或浓度为50 mg mL⁻¹的Zn²⁺)的存在不敏感。对六种参考物质中铅浓度接近每平方厘米1毫克的14个样品进行分析,与电感耦合等离子体原子发射光谱法(ICP - AES)分析的相关性为0.97,平均偏差为2.8%。从老房子、医院、烟草厂和发电站的不同位置收集了24组每组6个或10个油漆样品。每组中的一半使用转子/定子 - 25%(v/v)硝酸萃取并采用新的比浊法进行测量,另一半使用微波萃取并通过ICP - AES进行测量。以每平方厘米铅毫克数衡量,比浊法和ICP - AES法对这24组测量结果的平均相对百分差异为 - 0.63 ± 32.5%;平均差异为每平方厘米 - 2.1 ± 7.0毫克铅。对这些数据进行的非参数和参数统计检验表明,两种方法的结果没有差异。在联邦规定的每平方厘米油漆1毫克铅的水平下,这种比浊法符合美国环境保护局国家铅实验室认可计划(NLLAP)的性能要求,准确度在±20%以内,并且有可能满足美国环境保护局RRP规则的性能规范。

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