Source: UNIV OF WISCONSIN submitted to
IMPROVING SOIL TESTING METHODS FOR LEAD CONTAMINATED SOILS
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
TERMINATED
Funding Source
Reporting Frequency
Annual
Accession No.
1006547
Grant No.
(N/A)
Project No.
WIS01871
Proposal No.
(N/A)
Multistate No.
(N/A)
Program Code
(N/A)
Project Start Date
Oct 1, 2015
Project End Date
Sep 30, 2018
Grant Year
(N/A)
Project Director
Soldat, DO, JA.
Recipient Organization
UNIV OF WISCONSIN
21 N PARK ST STE 6401
MADISON,WI 53715-1218
Performing Department
Soil Science
Non Technical Summary
Lead (Pb) is a common, persistent contaminant of soils. Exposure to lead is hazardous to humans, and associated with a large number of negative health impacts, many of which affect neurological function and development. Ingestion of inhalation of soil lead is a primary source of lead exposure. Lead contamination (from leaded gasoline emissions, lead paint, lead shot, etc.) is ubiquitous in urban areas, but also commonly found at elevated levels in rural areas. Despite the widespread nature of lead contamination, evaluation of lead hazard is hindered by the lack of an inexpensive, accurate, and widely available test for soil lead. Accurate soil tests for bioavailable lead exist, but these tests are complicated to perform and cost prohibitive to the general public. Fortunately, there exists a great deal of soil testing infrastructure across the US already employing methods designed to estimate soil nutrient bioavailability to plants. The primary objective of this research is to evaluate these existing soil nutrient tests (along with some novel methods) for their ability to extract bioavailable forms of lead. An expected outcome will be that soil testing laboratories, such as the University of Wisconsin Soil and Plant Analysis Laboratory will be able to provide more accurate soil lead testing results and interpretations leading to increased evaluation and mitigation of soil lead hazard by the general public. This study will not seek to establish the actual bioavailability of lead minerals in soil; rather it seeks to find correlations with simpler and cheaper soil testing methods to the standard method developed to correlate with in-vivo bioavailability studies.
Animal Health Component
0%
Research Effort Categories
Basic
15%
Applied
75%
Developmental
10%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
1330110204025%
1010110204025%
7110110204025%
7230110204025%
Goals / Objectives
The overall goal of this project is to help soil testing laboratories be able to provide more accurate soil lead testing results and interpretations leading to increased evaluation and mitigation of soil lead hazard by the general public.This primary objective of this research is to evaluate several existing soil nutrient tests (along with some novel methods) for their ability to extract bioavailable forms of lead.
Project Methods
This project seeks to build upon the momentum of a current project called "Growing Health Soils for Heathy Communities (GHSHC)" being conducted in Milwaukee, WI. The objectives of that research project are to 1) demonstrate the effectiveness of soil and landscape interventions in reducing total lead, and 2) expand environmental health literacy education and access to soil testing. However, the GHSHC project does not attempt to characterize the chemical forms of lead in the soil or attempt to evaluate estimated changes in bioavailability. The proposed research seeks to further characterize the contaminated soil samples collected from the Lindsey Heights and KK River neighborhoods during the GHSHC project. The residents are currently being recruited by project leaders and soil sampling will occur under the budget of the GHSHC project with 50 samples being collected during the 2015 growing season and another 50 collected during the 2016 growing season. A pilot study found the majority of soils in these neighborhoods to be slightly alkaline with pH values ranging from 7.6 - 8.2. Total lead concentrations ranged from 7 - 3200 mg/kg which will be sufficient for establishing correlations among the soil testing methods we plan to evaluate.Upon receipt of the soils, each sample will be split in half with one half receiving a phosphate treatment to induce formation of lead-phosphate minerals with low bioavailability; the other half of the sample will remain un-amended. The phosphate treated soils will receive phosphoric acid at a phosphorus: lead molar ratio of 5: 1 based on the total lead content of the soil as determined by EPA 3050. The phosphate amended soils will be kept at 80% of field moisture holding capacity at room temperature for 14 days. After 14 days, the pH will be adjusted using calcium oxide to return the soil to its original pH and the allowed to equilibrate for another 14 days before being allowed to air dry and then oven dried at 40°C. Previous research has shown this method of phosphate addition to be an effective way to rapidly shift the bioavailability of lead in soils (Scheckel and Ryan, 2004).Soil lead will be characterized using the standard EPA method for total lead (EPA 3050), conventional soil nutrient methods, modified soil nutrient methods, and in-vitro bioavailability methods. The EPA 3050 method is the current regulatory standard used for soil lead assessment in the US. It extracts all lead in a soil sample regardless of chemical form. The following methods all extract a portion of the soil and are hoped to better represent bioavailability.Bioavailability Methods:In-vivo testing using swine exposed to contaminated soil is the gold standard for estimating the bioavailability of lead to humans. However, these methods are expensive at approximately $30,000 per soil sample (Zia et al., 2011). Therefore, in-vitro chemical extraction methods have been developed which correlate with the in-vivo bioavailability. One of the first of such tests that found wide use is called the Physiologically-Based Extraction Test (PBET), which employs a simulated gastric solution at body temperature with mixing and other parameters set to mimic the human digestive tract (Ruby et al., 1999). The USEPA follows a modified PBET test which was found to be well correlated with soil lead bioavailability fed to swine (Drexler and Brattin, 2007).While in-vitro bioavailability tests can be performed for significantly lower cost than in-vivo testing, they remain essentially inaccessible to the general public. Therefore, there is a great need to develop an even simpler and less expensive test that is reproducible and can accurately correlate with bioavailability.The in-vitro extraction solution will consist of 0.4 M glycine adjusted to pH 2.5 with HCl. One gram of soil will be added to the HDPE bottles and 100 mL of extraction fluid added. The extractor is turned on and the solutions will be rotated end-over-end at 30 rotations per minute for 1 hour. Immediately following extraction, the pH of the extraction solution will be measured. If the pH differs by more than 0.5 pH units, the extraction will be re-run and the pH will be monitored at 5, 10 ,15, and 30 minutes into the extraction. If the pH differs by more than 0.5 pH units the solution will be adjusted drop wise with HCl. After a successful extraction (with appropriate pH), the solution will be filtered through a 0.45 µm cellulose acetate disk filter and stored at 4 °C for lead analysis via ICP-AES.Conventional and Modified Soil Nutrient Methods: Conventional soil nutrient methods are commonly performed by soil testing labs to provide information on soil nutrient status to farmers and gardeners for a cost of $10 - $20 per sample. They are designed to extract a small fraction of the total nutrients in the soil - called labile, plant available, or bioavailable nutrients. Most of these chemical tests were developed in the early to mid-1900s, and consist of dilute acid or acids (pH 1.2 - 2.5) and short extraction times (5 minutes). While the Drexler and Brattin method attempts to precisely quantify the total bioavailable lead, an effective test need only correlate well with the Drexler and Brattin. Because soil nutrient tests are already conducted widely used across the US, if one could be identified that correlates well with the Drexler and Brattin (2007) bioavailability method, the barriers to more accurate soil lead hazard would be decreased resulting in an increase in knowledge of soil lead hazard by farmers, farm workers, and the general public. In this research we propose to evaluate how the lead extracted by four very commonly used soil nutrient tests compares to the standard in-vitro bioavailability test of Drexler and Brattin (2007) as modified by Zia et al. (2011). We also propose to evaluate a small modification of the Mehlich-3 test based on previous findings in the literature which are described below.The most widely used soil nutrient test in Wisconsin is the Bray P-1 (Bray and Kurtz, 1945). It works well for extracting phosphorus on slightly acidic to slightly alkaline soils. The method involves shaking 2 g of soil in 20 mL of the extracting solution (pH 2.6, 0.025 M HCl in 0.03 M NH4F) for five minutes at room temperature at 200 cycles/minute. The Mehlich-1 test (Mehlich, 1953) is commonly used to assess the plant available nutrient status of soils in the Southeastern US which tend to be lower in organic matter with lower pH than Midwestern soils. However, the Mehlich-1 extraction solution contains 0.0125 M H2SO4 and 0.05 M HCl and its acidic nature (pH 1.2) may be useful for simulating gastric release of lead from soil, and is therefore deserving of evaluation. The Mehlich-3 was developed to effectively assess soil nutrient status across a broad spectrum of soils. Because of this, it is commonly used across the US and Canada. The Mehlich-3 is the most complex of the soil nutrient tests and contains acetic acid, ammonium nitrate, ammonium fluoride, nitric acid and EDTA. Finally, the DTPA extraction for micronutrients in soil will be evaluated (Lindsay and Norvell, 1978) against the Drexler and Brattin method for estimating lead bioavailability. This test was developed to extract Cu, Fe, Mn, and Zn from neutral and calcareous soils via chelation with 0.005 M DTPA adjusted to pH 7.3. This test has promise because it was developed to address the over-estimation of micronutrients by acidic extracts and is commonly employed at every major soil testing laboratory in the US.

Progress 10/01/15 to 09/30/18

Outputs
Target Audience:The target audiences for this work include people living and gardening in areas with lead contaminated soils, policy makers, soil testing laboratories, outreach specialists, and other scientists. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?This project helped train a graduate student in the scientific method and process. She gained considerable experience and skill in soil test extractions, analytical laboratory methods, data analysis and interpretation, and oral and written communication of results. The project also trained three undergraduate students who helped with the laboratory work. The primary graduate student on this project was offered and accepted a position with the USEPA to remediate and evaluate lead contaminated soils. In addition, an undergraduate student was also trained as part of this project. Based on that experience, the undergraduate decided to enroll in graduate school to continue studying Pb contaminated soils. How have the results been disseminated to communities of interest?We presented our results to scientists on several occasions during the grant period including several presentations at two Annual Meetings of the Soil Science Society of America and another at the Society of Environmental Toxicology and Chemistry Meeting. The graduate student on this project won three awards for her presentations at these meetings. In addition, and undergraduate student also presented and won an award using data from this project. We published our findings in the highly regarded scientific journal Environmental Science and Technology, and have authored several Extension publications that communicate soil lead hazards to the general public. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? Despite the widespread nature of lead contamination, evaluation of lead hazard is hindered by the lack of an inexpensive, accurate, and widely available test for soil lead. Accurate soil tests for bioavailable lead exist, but these tests are complicated to perform and cost prohibitive to the general public. This project sought correlations with other simpler and cheaper soil testing methods to the standard method EPA developed to correlate with in-vivo bioavailability studies. We evaluated extractable Pb by several common soil testing methods compared to the EPA's standard method. This revealed that the Mehlich-3 test was best correlated with the EPA method, and could be a potential low-cost proxy for that test. The Mehlich 3 test is available across the US for as low as $15. In addition, we were able to analyze the Pb speciation in our soils by using the Advance Photon Source at Argonne National Lab. The results of this testing suggested that the EPA's standard method (and the Mehlich 3) may be significantly over-estimating the bioavailability of Pb. Other tests, like the DTPA or Bray, showed promise because they extracted Pb in a pattern that was more like the Pb speciation data we obtained. To build on those findings, we partnered with two different research groups in Australia who provided us soils that had previously been tested on animals for Pb bioavailability. We ran the Mehlich 3 on these samples and found that the Mehlich 3 overestimated the bioavailability from the animals. These data suggest that the Mehlich 3 could be used as a conservative, low cost test for estimating Pb bioavailability for Pb contaminated soils. However, the data also highlight the need for continued work in this area. In the final year of the project, we focused on concluding the experiments and publishing the work in the scientific literature. We prepared a manuscript with several of our collaborators listed as co-authors and submitted it to one of the top journals in this field. The manuscript was reviewed favorably, and was published after one round of revisions. This publication highlighted the ability of the Mehlich-3 soil test to serve as an acceptable method to inexpensively estimate the bioaccessibility of lead in contaminated soils. We helped two soil testing laboratories begin to offer this test to the general public. We are hopeful that this project will lead to increased awareness and more accessible testing for Pb in potentially contaminated soils across the United States.

Publications

  • Type: Journal Articles Status: Published Year Published: 2018 Citation: Plunkett, S.A.; Wijayawardena, M.A.A.; Naidu, R.; Siemering, G.S.; Tomaszewski, E.J.; Ginder-Vogel, M.; Soldat, D.J. 2018. Use of Routine Soil Tests to Estimate Pb Bioaccessibility. Environmental Science & Technology. 52:12556-12562.


Progress 10/01/16 to 09/30/17

Outputs
Target Audience:The target audiences for this work include people living and gardening in areas with lead contaminated soils, policy makers, soil testing laboratories, outreach specialists, and other scientists. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?This project helped train a graduate student in the scientific method and process. She gained considerable experience and skill in soil test extractions, analytical laboratory methods, data analysis and interpretation, and oral and written communication of results. The project also trained three undergraduate students who helped with the laboratory work. How have the results been disseminated to communities of interest?We presented our results to scientists at the Annual Meeting of the Soil Science Society of America and the Society of Environmental Toxicology and Chemistry Meeting. What do you plan to do during the next reporting period to accomplish the goals?We will continue evaluating the correlations among the different extractants using more contaminated soils. We will be returning to Argonne National Lab in 2018 to get better data on Pb speciation in our contaminated soils. We will also begin to publish manuscripts in scientific journals.

Impacts
What was accomplished under these goals? A great deal was accomplished during the past reporting year. First, we finalized an experiment that evaluated extractable Pb by several common soil testing methods compared to the EPA's standard method. This revealed that the Mehlich-3 was best correlated with the EPA method, and could be a potential low-cost proxy for that test. The Mehlich 3 test is available across the US for as low as $15. In addition, we were able to analyze the Pb speciation in our soils by using the Advance Photon Source at Argonne National Lab. The results of this testing suggested that the EPA's standard method (and the Mehlich 3) may be significantly over-estimating the bioavailability of Pb. Other tests, like the DTPA or Bray, showed promise because they extracted Pb in a pattern that was more like the Pb speciation data we obtained. Finally, we partnered with two different research groups in Australia who provided us soils that had previously been tested on animals for Pb bioavailability. We ran the Mehlich 3 on these samples and found that the Mehlich 3 overestimated the bioavailability from the animals. These data suggest that the Mehlich 3 could be used as a conservative, low cost test for estimating Pb bioavailability for Pb contaminated soils.

Publications

  • Type: Conference Papers and Presentations Status: Published Year Published: 2017 Citation: McAdow, K., S. Plunkett, D.J. Soldat, T. Whitman. 2017. Soil microbial structure and activity as affected by lead (Pb) contamination. ASA-CSSA-SSSA Annual Meetings. 22-25 October. Tampa, FL.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2017 Citation: Plunkett, S., D.J. Soldat. 2017. Evaluation of traditional soil testing methods to estimate lead (Pb) bioaccessibility. ASA-CSSA-SSSA Annual Meetings. 22-25 October. Tampa, FL.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2017 Citation: Plunkett, S., D.J. Soldat. 2017. Repurposed waste products ineffective for reducing Pb bioaccessibility in a mine contaminated soil. ASA-CSSA-SSSA Annual Meetings. 22-25 October. Tampa, FL.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2017 Citation: Plunkett, S., D.J. Soldat. 2017. In vivo validation of the Mehlich-3 as a soil Pb bioaccessibility assay. Society of Environmental Toxicology and Chemistry Annual Meeting. 12-16 November. Minneapolis, MN.


Progress 10/01/15 to 09/30/16

Outputs
Target Audience:The target audiences for this work include people living and gardening in areas with lead contaminated soils, policy makers, soil testing laboratories, outreach specialists, and other scientists. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?This project helped train a graduate student in the scientic method and process. She gained considerable experience and skill in soil test extractions, analytical laboratory methods, data analysis and interpretation, and oral and written communication of results. The project also trained three undergraduate students who helped with the laboratory work. How have the results been disseminated to communities of interest?We presented our results to scientists at the Annual Meeting of the Soil Science Society of America. We also presented our results at the Growing Power Conference in Milwaukee, WI which focuses on urban agriculture. What do you plan to do during the next reporting period to accomplish the goals?We will continue evaluating the correlations among the different extractants using more contaminated soils. We obtained data on the Pb mineralogy of some of our contaminated soils from Argonne National Lab in late 2016 and will spend time analyzing those data.

Impacts
What was accomplished under these goals? In 2016, we were able to run several lab experiments with Pb contaminated soils. The soils were contaminated with various levels of Pb using lead nitrate, then incubated with different amounts of phosphoric acic which resulted in a wide range of Pb solubility and therefore differences in Pb bioavailability. The Pb in these soils was then extracted using a standard but expensive and inaccessible test for Pb bioavailability (EPA method 1340, modified to pH 2.5), and then seven other more inexpensive and accessible soil testing methods. These tests included the Bray P1, Oslen, Mehlich-1, Mehlich-3, DTPA, 0.01 M CaCl2, and 0.4 M Glycine (pH 2.5). Of these tests, we found that the Mehlich-3 had the best correlation to the modified EPA 1340 method, suggesting that the Mehlich-3 may serve as an inexpensive, accessible test that can estimate potential Pb bioavailability from soils.

Publications

  • Type: Conference Papers and Presentations Status: Published Year Published: 2016 Citation: Plunkett, S.A., and D.J. Soldat. 2016. Evaluation of traditional soil testing methods to evaluate lead (Pb) hazard. ASA-CSSA-SSSA Annual Meetings. 6-9 Nov. Phoenix, AZ.