Chronic exposure of children to lead can result in permanent physiological impairment. In adults, it can cause irritability, poor muscle coordination, and nerve damage to the sense organs and nerves controlling the body. Surfaces coated with lead-containing paints are potential sources of exposure to lead. In April 2008, the U.S. Environmental Protection Agency (EPA) finalized new requirements that would reduce exposure to lead hazards created by renovation, repair, and painting activities, which disturb lead-based paint. On-site, inexpensive identification of lead-based paint is required. Two steps have been taken to meet this challenge. First, this paper presents a new, highly efficient method for paint collection that is based on the use of a modified wood drill bit. Second, this paper presents a novel, one-step approach for quantitatively grinding and extracting lead from paint samples for subsequent lead determination. This latter method is based on the use of a high-revolutions per minute rotor with stator to break up the paint into approximately 50 micron-size particles. Nitric acid (25%, v/v) is used to extract the lead in <3 minutes. Recoveries are consistently >95% for real-world paints, National Institute of Standards and Technology's standard reference materials, and audit samples from the American Industrial Hygiene Association's Environmental Lead Proficiency Analytical Testing Program. This quantitative extraction procedure, when paired with quantitative paint sample collection and lead determination, may enable the development of a lead paint test kit that will meet the specifications of the final EPA rule.
A microwave-assisted method for preparing samples for determination of elements In solid waste has been developed (draft EPA Method 3051). Validation of the sample preparation method was performed through a collaborative study to determine its precision and accuracy. Fifteen independent laboratories digested 4 National Institute of Standards and Technology (NIST) standard reference materials (SRMs) and 1 solvent recovery waste in duplicate. Digestates were analyzed for 19 elements using inductively coupled plasma (ICP) emission spectroscopy. The precision and bias of the method were evaluated. When compared with an open vessel hot-plate digestion method (SW-846 Method 3050), the microwave method produced similar analytical results with better overall precision. Bias for the 1 sample that allowed this determination was found to be excellent.
The techniques which are typically used to prepare RCRA wastes for analysis for metals and other elements are generally relatively time consuming, requiring several hours to several days to complete. They also often involve the use of acid digestions and thermal decomposition steps which may result in analyte losses, incomplete recoveries, or sample contamination. These limitations are well known to the analytical community and to the end users of these data in EPA, States, and industry. The resulting inefficiency of these techniques reduces laboratory sample throughput, drives up the cost of analytical testing, and impedes decision making. Given these concerns, the OSW Methods Section is interested in developing cost effective sample preparation techniques for metals and other elements in environmental and process waste samples. Once developed, these techniques can then be written as methods for inclusion in Test Methods for Evaluation of Solid Waste SW-846 and made available to the user community. This paper reports on the evaluation of a microwave assisted sample preparation method for determining elements in solid waste. The Method was evaluated for microwave digestion of sediments, sludges, soils, and oils.
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.
A major aspect of lead hazard control is the evaluation of soil lead hazards around housing coated with lead-based paint. The use of field-portable X-ray fluorescence (FPXRF) to do detailed surveying, with limited laboratory confirmation, can provide lead measurements in soil (especially for planning abatement activities) in a far more cost-efficient and timely manner than laboratory analysis. To date, one obstacle to the acceptance of FPXRF as an approved method of measuring lead in soil has been a lack of correspondence between field and laboratory results. In order to minimize the differences between field and laboratory results, RTI International (RTI) has developed a new protocol for field drying and sieving soil samples for field measurement by FPXRF. To evaluate this new protocol, composite samples were collected in the field following both U.S. Department of Housing and Urban Development (HUD) guidelines and ASTM International (ASTM) protocols, measured after drying by FPXRF, and returned to the laboratory for confirmatory inductively coupled plasma atomic emission spectroscopy (ICP-AES) analysis. Evaluation of study data from several diverse sites revealed no statistical difference between paired FPXRF and ICP-AES measurements using the new method. O
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