Sarah Kebe CHEM390 Professor Ford Research Proposal 11/27/17

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1 Sarah Kebe CHEM390 Professor Ford Research Proposal 11/27/17

2 Instrumentation Funds are requested for an updated Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) apparatus in order to improve the existing facilities for faculty-student research and education in the Chemistry Department at Indiana University of Pennsylvania (IUP). The requested instrumentation will provide a highly accurate and efficient measurement system. This will thereby enable necessary development of the ICP-OES capabilities in the Chemistry Department. The PI will be the primary users of this instrumentation, both of whom have research projects that extensively involve undergraduate students. The instrumentation will also be used in our undergraduate and M.S. programs, enhancing the research training of all of our majors as well as encouraging participation in the specific projects described herein. Intellectual Merit The requested instrumentation would immensely update research abilities in the Chemistry Department via IUP. Using ICP-OES, one can test for various analytes within samples. Broader Impacts A comprehensive understanding ICP-OES will help in analyzing snow samples to have a better understanding on how pollution affects it. Automated sampling and simultaneous measurements will rapidly downsize the time to acquire data. Students will then have more time to analyze results.

3 Project Description 1.a Instrument Location The Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) instrumentation will be located in Dr. McElroys s assigned research space in Weyandt Hall. 1.b Undergraduate Research at IUP Chemistry 1.b.1 University and Department Overview Indiana University of Pennsylvania (IUP) is a regional state university of approximately 12,000 students in rural western Pennsylvania, and one of the two largest of fourteen schools in Pennsylvania's State System of Higher Education (SSHE; this does not include Pennsylvania State University or University of Pittsburgh). IUP upholds a student: faculty ratio of 16:1 The majority of students are from Pennsylvania, with many from the largely rural counties of western and central Pennsylvania. The Chemistry Department at IUP is an undergraduate department of twenty faculty offering five Chemistry majors (Chemistry Track, Pre-Medical Track, Pre- Pharmacy Track, Interdisciplinary Track, Chemistry Track [BA]), one Biochemistry major [BS] and one education major (Chemistry Education). 1.b.2 Primary Faculty-Student Research Activities The Chemistry Dept. at IUP is both an undergraduate and graduate program. As such, faculty are committed to include students in every aspect of their research programs. Students are trained both in the classroom and outside to make scientific observations, collect and analyze data to test multiple working hypotheses, and to synthesis and present these results in written and oral communication. Our goal is to fully incorporate our students into the community of science throughout their undergraduate career so that they will be well- suited for graduate studies or to step into a professional career as a scientist. Therefore, professional experiences have been incorporated into the curriculum at IUP and students are now required to participate in genuine research with a faculty mentor and formally present these results. In doing so, students complete research projects with faculty that involve a two-semester sequence of research design and methods which involves everything from experimental design to statistical analysis to scientific ethics. For many students, this work is completed with small internal research funds without compensation for hourly wages, but for students working with faculty on externally-funded projects, they are compensated as research assistants.

4 1.c Research Activities to be Enabled 1.c.1 Results from Prior Support No PIs have participated in an NSF MRI award in the past five-year period. Neither has either been PI or co-pi of any other NSF award in the past five-year period. 1.c.2 Specific Research Activities to be Enabled 1.c.2i Chemical Analysis of Snow Abstract: The main concern of this research includes analyzing snow (water) quality and presence of contaminants such as salts, heavy metals, and TDS (total dissolved solids). Fresh snow samples were collected from various sites via the town of Indiana located in Pennsylvania. These samples are then taken back to the lab to be analyzed using Ion Chromatography (IC) and Inductively Coupled Plasma-Optical Emission Spectroscopy. In doing so, one can determine how and if pollution affects snow fall, similar to the production of acid rain. Seven anions were measured and detected and measured with the use of IC: Chloride, Bromide, Nitrate, Fluoride, Iodide, Sulfate, and Phosphate. To fully approach this goal, a database can be created in time to better analyze and identify trends in quality of the snow around us. Undergraduate Student Research and Training: This project began in the past year. Dr. McElroy and an undergraduate student devised a sampling procedure and collected snow from three different locations around the university at various times throughout the winter. The student was trained in the laboratory procedures to determine pollution in snowfall using IC and ICP-OES. Due to on-going maintenance issues with the ICP-OES, metal content results were not able to be formulated.

5 Methodology: Ion Chromatography: All samples were tested under the methodology of the on-going Beaver Run monitoring project. 3 An 850 Professional IC Conductivity detector was employed for the detection of anions within the instrument. 2 The flow used was.700 ml/min, with a pressure of 7.83 MPa, at a temperature of 35 C. 2 Then 15 ml of sample is drawn into a syringe and attached to a filter cartridge and the first 2 ml is discarded into waste. 2 The remaining sample is then filtered into IC test tubes. 2 The quality control parameters were noted and followed, including the construction of calibrations curves, the use of duplicate samples, a lab fortified blank (LFB) for accuracy, a lab fortified matrix (LFM) for possible matrix interference, method blank (MB) for contamination. 2 All data reports include the results for primary and duplicate samples. 2 If quality control analysis shows problems specific actions are taken depending on the problem area. Actions include rerunning or remaking any LFB, LFM, or MB. If problems occur with samples or duplicates the analyst must review their sample preparation procedures. Routine maintenance may be done and written records are kept for future reference. Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES): Similar to the associated methodology to IC, all samples plan to be tested under the ongoing Beaver Run monitoring Project. 3 Sample preparation for the ICP-OES machine includes acid digestion with a 1:1 Nitric Acid solution. 100 ml of sample is digested with 2 ml of the Nitric Acid solution. The bottle is to be mixed thoroughly by shaking and then will be stored in the refrigerator for future testing via ICP-OES. 2 A calibration curve should be constructed during each analytical run for reference material. To ensure the quality of each run, the use of LFB, LFM, and MB samples were applied. As for unacceptable runs, corrective action is the same as to IC. The machine will be up kept to a satisfactory degree while written records should also be kept for reference material. Preliminary Results: The following tables display the anion levels at the three sampling sites: 1 Chloride: Fluoride: Bromide: Iodide:

6 Nitrate: Sulfate: For every single sample the Chloride anion was present. It was concluded the sample was collected near the sidewalk which caused the high levels of chloride from salting. The mean level of chloride was 4.67 ppm and if you apply the Grubbs test you can exclude the sample taken on 2/10/17 in the Oak Grove (OG) as a significant outlier. 2 It can be seen fluoride is not present in every sample obtained. However, the presence of fluoride can be related to the pollution in the air from coal burning plants. Levels of such were most likely higher in the past than as of now due to less usage of fossil fuels such as coal. Both Iodide and Bromide was measured at very low levels and therefore irrelevant in terms of pollution. Nitrate was also present in all samples and at considerable values. Nitrates primarily come from the exhaust of both gas and diesel vehicles. Considerable levels of nitrates are explainable because of the high use of motor vehicles in today s world. Nitrates within the atmosphere contribute heavily to acid rain accumulation through the formation of HNO3 within precipitation. 2 Similar to Nitrates, the occurrence of sulfates also contributes to acid rain production via precipitation (H2SO4). However, the values of so were lower on average in comparison to Nitrate levels. The production of acid rain leads to conflict in terms of drinking water and presumably in eating snow. Rain and snow (the principal sources of ground water) have ph values near 5.6, if they are relatively free of pollution. However, in many areas of the United States acid rain is now the norm because of pollution emissions from sources such as coal-fired power plants and car exhaust. Acid rain can have ph values near 4. 4 Drinking water which has been contaminated with acid rain can even cause brain damage over time. 5 As stated above the results for metal species content is pending at the current time. Acquisition of and Training on the ICP-OES System: The requested ICP-OES will be acquired, installed and operation verified. As this is not a time sensitive experiment, samples can be prepared according to the methodology as stated prior and stored. Therefore, preparation for the experiment can begin prior to securing an ICP-OES instrument. This can also enable a sufficient amount of time whereas undergraduate student researchers can be trained upon the care and usage of the apparatus. This will include an overview of ICP, demonstrations of steps of operating, and guidelines on analyzing results. Following, the undergraduate researcher will plan to operate the machine under direct supervision of the PI. This will ensure an appropriate understanding.

7 Determination of Metal ions in Snow Samples: Contamination of Groundwater is a serious problem being faced by many countries. Heavy metals enter the environment by natural and anthropogenic means. 6 Such sources include: natural weathering of the earth s crust, mining, soil erosion, industrial discharge, urban runoff, sewage effluents and pest or disease control agents applied to plants, air pollution fallout. 6 The pollution of the aquatic environment with heavy metals has become a worldwide problem during recent years, because they are indestructible and most of them have toxic effects on organisms. 6 Among environmental pollutants, metals are of particular concern due to their potential toxic effect and ability to bio accumulate in aquatic ecosystems. 6 Thus, when taking this to mind, one can hypothesize how snowfall may be affected by this similar to rainfall. With the use of ICP, heavy metals can be measured up to trace level concentrations while providing great accuracy and precision. Research Summary: It can be deemed that the content obtained from fresh snowfall presents an adequate amount of anionic material. Further sampling and testing plans to occur in the future. Obtaining certain results are still in progress and therefore the content of metals in the samples cannot be measured and characterized. This hinders the ability to fully determine whether the ingestion of snow can pose a health risk and more so how. The proposed research aims to highlight environmental monitoring along with its significance. The ongoing goal or next step for this project would be to ultimately determine sources of pollution in snowfall. From the results formulated one can most likely conclude eating snow is not a keen idea. 1.d. Description of the Research Instrumentation and Needs Inductively Coupled Plasma- Optical Emission Spectrometer (ICP-OES) is one of the most widely using technique for determination of multi-elements in various environmental matrices in single aspiration. 6 Therefore, the mere need for an ICP is irrelevant in this proposal. More so, the necessity for an upgraded and modernized ICP is of importance. Our current system has hindered us from continuing this research due to a constant need for ongoing maintenance. In obtaining a new ICP-OES we can ensure our results to be at their best.

8 Works Cited [1] IUP at a Glance (accessed Nov 15, 2017). [2] Woodyard, B. M.; McElroy, N. Chemical Analysis of Snow via Ion Chromatography and Inductively Coupled Plasma Optical Emission Spectroscopy; rep.; 2017; pp [3] McElroy, N. (accessed Nov 20, 2017). [4] Acid Rain and Ground Water ph (accessed Nov 21, 2017). [5] Penman, A. Acid Rain (accessed Nov 27, 2017). [6] Raju, O. V. S.; Prasad, P. P. P.; Reddy, Y. International Journal of Scientific Research 2012, 2 (11),