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
A simple, total decomposition method for lead and other metals in paint has been developed. Complete decomposition is achieved through a combination of reagents over several digestive steps in a microwave oven. Results of analysis of several NIST paint SRMs show excellent recoveries ranging from 85.5 to 111%. Additionally, recoveries of a number of trace elements for two soil and one dust NIST SRM were also excellent.
Lead in paint continues to be a threat to children's health in cities across the United States, which means there is an ongoing need for testing and analysis of paint. This ongoing analytical effort and especially development of new methods continue to drive the need for diagnostic testing materials that provide the analytical challenges of real-world paints. To this end, 31 different types of paint test materials were developed and prepared. Preparation of the materials included development of lead-containing paint films yielding an overall relative standard error for one individual test sample being less than 10%. The 31 diagnostic test materials prepared with these paint films included two lead pigments; lead concentrations from nominally 0 to 2.0 mg lead/cm(2) (0 to 5% lead by weight); overlayers of both "lead-free," oil-based and water-based paints; Al, Ba, and Mg as potential chemical interferents; red and black potential color interferents; and substrates of wood, metal, masonry, and plaster. These materials challenge each step in method development and evaluation, including paint sample collection and preparation, lead extraction, and measurement of solubilized lead. When the materials were used to test performance of a new lead-in-paint testing method based on extraction using a rotor/stator method and measurement using turbidimetry, the results agreed to within ±20% of the expected lead values for 30 out of 31 of the diagnostic test materials, thereby demonstrating their levels of quality and utility.
The use of microwave energy to facilitate sample decomposition prior to elemental analysis is now receiving considerable attention. Both wet and dry digestions are achievable. When microwave energy is used in combination with acid mixtures in closed vessels, the combined pressure and rapid heating can reduce digestion times to a few minutes from hours or days that may be required for open beaker digestions. This savings in time and labor is significant and has prompted the Office of Solid Waste to evaluate this technology as a preparation tool for solid wastes. Of particular interest are used oils and other fuels slated for incineration, incinerator ash, and particulates from these processes. This study reports on the evaluation of a commercially available microwave oven sample preparation system for this application. The effect of sample preparation conditions, including the acid matrix, heating time, and pressure, were evaluated for fifteen toxic or hazardous elements in particulates, ashes oils, and oil fuels. Analyses were carried out by inductively coupled plasma emission spectroscopy.
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