Environmental Chemistry:

Undergraduate and Graduate

Classroom, Laboratory, and Local
Community Learning Experiences
 ACS SYMPOSIUM SERIES 1276

Environmental Chemistry:
Undergraduate and Graduate
Classroom, Laboratory, and Local
Community Learning Experiences

Elizabeth S. Roberts-Kirchhoff, Editor

University of Detroit Mercy
Detroit, Michigan

Mark A. Benvenuto, Editor

University of Detroit Mercy
Detroit, Michigan

Sponsored by the
ACS Division of Environmental Chemistry, Inc.

American Chemical Society, Washington, DC

Distributed in print by Oxford University Press

Library of Congress Cataloging-in-Publication Data

Names: Roberts-Kirchhoff, Elizabeth S., editor. | Benvenuto, Mark A. (Mark

Anthony), editor. | American Chemical Society. Division of Environmental
Chemistry.
Title: Environmental chemistry : undergraduate and graduate classroom,
laboratory, and local community learning experiences / Elizabeth S.
Roberts-Kirchhoff, editor (University of Detroit Mercy, Detroit,
Michigan), Mark A. Benvenuto, editor (University of Detroit Mercy,
Detroit, Michigan) ; sponsored by the ACS Division of Environmental
Chemistry, Inc.
Description: Washington DC : American Chemical Society, [2018] | Series: ACS
symposium series ; 1276 | Includes bibliographical references and index.
Identifiers: LCCN 2018018539 (print) | LCCN 2018020709 (ebook) | ISBN
9780841232853 (ebook) | ISBN 9780841232860
Subjects: LCSH: Environmental chemistry. | Air--Pollution--Research. |
Cosmetics--Analysis.
Classification: LCC TD193 (ebook) | LCC TD193 .E57 2018 (print) | DDC
577.27--dc23
LC record available at https://lccn.loc.gov/2018018539

The paper used in this publication meets the minimum requirements of American National
Standard for Information Sciences—Permanence of Paper for Printed Library Materials,
ANSI Z39.48n1984.

Copyright © 2018 American Chemical Society

Distributed in print by Oxford University Press

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 Foreword
The ACS Symposium Series was first published in 1974 to provide a
mechanism for publishing symposia quickly in book form. The purpose of
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sponsored symposia based on current scientific research. Occasionally, books are
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ACS Books Department

 Contents
Preface .............................................................................................................................. ix

1. Introduction to Environmental Chemistry of the Arctic: An Introductory,

Lab-Based Course Offered Both Face-to-Face and by Distance ......................... 1
Jennifer J. Guerard and Sarah M. Hayes

2. Community-Based Undergraduate Research: Measurement of Hazardous

Air Pollutants with Regard to Environmental Justice ....................................... 21
Kathryn Zimmermann, Laura Young, and Kelsey Woodard

3. Undergraduate Research Experience in Remote Sensing .................................. 49

A. Kahl

4. Trends in Atmospheric Ammonia: An Environmental Chemistry Class

Project ..................................................................................................................... 57
Vivian C. Ezeh

5. Using DNA Barcoding To Identify Duckweed Species as Part of an

Undergraduate Ecology Course ............................................................................ 67
Stokes S. Baker

6. Synthesis of a Novel Series of Nitrogen-Containing Ligands for Use as

Water Remediators, All Incorporating Long-Chain Aliphatic Moieties .......... 81
Justin Pothoof, Michele Bhagwagar, Grace Nguyen, Sara Tinawi, Sara Makki, and
Mark A. Benvenuto

7. Analysis of Cosmetic Mineral Eyeshadows and Foundations with a

Handheld X-ray Fluorescence Analyzer .............................................................. 89
Tiffany Tieu Ngo, Sara Thomas, Diamond Stokes, Mark A. Benvenuto, and
Elizabeth S. Roberts-Kirchhoff

8. Arctic Communities as Sites of Local Field Work in Environmental

Chemistry .............................................................................................................. 105
Mark H. Hermanson and Sydney Le Cras

9. Mapping of Brownfield Properties in the Detroit Community Using GIS ..... 125
Alexa Rihana-Abdallah and Yuncong Pang

Editors’ Biographies .................................................................................................... 135

vii
 Indexes

Author Index ................................................................................................................ 139

Subject Index ................................................................................................................ 141

viii
 Preface
“We do not inherit this land from our parents. We borrow it from our children.”
- Amish saying, or Native American Proverb, or Chief Seattle

There is probably no more direct connection between the science of

chemistry and our modern society than that encompassed in the field we now call
environmental chemistry. As populations have grown, and population density in
certain areas has increased dramatically, the impact of all human presence on our
air, water, and soil has become pronounced. In many cases, the impact has been
negative, yet every human being must leave some footprint of their time on Earth,
no matter how small. This makes it important that we examine our surroundings
in some detail.
This book has its roots in the symposium: “Environmental Chemistry:
Undergraduate and Graduate Classroom, Laboratory, and Local Community
Learning Experiences” held in 2017 at the 253rd National Meeting of the
American Chemical Society in San Francisco, CA. There were several excellent
presentations there, which we wished to capture. There are also some authors in
this volume who were unable to attend, but who are doing good work in the field
today. We have an impressive collection of ways that environmental chemistry
is explored by both undergraduate and graduate students in independent research
projects and course-based undergraduate research experiences. Students are
exploring these topics in interdisciplinary groups both within their institution
and the greater community. For example, Guerard and Hayes (Chapter 1)
describes a novel entry-level environmental chemistry course with students onsite
working collaboratively with students at distant sites focused on the chemistry
of the Arctic. In a community-focused project, Zimmerman et al. (Chapter
2) reports on the passive sampling of air pollutants in local communities as an
interdisciplinary project by students from political science and basic science
working with professionals from a local environmental law firm. Kahl (Chapter
3) details a collaboration between faculty and students from several campuses to
support a network of data loggers to collect information on water quality across
western Pennsylvania, while Ezeh (Chapter 4) reports on a course-based research
experience where data on atmospheric ammonia was collected. An interesting
use of DNA barcoding to catalog the varieties of duckweed in Michigan waters
as part of an undergraduate ecology course is described by Baker (Chapter 5).
Benvenuto and his students (Chapter 6) report on the synthesis of a novel set of
ligands designed to chelate metal ions in aqueous systems. Roberts-Kirchhoff,
Benvenuto and their students (Chapter 7) describe the results from the elemental
analysis of consumer products. Hermanson and LeCras (Chapter 8) describe

ix
a second example of students involved in collecting data on environmental
chemistry in the Arctic with their report of the analysis of atmospheric mercury
and flame retardants. We conclude the volume with Rihana-Abdallah and Pang’s
summary (Chapter 9) of brownfields in both Michigan and Detroit, a city that has
played a major role in the industrialization of America.
We believe this book has the potential to become an important piece of the
greater mosaic that is an understanding of the factors which make up the chemistry
of our local, regional, and global environment, and to make the current ideas and
this discussion available to a much wider audience. We hope that the chapters
herein inspire our readers to execute further projects and deeper study of our local
and greater environment. It is indeed worth remembering that we only borrow
what we use today from our children’s generation.

Elizabeth S. Roberts-Kirchhoff, Ph.D.

Assistant Dean for Academics
College of Engineering & Science
University of Detroit Mercy
Detroit, Michigan, United States
robkires@udmercy.edu (e-mail)

Mark A. Benvenuto, Ph.D.

Fellow, American Chemical Society
Professor and Department Chair
University of Detroit Mercy
Detroit, Michigan, United States
benvenma@udmercy.edu (e-mail)

x
 Chapter 1

Introduction to Environmental Chemistry of

the Arctic: An Introductory, Lab-Based Course
Offered Both Face-to-Face and by Distance
Jennifer J. Guerard1 and Sarah M. Hayes*,1,2
1Department of Chemistry and Biochemistry,

University of Alaska Fairbanks, 900 Yukon Dr.,

Fairbanks, Alaska 99775, United States
2Present address: Eastern Mineral and Environmental Resources Science

Center, U.S. Geological Survey, 954 National Center,

Reston, Virginia 20192, United States
*E-mail: shayes@usgs.gov. Phone: 703-648-6461.

In this chapter, we present a model for an entry-level lab-based

undergraduate environmental chemistry course delivered
simultaneously by face-to-face and distance modalities. This
course frames conceptual chemistry using the theme of Alaskan
Arctic environmental issues in order to increase engagement
and perceived relevance of chemical principles. Synchronously
delivered lectures and guided discussions along with the
incorporation of peer-mentored research projects encourage
the development of a learning community among students in
the course. Distance students participate in the same virtual
and “kitchen” lab experiments as on-campus students, thus
providing an educationally equivalent curriculum to all. In
mixed teams of on-campus and distance students, all students
participate in research projects to allow entry-level students to
explore their interests in STEM fields. Students thereby begin
to build an identity as a scientist and hopefully this course will
serve as a mechanism to improve recruitment and retention
of students, especially from traditionally underrepresented
groups, in the chemical sciences and other STEM fields of
study. Responses from the first course offering communicated
positive attitudes toward the course content and methods.

© 2018 American Chemical Society

 Introduction
Alaska and the Arctic: A Contextually Relevant Framework for
Environmental Chemistry
Environmental chemistry has been increasingly introduced into undergraduate
curricula in recent decades (e.g., (1–4)). Contextually driven activities improve
both understanding and engagement in undergraduate courses by highlighting the
relevance of chemistry and its application to the real world (4). Environmental
chemistry is an especially useful context in which to present chemical concepts,
especially for non-majors (3). Incorporating environmental and climate-change
issues into chemistry courses has been shown to improve scientific literacy and
conceptual understanding (5, 6).
High-latitude systems are especially sensitive to changes in climate. The
Arctic has continued to see air temperatures increasing at double the global average
rate, bringing with them a host of environmental changes from decreases in sea-ice
extent to thawing permafrost (7). Alaska represents a diverse set of ecosystems
from coastal Western hemlock-Sitka spruce forests to the treeless Arctic plains
(8). Wetlands cover an extraordinarily high proportion of Alaska, occupying 43%
of Alaska’s surface area compared to only around 5% of land surface area in the
lower 48 states (9). The fate and transport of contaminants in the Arctic is also
of concern, as organic contaminants have been observed to undergo long-range
transport to high latitudes (10). Thus, assessing surface water quality is critically
important for understanding Alaska’s environmental health.
This is especially true in rural communities, where residents live in close
connection to and rely upon their environment. Environmental stresses affect
subsistence practices, food availability, water quality, and infrastructure, among
many other aspects of life (11–15). Many Alaskans connect with the One Health
paradigm, i.e. the idea that the health of humans, animals, and the environment
are inextricably linked (13, 16, 17). As such, Alaska and the Arctic are an
ideal backdrop against which to highlight environmental chemical processes
in atmospheric, aquatic, terrestrial, and biological spheres, in addition to being
directly relevant to communities within the state.

Course-Based Undergraduate Research and Peer Mentoring

The demonstrated benefits of incorporating research into course curricula are
well known (e.g., (18)), suggesting that research not only affects attitudes toward
the relevance of chemistry (5), but also improves confidence, understanding, and
success in later courses (19–22). Undergraduate involvement in research has also
been linked to improved critical thinking, intellectual independence, and increased
retention in fields related to STEM (23).
Mentoring has specifically been observed to improve the student research
experiences and retention of students from traditionally underrepresented groups
(24, 25). Mentored research early in the undergraduate experience, particularly
that which blends both faculty and near-peer mentoring, can be an effective
method for integrating students into the research process (e.g., (26, 27)). Effective
mentoring has been linked to increased independence and competency (28–31), as
2
well as improved retention (24, 32, 33). Peer mentoring in research contexts, when
undergraduates mentor each other, is viewed positively by undergraduates and
have benefits including becoming part of a community, growth of self-confidence,
and a sense of accomplishment (34). These factors are important for persistence
within STEM (35). Further, studies have shown that peer instruction can lead to
improved conceptual understanding (36, 37).
While traditional undergraduate research provides many benefits such
as those listed above, course-based research is also beneficial to students.
Participation in a classroom-based research experience at the introductory level
has been linked to positive changes in student interest toward pursuing science
careers and attitudes toward science in general (38). Course-based research
experiences are also attractive to students because of the finite time commitment
required (39). Course-based research experiences have been shown to provide
several benefits that promote inclusion, that may be especially important for
traditionally underrepresented students, including: improving awareness of
research opportunities, learning of the benefits of research, and providing
interactions with faculty (40). Together, these benefits may serve as a gateway to
future more traditional undergraduate research experiences.

Engagement Challenges with Distance Learning

Course-based research is an example of integrating active learning techniques
in the classroom, and has been shown to statistically improve student grades,
long term comprehension (41, 42), and reduce the achievement gap between
disadvantaged students and their peers (43). These techniques are supported by
pedagogical studies that have concluded that classroom lecture learning accounts
for less than 10% of the lifetime learning (44). The effectiveness of a variety
of active learning techniques has been demonstrated, including: case studies,
student discussions, lecture pauses, and involving students as creators. However,
incorporating active learning techniques in distance courses can be especially
challenging.

This Study
The authors developed a blended face-to-face and distance lecture and
lab-based course that interweaves Alaska and Arctic-relevant issues throughout
the curriculum, emphasizing chemical principles and their roles in the
environment. This course incorporates active learning in several forms as
well as faculty-directed and peer-mentored research projects. In keeping with
best practices (45), the curriculum deliberately integrates the face-to-face and
distance courses by mixing student teams to facilitate the development of learning
relationships between students. We have intentionally designed an environmental
chemistry course that involves students as both researchers and peer mentors to
strengthen the sense of a learning community among participants. This course
engages students in all aspects of the research cycle, including: developing
laboratory techniques, applying the scientific method, making and recording
careful observations, interpreting numerical data, and sharing their results.
3
Thus, entry-level students learn introductory chemical concepts by engaging in
faculty-directed research and exploring the status of environmental health in
Arctic ecosystems and communities.

Rationale
In this chapter, we describe a model for a lab-based course offered
simultaneously by on-campus and distance modalities in which chemistry is
taught in the context of Arctic environmental health. The target demographics are
early career or nontraditional undergraduate students regardless of their physical
location within Alaska or declared major of study. As a core-designated course,
this course is accessible and attractive to students from diverse majors of study
and will hopefully serve as a mechanism to build science literacy across the state.
Distance learning is a particularly important method of instruction for Alaska
because, being the largest state in the United States, it has many rural communities
that are separated by large distances and not connected by roads (Figure 1). In
2000, Alaska had less than 13,000 miles of public road (46). In fact, several
unique factors can impact the student experience at distance campuses or in rural
communities in Alaska compared to most locations in the rest of the U.S. These
include: limited bandwidth for internet connectivity, below freezing temperatures
for most of the academic year, and most outlying communities are not connected to
the road system, meaning materials have to be transported either by water during
the summer or by air. All of these factors must be taken into account when planning
a successful lab and field-based distance course like the one described here.
The University of Alaska system has a high proportion of non-traditional
and rural students. It is common for students to take courses online, though
there are currently few offerings in chemistry or that incorporate research, and
few undergraduate environmental chemistry courses (distance or face-to-face),
especially targeting early undergraduates. This was seen as a great opportunity to
make chemistry relevant for our students by applying it to the Arctic environment
where they live and capitalizing on faculty research expertise. This course was
designed to attract students early in their post-secondary education in order to
provide a course-based lab and peer-mentored research experience by distance, in
hopes of improving STEM recruitment and retention.
Students are expected to come to this course with no previous research
experience. They are guided through small but highly relevant research projects
examining surface waters from their home communities. The project portion is
intentionally designed to involve students as both researchers and peer mentors
(Figure 2). In cooperation with other members of their research teams (which
are ideally mixed between face-to-face and distance students), students examine
water quality indicators within the context of human, animal, and ecosystem
health. In this way, we are directly incorporating One Health relevant research
into the curriculum in a way that is accessible to students with little prior science
knowledge.

4
 Figure 1. This course is offered in both distance and on-campus modalities to
allow students in rural communities across Alaska to participate and build
relationships with students on-campus. Alaska has unique challenges, including
a very limited road system.

We hope to recruit or retain nontraditional STEM majors, who might not

be as successful starting off in a more traditional, calculation-based general
chemistry setting. Applying conceptual chemistry in the context of Arctic
environmental health is aimed to frame the content in an especially relevant and
accessible format for rural Alaskans. Engaging students in research empowers
them to assess the health of their home communities. Further, building personal
relationships between rural students and the main University of Alaska Fairbanks
(UAF) campus could support rural students interested in finishing their degree
program at UAF.
Degree requirements include core courses, which are designed to provide
“students with a shared foundation of skills and knowledge that, when combined
with specialized study in the major and other specific degree requirements,
prepares students to better meet the demands of life in the 21st century” (47).
These core requirements include eight credits of natural science, which are
fulfilled by taking two specially designated lab-based courses selected from the
100 and 200-level science classes.

5
 Enrollments were capped such that there was a limit of twice as many
face-to-face students as distance students, to best facilitate the integrated group
research projects with mixed teams of distance and on-campus students. The
ratio of distance to face-to-face students with regards to this course and student
success has not yet been thoroughly tested, and are open to adjustment in the
future depending on the composition of the research groups in future deliveries.

Figure 2. Theoretical framework for faculty-guided research projects and

mentoring of research teams made up of on-campus and distance students.

Student Learning Outcomes

This course was intentionally designed to require less advanced math

prerequisites compared to that required by most STEM core courses at UAF,
in order to reach students early in their post-secondary experience and remove
barriers for exposure to the chemical sciences. Taken directly from the syllabus
(48), after successful completion of this course, students will be able to:

1. Understand the basic chemical concepts as they relate to the function of

ecosystems and the existence/transformation of contaminants.
2. Outline basic metrics for assessing air, water, and soil quality and explain
their importance as indicators of environmental health.
3. Identify examples of anthropogenic influences of natural cycles and
explain how that impacts ecosystem health.
4. Evaluate student-generated water quality data from across the state and
interpret data to assess anthropogenic perturbation of ecosystems.

Each of these student learning outcomes were integrated throughout the entire
course, through synchronous lecture, discussion, laboratory, and peer-mentored
research activities as described below.

6
 Implementation

Successful execution depends on developing strong integration between lab

and lecture topics (Table 1), creating lab kits with clear instructions, integrating
tablet technologies to create a seamless interface between on-campus and distance
students, and supporting teams in forming strong collaborations. The course
syllabus is available from the UAF Department of Chemistry and Biochemistry
website and a course schedule is shown in Table 1 (48).

Integration of Face-to-Face and Distance Course Delivery

This course was set up for enrollment in either a face-to-face or distance

format, each worth the same number of credits and providing equivalent
experiences. The lecture was held synchronously with both face-to-face and
distance participants, in order to foster productive real-time discussion on course
topics, and facilitate the development of a learning community during each
class period. While distance courses are often perceived to be less engaging
than face-to-face courses, specific strategies were implemented to enhance
engagement and facilitate active learning. Both peer-to-peer and instructor-to-peer
communication have been reported by students to be the most important factors
in facilitating engagement in online courses (49). This is also reflected in the fact
that student completion rates in online courses tend to be higher when students
perceive a sense of community (50, 51). We chose to enhance this through
peer-discussion online, peer-mentored research, and faculty facilitated discussion
during synchronous class time, along with regular directed feedback between
instructor and student relating to coursework.
Lectures were delivered through the university learning management system
(LMS), where non-animated slides and audio were transmitted so as to lower the
bandwidth requirement for distance students. The software allowed for distance
students to raise hands, type questions, and/or speak by audio during the class
session, as needed, in order to be fully interactive during the session.
In addition to lecture, all of the other facets of the course were delivered online
as much as possible. Reading questions and exams were conducted through the
LMS, and all lectures were recorded and posted on the LMS. Lab report forms
were filled out either in person for face-to-face students, or scanned/photographed
and uploaded into the LMS for distance students. A discussion forum hosted on
the LMS was required for all students in order to foster interaction between face-
to-face and distance students, which was actively monitored by the instructors.
To ensure distance students had tools necessary for full and engaged
participation, android tablets were sent out with the distance laboratory kits
on loan. Distance students were responsible for their own internet access, but
otherwise the tablets contained all the necessary apps to participate fully in the
course pre-loaded onto the device, which then became their portal for the course.

7
 Table 1. Tentative Course Schedule. Lecture topics, case studies and
laboratory experiments are tightly coupled to facilitate student learning.
Wk. Topic Case Study Laboratory
0 Course Introduction
1 Labor Day The Obligation to 1: Safety and Scientific
Intro. to Env. Chem. Endure Method
2 Air Quality Bear Trouble 2: Air Quality Models
and Intro. to pH
3 Introduction to Water Regulating Triclosan 3: Water Quality and
Quality Contamination
4 Water Quality and PCB Transport in the 4: Sampling Surface
Treatment Arctic Water
5 Water Quality of Sulfolane 5: Surface Water Analysis
Groundwater
6 Marine Water Quality Ocean Acidification 6: Marine Water and
Ocean Acidification
7 Contaminant none 7: Contaminant
Transformations Partitioning
EXAM 1
8 Weathering and Soil Permanent Permafrost 9: Weathering and Soil
Formation Formation
9 Metals and Inorganic Pebble Mine 10: Soil Quality and
Contaminants Contamination
10 Environmental Coliforms in Antarctica 8: Microbial World
Microbiology I
11 Environmental Biodegradation of Oil 11: Biodiversity and
Microbiology II Biomagnification
12 Ecological Interactions Bioaccumulation in the No lab
Thanksgiving Arctic
13 Forrest Fires and Glacier Bay Succession Group work on
Ecological Succession presentations
14 Climate Change in the Climate Change Data 14: Energy Sources and
Arctic Climate Change
15 EXAM 2
3:15-5:15 pm Final Exam- Student Presentations

Context-Driven Chemistry

In addition to incorporating Alaska and Arctic specific issues into lectures,

several lecture periods included guest lecturers from various departments within
the university who offered extpertise in different areas. Guest lecturers were
researchers who shared their research and how it related to environmental

8
chemistry, thereby giving students the opportunity to see how scientists were
actively using environmental chemistry to solve real-world problems.
Weekly case studies from poplar news or science articles or National Center
for Case Study Teaching in Science (NCCSTS; (52)) were chosen for their
environmental and/or Arctic themed relevance. These formed the basis for
discussion board topics, in which a few discussion prompts were posted each week
to facilitate student sharing. Some of the prompts focused on comprehension of
the issues, while others focused on student reactions and the impacts students had
observed in their home communities. Participating in discussion forums (both
posting and replies) was a required part of the course for all students.

Distance and On-Campus Laboratory Experiences

There are several established ways to approach distance laboratory
experiences, including: lab intensives, kitchen labs, and virtual labs. Lab
intensives are when students travel to a campus for a few days to perform
experiments with their classmates, and are most similar to a traditional lab course
experience, except with a compressed time frame. This option has been used
successfully in rural Alaska because most students enrolled can readily travel to
a central location at one of the university’s satellite campuses, but lab intensives
can lack flexibility. Kitchen labs are experiments designed to be performed in
a student’s home without significant hazards, and often without sophisticated
equipment. Kitchen labs are attractive because they provide a flexible, authentic
lab experience with minimal safety hazards. Virtual labs allow students to
explore concepts through a computer-based simulation and are useful to visualize
molecular-scale or other phenomena that cannot be observed, when resources are
not available or experiments are too hazardous to perform an experiment at home.
For this course, we chose to do a combination of kitchen and virtual lab exercises
because of the opportunity to directly link lab and lecture content on a weekly
basis and allow flexibility for students.

Distance Laboratory Kits

Mail-delivered lab kits were developed in partnership with eScience Labs
(53). We collaborated with eScience Labs to create completely self-contained
laboratories with complete step-by-step instructions (Figure 3). We were able to
modify several existing experiments from eScience Lab material, but rewrote a
substantial portion of the lab manual to refocus on environmental chemistry and
Arctic-related issues. We worked closely with eScience Labs, meeting regularly in
a combination of remote and in-person meetings during the six months prior to the
first course offering. The result was a set of customized lab kits specifically for our
course, several newly developed laboratory activities, and a 167-page laboratory
manual.
Completed lab kits were shipped to the instructors in Fairbanks so a few
remaining supplies could be added prior to shipment to distance students. Added
materials included: loaned instructional tablets pre-loaded with a complete
lab manual and all applications needed to successfully complete the course,
9
printed packets with copies of the lab manual pages for students to write
on, and acid-washed sampling containers used in the research project, and
pre-postage-paid thermosafe containers and ice packs for shipping aliquots of
research project samples back to UAF during the term.

Figure 3. Lab manual and lab kit developed for the course through a
collaboration with eScience Labs.

During the first offering of the course, the instructors held regular office
hours both in person for face-to-face students and online through LMS to answer
any questions that students might have regarding performing lab experiments.
However, there were very few procedural questions, a testament to the excellent
lab kit we produced. During the first course offering, the instructional team
also met weekly to create videos demonstrating how to perform each laboratory
experiment. In future offerings, these videos will be pre-loaded on the lab kit
tablets and hosted online to offer maximum support for students while minimizing
the required bandwidth.
Several virtual labs were used when the content was either not available or too
hazardous to be delivered by air mail. For example, a virtual lab exploring aquatic
macroinvertebrates was used instead of a real pond dip because by the 10th week of
the semester most surface water in Alaska is frozen (Table 1). We also endeavored
to find virtual labs that would be self-supporting or require minimal bandwidth.
On-campus labs relied on the same laboratory manual and experiments as
distance students received in mailed the lab kits. This provides an educationally
equivalent opportunity for all students enrolled in the course. On-campus labs
have the advantage of being less expensive to run and the lab fees are lower for
the on-campus students relative to the distance students because supplies can be
purchased in bulk, do not have to be packed into an individual lab kit, and supplies
can be used by several courses to minimize costs.

10
Lab Safety

Laboratory safety, regardless of physical venue is always of the utmost

importance. The instructional team worked extensively with eScience Labs,
UAF Environmental Health and Safety, and our departmental safety specialist
to ensure that we were doing everything possible to promote a culture of safe
practices for both our face-to-face and distance students. Lab kits sent to distance
students included standard personal protective equipment, including: safety
glasses, gloves, apron, and bench paper. For the field sampling component of
the research project personal safety was stressed in the lab manual and in class
several times prior to the activity. To manage risk, the instructional team required
that each student select a site a week prior to sampling and submit it for approval,
which was then considered in conjunction with safety specialists. Life jackets
were required (although not provided) when working in and around water. It
is imperative to work with university safety experts when designing specific
protocols for sampling and all aspects therein.

Peer-Mentored Research Projects

One of our motivations in developing the course was to empower rural

students to contribute to meaningful research within their home communities.
Alaska has a paucity of data on surface water and drinking water quality in many
areas (54). Thus, we could contribute to the state of knowledge in a meaningful
way by engaging students in measuring water quality across the state. Because
most surface waters are frozen September to April, this course had to be run in the
fall semester with sampling occurring as early as possible to be sure that students
had liquid-phase natural surface waters to sample and minimize ice-related risks.
Students began preparing in week 2 of the semester by identifying a sampling site
and submitting it for instructor approval (Table 1). In week 3, students perform
a practice analysis with all the equipment used in the field on tap and distilled
water, so that students will feel comfortable with the tablets and bluetooth
pH, temperature, and redox probes (ORP), as well as the test strips provided.
Instructor videos help students select good sampling sites, use proper sampling
techniques, and calibrate and use their bluetooth probes properly (55).
In week 4, rural students collect water samples, filter and split their 1 L
sample into four 250-ml splits, reserving one for themselves and prepare the
remaining three splits for shipment to UAF in coolers provided. On their split they
analyze some of the water quality parameters (pH, temperature, ORP). Meanwhile
on-campus students prepare for arrival of mailed samples and prepare materials
needed for the more sophisticated analyses performed at UAF, including: flame
atomic absorption (FAA) to measure cations, ion chromatography (IC) to measure
anions, and characterization of dissolved organic matter (DOM) by UV-Visible
spectroscopy and fluorescence.
In week 5, all students analyze water quality indicators with on-campus team
members duplicating rural student results. Measured parameters include: pH,
chloride, alkalinity, hardness, phosphate, ammonia, and total iron. Some of these
parameters may be altered by the time delay between sampling and measurement
11
which was discussed, but was coordinated in this way for time distribution between
labs. On-campus students also make UV-Vis measurements and prepare samples
for the more advanced instrumentation, which faculty demonstrate for all students.
In this project, research team members develop different, but equivalently
valuable, expertise with the rural students becoming site experts and the
on-campus student becoming more knowledgeable about the advanced
instrumentation used to analyze waters. While the on-campus students get to
experience the site through videos and observations collected by the rural student,
they will never have the same understanding as the student embedded in the
community where it was collected. Similarly, while videos and explanations of
sample preparation are available to rural students, it is not the same as physically
preparing samples for the other analysis techniques. However, both experiences
are essential to successful completion of the research project. The distance
student becomes the site expert, and the on-campus students then also perform
Hach test strip kits just like the distance students, but then work together to assess
the overall health of the water body.
For the rest of the semester, especially week 13 lab (Table 1), students work
in their teams to research more about the water body they sampled and interpret
their water quality data. They consider what the water is used for and how human
activity might affect the water quality upstream and downstream. Teams examine
their measured water quality parameters versus the Alaska State Water Quality
Standards to see if they are within legal limits and evaluate the overall health of
the water. Students chat by video on the tablets, and then jointly work to develop
a presentation about the water quality of that site.

Results

First Offering Successes

The technical aspects of the distance delivery of the course worked very
smoothly. There were very few questions relating to performing the lab, despite
all students being distance students. Distance delivery of lectures via the LMS
was quite smooth and in the rare cases that students were not able to attend class
synchronously they could still watch the lecture videos. Both instructors attended
and participated in all lectures during the term, which brought diverse perspectives
and energy to the presentation of material, and guest lecturers provided additional
expertise in specific topics and brought new perspectives into the classroom.
One of the most successful parts of the course was the weekly asynchronous
discussions, where students interacted above and beyond the requirements by
continuing to discuss in a thoughtful way with each other. The self-perpetuating
nature of student interactions and depth of student contributions was one of the
main successes and joys of the course for the instructional team.

12
First Offering Challenges

The first offering of this course did not conform exactly to the model we
proposed above. The course attracted only three students, all juniors or seniors,
and all enrolled in the distance course. Students all lived in locations connected to
the road system served by the USPS and did not have problems with bandwidth.
This was largely attributed to the course first being offered as a trial course that
did not fulfill a graduation requirement. However, the course has since gained core
designation, which will hopefully help in recruiting our target demographic in the
future. We would also like to build relationships with rural campuses to help with
future recruitment.

Assessment of Student Attitudes

Formative and summative evaluation of the course was built in from the
beginning using an external evaluator who performed pre- and post-assessment
of student attitudes and learning, which were anonymized and withheld from the
instructional team until after grades were assigned. With the small class size, it
is impossible to generate statistically relevant results. However, both of the two
students who participated in both the pre and post surveys reported increased
likelihood in response to the question, “How likely is it that your eventual career
will directly pertain to the environmental field?” Students also reported a strong
integration between lab and lecture.
Below are representative student quotes received in the semester-end
evaluations:

“Chem 194 has been a rewarding experience that provided important

information on problems in the local environments, as well as larger
problems we are facing worldwide. The combination of interesting
lectures with practical labs has made the class engaging and fun.”

“I’m really glad I took Chem 194, as it provided me with a wealth of

information on environmental problems, and potential solutions to help
evaluate and preserve the quality of different ecosystems.”

“The labs were straight forward, and the action of sampling from a field
site was a very enriching experience that really tied the class to local
issues.”

“Introduction into Environmental Chemistry in the Arctic really

peaked my interest and introduced me to many concepts that I had not
encountered before.”

“The water project was very unique, and helpful to seeing the connections
of water parameters and the topics of many lectures, and how they
connect to the environment.”

13
 “I liked the amount of communication with the other class members
throughout the semester. I liked having to read and respond to discussion
board posts, but not being required to communicate any more often or
seriously than that. I was glad I could work independently on the labs
and weren’t required to collaborate with others for those.”

“I liked the amount of communication from the instructors to the class

about assignments, exams, problems, etc.”

“I’m not sure that the lab was super useful to me. I definitely felt as if it
was intended for people that had not worked at all in science before. I
liked the overall course content, but the lab felt very simplistic.”

The tone of most of these comments suggest that, although there are some
things the instructional team can improve upon, students valued the course’s Arctic
focus and it would be appropriate for our target demographic.

Future Work
This course was fully developed in summer and first offered in Fall 2015
as a trial course and has since been approved for a core designation, which also
involved moving from a 3-credit to a 4-credit course. This corresponds to an extra
hour of lecture per week from the 2015 offering, which will be used to incorporate
more active learning strategies, facilitate more in-class discussion, and increase
collaboration between on-campus and distance students. It is important for faculty
to not just deliverer content and facilitate discussion during synchronous lecture,
but also to actively engage with students in all facets of the course, including
discussion forums, laboratory activities, etc. Additional data from future offerings
will allow for long-term data collection on enrollments, recruitment, and STEM
retention.
Unfortunately, subsequent offerings of the course have not yet occurred due
to other unrelated constraints. Future offerings will also grow the water quality
data sets generated by students within the course. Specifically, we are looking to
collect data on basic water quality across the state, a property that is lacking (54)
and to present this accumulated data in an online venue for public access.
The next phase of this project will involve developing an interactive map
to display student-collected data from the class in a publically available venue
(Figure 4). In this way, students can contribute to publically available data on
Alaska’s surface water. This could eventually serve as a resource for policy makers
and scientists in identifying surface water quality concerns and faciliate resource
managment decision making.
Potential extensions for the course could include community engagement
activities to discuss water quality and/or environmental issues, and to contribute
to our knowledge of natural Arctic waters. Partnerships with satellite campuses
may also bring mutual benefits of increased enrollments and additional pathways
for students to pursue their educational dreams.
14
Figure 4. Collection of student-generated data in an interactive map describing
status of surface water quality in the state of Alaska.

Conclusions
This course model describes translatable models for the implementation of an
integrated face-to-face and distance laboratory, and a course-based peer-mentored
research component. The contextually driven laboratory and research activities
may especially serve rural/nontraditional students by identifying issues relevant to
their local community and environment. Part of this course’s success is improving
students’ self-identity within science and capitalizing on issues students care about
as a mechanism to increase engagement. Our model is specific to Alaska and the
Arctic, but the course content can be tailored through case studies, peer-mentored
research projects, and exploration of location-relevant environmental issues to
other ecosystems. We welcome interest in translating this course model to other
ecosystems through collaborative projects.

Acknowledgments
The authors wish to gratefully acknowledge Chris Iceman, Annie Chartrand,
and the Department of Chemistry and Biochemistry for their participation
and support of the class. Also, the invaluable contributions of several UAF
Biomedical Learning and Student Training (BLaST) Learning, Research, and
Training Technicians (LRTTs): Lori Gildehaus, Johanna Green, and Theresa
Vertigan for their guest lectures and contributions to the lab. The UAF eLearning
staff, especially Madara Mason and Christin Bouffard for their support in
course development through the UAF Chancellor’s Innovation in Technology
and eLearning (CITE) Fellows Program. Our collaborators at eScience Labs,
15
especially Scott Higgins, Ellen Thompson, and Valarie Houghton for taking
on this course as a labor of love. Our external evaluator, Lori Sowa, nd the
UAF Alaska Summer Research Academy (ASRA) program for supporting the
translation of this work to middle and high school audiences. Support for this
project was provided by the UAF Office of Undergraduate Research and Scholarly
Activities through a 2015 Mentor Award, and the UAF BLaST program through
a Curriculum Development Project. Research reported in this publication was
supported by the National Institute Of General Medical Sciences of the National
Institutes of Health under Award Numbers UL1GM118991, TL4GM118992, or
RL5GM118990. The content is solely the responsibility of the authors and does
not necessarily represent the official views of the National Institutes of Health.

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19
 Chapter 2

Community-Based Undergraduate Research:

Measurement of Hazardous Air Pollutants with
Regard to Environmental Justice
Kathryn Zimmermann,*,1 Laura Young,2 and Kelsey Woodard3
1School of Science and Technology, Georgia Gwinnett College,

1000 University Center Lane, Lawrenceville, Georgia 30043, United States

2School of Liberal Arts, Georgia Gwinnett College,

1000 University Center Lane, Lawrenceville, Georgia 30043, United States

3Center for Teaching Excellence, Georgia Gwinnet College,

1000 University Center Lane, Lawrenceville, Georgia 30043, United States

*E-mail: kzimmermann@ggc.edu.

Environmental justice focuses on disparate exposures of

communities to pollution based on race, national origin,
or income level. This collaborative study, which paired
faculty and undergraduate students from political science and
chemistry disciplines with an external community advisor,
collected data to help bring environmental justice issues to the
forefront of discussions in their community. Interdisciplinary,
undergraduate researchers from Georgia Gwinnett College
measured gas-phase polycyclic aromatic hydrocarbons (PAHs),
using passive sampling methods, in communities with differing
demographic indicators. This undergraduate research project
leveraged student interest and motivation in social justice
themes to address a community-based question that combines
physical (environmental chemistry) and social science (political
science).

© 2018 American Chemical Society

 Introduction

Georgia Gwinnett College

Georgia Gwinnett College (GGC), a public, open-access, four-year, liberal

arts college in the University System of Georgia, opened in 2005. In the last
twelve years, GGC has grown exponentially from 120 students to over 12,000
students, with 67.7% enrolled as full-time undergraduates (1). GGC was recently
ranked as the most ethnically diverse college in the South (2), and has the
distinction as an emerging Hispanic Serving Institution. Many of GGC’s students
are self-supported, first generation college students, and, as of Fall 2016, 52% of
GGC students were Pell Grant Eligible (1). GGC offers an unique opportunity
to gain higher education, often admitting at least 80% of applicants. The student
demographics as of Fall 2015 are listed below in Table 1, exemplifying the
diversity of the college as a whole, the school of science and technology (SST), the
school of liberal arts (SLA), and the student demographics in the Environmental
Justice Community Innovations Project (EJ-CIP) conducted during the 2016-2017
academic year.

Table 1. Demographic distribution of student population of the entire college

(GGC), the SST, the SLA (1), and the undergraduate project described in
this chapter (EJ-CIP)
Demographic % % % First % % Above
Black Hispanic Generation Female the age
College Studenta of 23
GGC 32.6 16.9 41.7 56.2 24.6
SST 33.3 16.3 38.8 44.4 25.2
SLA 37.2 17.6 40.5 63.6 27.0
EJ-CIP Projectb 57.1 0 N/S 85.7 28.6
a For the Fall 2015 semester, 2,469 students who did not provide first-generation information

are excluded from the sample (1). b Demographic information for the EJ-CIP Project was
collected using self-reported data from a student survey of the project. N/S corresponds to
data that was “not surveyed” in this questionnaire.

The EJ-CIP undergraduate research project brought together an

interdisciplinary team of two GGC faculty members (Political Science
and Chemistry) and seven undergraduate students. GreenLaw, a non-profit
environmental law firm based in downtown Atlanta, served as the
community-based external advisor to the project. The environmental justice focus
of the project served to leverage student interest and motivation in the application
of both social and physical scientific practices to a community-based issue. The
outcome goals of this undergraduate research project were multifaceted and listed
as follows:

22
 • Motivate and engage students in applied research and experiential
learning through a community-based, interdisciplinary project;
• Integrate students with an external advisor, as well as other members, in
their regional community;
• Improve student knowledge of environmental justice history, policies,
and research; and
• Improve interdisciplinary communication and understanding at an
undergraduate level.

Experiential Learning at an Open Access Institution

GGC, and other public, four-year universities of its kind, are met with various
challenges and opportunities to meet the demands and needs of their diverse and
open access student population (3). To address some of these challenges at GGC
and other institutions, the University System of Georgia (USG) Board of Regents
became an official partner of the Liberal Education and America’s Promise
(LEAP) Initiative under the Association of American Colleges and Universities
(AACU), forming a consortium called LEAP State Georgia Consortium. In 2005,
the AACU’s LEAP Initiative was launched with a call to national public advocacy
and campus action, responding to contemporary demands for an increase in
college-educated workers and more engaged and informed citizens. Termed as
high-impact educational practices, LEAP activities are a parasol of experiential
education, widely tested and shown to engage and challenge students. They are
also proven to increase rates of student retention and be beneficial for college
students of various backgrounds (4, 5).
The Association for Experiential Education defines this practice as “a
philosophy and methodology in which educators purposefully engage with
students in direct experiences and focused reflection in order to increase
knowledge, develop skills, clarify values, and develop one’s capacity to contribute
to their communities (6).” In other words, the process through which a learner
constructs knowledge, skill, and value from direct experience is called experiential
learning (EL). These direct experiences take on various forms, including first-year
seminars and experiences, community service, fieldwork, sensitivity training
groups, internships, cooperative education with community partners, participation
in faculty-led research, service-learning, and community-based learning and
research, the latter of which will be explored in the next section.
Renowned philosophers, educators, and trailblazers of the EL approach,
Aristotle, John Dewey, David Kolb, Kurt Lewin, and Jean Piaget, all believe
that true learning takes place when the experience allows the student to 1)
harness their own learning, both in and outside the classroom; 2) bridge prior
and current knowledge; 3) serve a societal and individual learner purpose; and 4)
realize-life/world application. Speaking to the harnessing, bridging, purpose, and
application, Dewey (7) believed that educators (faculty) must understand and take
into account human experience, stating that “Education is not preparation for life;
education is life itself.” By doing so, faculty serve as facilitators of learning and
become better reflective practitioners, bridging the traditional and progressive
sides of education.
23
GGC’s Community Innovations Project Program
In 2015, a survey by Hart Research Associates on behalf of the AACU
demonstrated that employers place a high priority on collaborative team work and
application of skills to real world issues when hiring recent graduates (Figure 1)
(8). However, this survey also showed a disconnect between the skill sets desired
for employment and employers’ ratings of these skills in newly hired graduates
(8). In an effort to address this incongruity in expectations and observations
of employers, to align with LEAP’s charge, and to support GGC’s vison and
mission, GGC’s Center for Teaching Excellence (CTE) supported the creation
of the Community Innovations Project (CIP) program. The goal of this program
is to encourage engaged, public scholarship, giving students an opportunity
to work alongside faculty on interdisciplinary projects which are considered
important to (and defined by) members of the community. Such an opportunity
integrates faculty roles of teaching, research, and service, allows students to
gain hands-on experience putting their knowledge into practice, and cultivates
genuine, intentional relationships with the community.

Figure 1. Top: Percentage of employers that rated the described skills as

very important for recent graduates to have. Bottom: Percent of “much”
greater likelihood of hire if recent college graduates have had the following
experiences. Reprinted with permission from Falling Short: College Learning
and Career Success. Copyright 2015 by the Association of American Colleges
and Universities (8).
With its underpinnings in service learning, the pilot CIP program is a form of
community-based research (CBR), where expertise is derived from community
members themselves. Community members are the content experts and voice of
expression for the community’s need for interaction with the academic institution.
This interaction allows for reciprocity and supports a mutually beneficial
relationship between key players (students, faculty, community members/external
advisors, and institutions). This also allows for a true intergenerational partnership
24
of learning to occur, thereby fostering learning communities to meet the call of
nurturing civic minded students and future leaders. Principles of CBR are (9):

• To create a collaborative relationship between members of the

community and researchers (professors and/or students). It engages
university faculty, students and staff with diverse partners and community
members;
• To validate multiple sources of knowledge and encourage the use of many
methods of discovery and of distribution of the knowledge produced; and
• To create a form that is also participative (among other reasons, change is
usually easier to achieve when those affected by the change are involved)
and qualitative.

The CIP program was inspired by a similar program currently employed at

Harvey Mudd College. The Clinic Program, a hallmark of the Harvey Mudd
College for over 50 years, focuses on small groups of undergraduate students
working for corporate and government sponsors to design, develop, or conduct
research according to the needs of the sponsor (10, 11). The CIP program takes
a similar approach, but implements this community-based EL at an open-access,
liberal arts, institution. In Spring 2016, the pilot program successfully launched
a request for proposals for interdisciplinary faculty/student teams to work on a
one-year project addressing real-world problems, identified as important by a
local external community partner organization, such as a for-profit company,
not-for-profit organization, governmental agency, or non-academic unit of GGC.
Project teams consisted of two or more GGC faculty Principal Investigators
(PIs), three or more students (junior standing), and an advisor from an external
organization. Grant awards were in the amount of $7,000 for each one-year
team project, with $3,000 allocated to faculty for summer stipends during project
planning. Using the PARE (Prepare, Action, Reflection, and Evaluation) Model
as a guide, the CTE held a pre-planning summer orientation to curate a supportive
environment and explore topics including types of EL pedagogy, student
learning outcomes and expectations, importance of reflection, community partner
relationship and expectations, logistics and risk management, and mandatory
project reporting dates. The CTE also communicated with external advisors
regarding the CIP process, expectations, and memorandums of understanding
(MOUs).
At the end of the academic year, all projects were expected to result in a
deliverable, such as a formal report, presentation, or prototype/work of design,
etc. All project teams were also required to make a formal presentation at the end
of the academic year. During the pilot year, two projects were funded, including
the EJ-CIP project focused on environmental justice with regard to hazardous air
pollutants. With evaluation feedback from 2016 – 17 pilot CIP teams, the program
has continued for another academic year, providing Grantmanship Informational
sessions for interested faculty teams, focusing on professional development in
proposal writing and discussion of opportunities and challenges presented by
previous awardees.

25
Environmental Justice and Air Pollution

The United States Environmental Protection Agency (U.S. EPA) defines

environmental justice as the “fair treatment and meaningful involvement of
all people regardless of race, color, national origin, or income with respect to
development, implementation, and enforcement of environmental laws (12).”
Although environmental justice is not universally defined, it usually refers to
the belief that citizens of a certain ethnicity or socioeconomic class should not
disproportionately face the burden of the externalities related to pollution and
other environmental health hazards. Though there are different interpretations
of this term, most definitions share the common theme of justice in distribution,
procedures, and process (13).
Air quality, which can negatively influence human health (such as rates of
asthma and negative effects on the cardiopulmonary system) (14, 15), has been
previously studied with respect to environmental justice. Several studies, focusing
on atmospheric particulate matter (PM), have shown that minority and low income
communities have higher exposure to environmental contaminants via air pollution
(16–20). Apelberg et al. (21) found that on-road sources of air toxics might
be an area to focus policy changes with respect to reducing the disproportionate
health burden of air pollution based on socioeconomic status or race. This is
important because, while the National Ambient Air Quality Standards (NAAQS)
monitoring provides data for exposure differences between communities for air
quality parameters such as CO, lead, NO2, O3, PM and SO2, less is known about
the distribution of exposure to toxic hazardous air pollutants (HAPs). This is due to
the diverse chemical properties and the number of molecules categorized as HAPs
(22, 23). Two previous studies (24, 25) have shown that, due to mobile sources
(such as high traffic density), exposure to air toxics and the associated risks are
disproportionately shouldered by minority and low-income communities. As a
result, the EJ-CIP project investigated environmental justice with respect to HAPs,
focusing on polycyclic aromatic hydrocarbons (PAHs).
The topic of environmental justice is of particular importance in the state of
Georgia, since, as of 2010, it is one of only five states that has not addressed
environmental justice in the form of any initiatives, task forces, programs, or
employees working at the state level (26). Thus, one aim of this study was to
analyze the spatial variability in concentrations of gas-phase PAHs and possible
correlations of PAH concentrations with demographic indicators such as percent
minority population, percent linguistic isolation, or percent below poverty level.
A second goal for this study was to provide preliminary data and proof of concept
for using passive air sampling as a method to build a database of spatial HAPs
concentrations that can be used to support community discussions and policies
regarding environmental justice and air quality.

Interdisciplinary Undergraduate Research: Importance of Combining

Political Science and Environmental Chemistry

Higher education is increasingly looking for ways to facilitate

interdisciplinary communication. In fact, interdisciplinary curriculum was
26
found to be the “number-one issue in American education (27).” This focus is
because of the many benefits due to increased conversations amongst disciplines.
Specifically, interdisciplinary education encourages critical thinking within
one’s own discipline and leads to more holistic approaches to solving some of
the world’s more complex, pressing issues, while improving self-discipline.
Interdisciplinary education also prepares students for modern working conditions
that call for increasing amounts of multi-professional teamwork, giving future
generations further ability to consciously approach complex problems in group
settings with colleagues of different skill sets (28). Increasing communication
and collaboration in non-traditional academic groups also typically leads to an
increase in creativity (27).
Embarking on interdisciplinary research or teaching requires focus on
thematic integration, which becomes the organizer and a driver for the curriculum.
Knowledge integration is also important. This “is achieved when interactive and
connective relationships…are established between the knowledge and skills in
the two or more disciplines (27).” Special attention must therefore be placed on
finding a common link between the disciplines and focusing on the skills needed
to understand those links. This means learner-initiated integration is also key
because it helps lead students to discover connections. This is done by placing
a value on independent thinking which can help the student ask questions and
find connections between the disciplines; “to develop sequential understandings
in separate areas of knowledge and skill; and to establish thought patterns
or mindsets that lead them to look for” the necessary links and “connective
relationships across all areas of learning (27).” The topic of environmental justice
(the subject of the EJ-CIP research project) provides thematic integration to
engage multiple disciplines because of the interdisciplinary nature of the topic
itself.
Specific to the issue of environmental justice, physical scientists must
gather data and quantify exposures of different populations to HAPs, and policy
specialists must analyze demographics of different communities, examine policies
currently in place that address this issue, and generate ideas for moving forward
with evidence-based policies. Thus, environmental justice combines a mixture
of scientific expertise, socio-economic analysis, and a knowledge of legal and
historical requirements. For example, public policy experts are interested in why
certain groups are targeted with externalities related to pollution, why the targeted
groups are unable to fight against policies that affect them negatively, and why
regulatory efforts by policymakers may fail to protect vulnerable populations.
Those interested in health policy use the level and type of exposure to understand
what policies should be adopted to combat health related issues in differing
regions or communities. Public administrators focus on issues related to urban
planning, including the regulations and laws dictating the placement of polluting
facilities. Alternatively, political economists aim to understand the impact of
pollution on the economy. Political economists can also combine their work with
health policy experts to determine the number of sick days missed from work
due to environmental justice issues and the impact these absences have on the
economy as a whole.

27
 The environmental justice work of public policy experts would not be possible
without the data provided by physical scientists such as chemists, biologists, and
epidemiologists. The work of physical scientists is essential for collecting the data
analyzed by policy experts to answer the questions they pose and to implement
evidence-based policies (29). Specifically, chemists are able to analyze complex
mixtures to quantify HAPs in communities, giving an estimation of exposure rates
to different toxic compounds. Biologists can use mouse-model studies or cellular
assays to assess the toxicity of different compounds or the possible synergistic
effects of mixtures. This work combines with that of epidemiologists using cross-
sectional or longitudinal studies to assess human health effects of exposure.
One of the challenges faced by the teaching and learning of both political
science and chemistry (the two disciplines most heavily combined in this project)
is to maintain relevance in the eyes of students. During the EJ-CIP project, the
thematic integration of the two fields to investigate social justice issues in the form
of exposure to toxic air pollutants was used to demonstrate the relevant nature
of both fields in the lives of students and their communities. One goal of such
project-based research within the community is to give students the opportunity
to link expertise gained from coursework with application to a real-life challenge
and the ability to drive or direct positive change. For example, students who study
public policy (SLA students) may encounter challenges interpreting the source or
meaning of chemical exposure data. SST students, on the other hand, may not
see the relevance of their work or how it can possibly impact policy decisions.
This deficiency in interdisciplinary understanding from both fields can result in
the impediment of sound future policy analyses and implementation.
In sum, from an environmental justice perspective, there is an intimate
link between science and public policy. This relationship also exists between
policy and other scientific endeavors, since funding for a variety of scientific
investigations is often influenced by public policy and it is imperative that
public policy is evidenced-based and data-driven. Since this mutualism between
policy-makers and scientists makes it necessary that communication between the
two fields flows efficiently (29–32), it is important to introduce undergraduate
students to the role of science in public policy and vice versa. Thus, the EJ-CIP
project integrated students on an interdisciplinary level, early in their career
development, aiming to strengthen communication across the policy and physical
science disciplines.
Previous approaches to this challenge have included curriculum development
for upper level chemistry courses that include problem- and project-based
learning with an environmental focus (31, 33–37). However, teaching chemistry
with public policy implications and themes only confronts one-half of the
communication challenge. Interdisciplinary communication must be encouraged
in both directions. Not only must physical science students understand policy
implications, but political science students must also be proficient in the scientific
method and data interpretation. As a result of the above challenges, effort in
the EJ-CIP study was directed to require students to work outside of their field
of expertise. SLA students worked alongside SST students in the field and
laboratory, while SST students worked with SLA students on demographic and
policy analysis (Figure 2). This encouraged students to ask questions of one

28
another, communicate openly, and discover important relationships between the
social and physical sciences, resulting in facilitated dialogue between future
policy makers and scientists from an early stage in their careers.

Figure 2. A Venn diagram which shows the interdisciplinary nature of the project,
in which students from both fields of expertise were required to conduct methods
and work in the field of their collaborators.

Experimental Methods
Interdisciplinary Nature of the Research Team

This project integrated students into a field of study that was beyond their
current realm of expertise, aiming to improve dialogue and understanding between
science and policy. Students worked collaboratively within this team to reach
a goal (obtaining and disseminating results), which encouraged the growth of
beneficial hard and soft skills, including, but not limited to, conducting research
in an experiential and quantitative fashion, communicating technical information
both orally and in writing, and working in real world, modern conditions in their
respective fields. Via their external advisor, GreenLaw, students interacted with
professionals outside of the college, to see the operation of environmental law
and advocacy groups first-hand, as well as to make contacts with professionals
having similar interests and goals. Although it is possible for the SST and
SLA aspects of this program to stand alone, the interdisciplinary nature of the
program allowed students and faculty to gain experience with environmental
chemistry analyses while simultaneously engaging in an upper level policy
analysis. Collaboration with outside groups also added an additional component
of community engagement that encouraged the development of professional soft
skills outside of the typical college setting.
Importantly, students with different academic backgrounds worked together
to solve a complex problem relating to their community. The team consisted of
seven students from three different disciplinary backgrounds. Two students were
29
majoring in biochemistry, one in environmental science, and four were political
science majors concentrating in legal studies. The political science majors had
very limited knowledge regarding the science needed to inform policymakers nor
were they experienced with lab work. The biochemistry students, however, were
unaware of the policy implications related to the work they often performed in
the lab. For the environmental studies student, the interdisciplinary nature of the
project helped to consolidate the knowledge learned inside the classroom with
actual fieldwork and lab experience.

EJSCREEN
Seven sites were chosen for analysis, with each student choosing a site to
research. This format gave students “ownership” over the data collection and
analysis specific to their site. Students used the EJSCREEN tool, a publically
available database provided through the U.S. EPA (38). EJSCREEN “allows
users to access high-resolution environmental and demographic information for
locations in the United States, and compare their selected locations to the rest of
the state, EPA region, or the nation (38).” It should be noted that screening-level
tools, such as EJSCREEN, are limited in scope and data, and therefore, do
not determine the existence or absence of environmental justice concerns in
a specific geographic location (38). Thus, this project used EJSCREEN to
select possible sites of inquiry and then followed with subsequent chemical
measurements and demographic analyses. Students investigated the demographic
distributions of several possible sites, but also investigated the predicted air
pollution environmental indicators provided by EJSCREEN such as, particulate
matter less than 2.5 microns in aerodynamic diameter (PM2.5), the national air
toxics assessment (NATA) diesel PM, and NATA air toxics cancer risk. These are
described as follows:

• PM2.5 (annual average concentration, µg/m3, calculated from a

combination of air quality monitoring sources);
• NATA Diesel PM (concentration of diesel PM estimated in µg/m3); and
• NATA Air Toxics Cancer Risk (estimated lifetime inhalation cancer risk
using emissions estimated from the National Emission Inventory (NEI));

Sampling sites in the Atlanta metropolitan region were chosen based on these
environmental indicators, as well as, several demographic parameters listed below
(38):

• Percent low income: The percent of people in a location living in

households where the income is less than or equal to twice the indicated
federal poverty level;
• Percent minority population: The percent of people in a location who
have listed their racial status as something other than white and/or list
their ethnicity as Hispanic or Latino; and
• Percent linguistic isolation: The percent of individuals in a location living
in a household in which all household members older than 13 speak a
30
 non-English language and also speak English less than what is considered
very well.

Data for these demographic parameters for each site are listed below in
Table 2.

Table 2. Demographic data obtained for each site from EJSCREEN (38)
Site ID % Low income % Minority %Linguistically
Isolated
A 15 19 0
B 24 90 0
C 49 63 6
D 54 87 11
E 77 66 9
F 27 38 12
G 36 16 0

Students were required to contact sites to gain permissions to hang samplers.

This included providing a description of the proposed project, details of samplers,
timelines, etc. The calls also allowed students to practice discussing the
importance of the reasons behind their work, thus increasing the awareness of
environmental justice issues in the state of Georgia. Selected sites for hanging
samplers included several elementary schools, a science nature reserve, several
Georgia Environmental Protect Division sampling sites, and a private residence.

Passive Air Samplers and Laboratory Techniques

For this pilot study, students’ initial focus included atmospheric PAHs. The
study aimed to quantify gas-phase concentrations of the 16 PAHs listed on the U.S.
EPA Priority Pollutant List (39). PAH sources include incomplete combustion
processes such as vehicle (diesel) emissions, residential activity and industrial
heating (40). PAHs have shown mutagenic properties in bacterial and mammalian
assays, and are classified by the International Agency for Research on Cancer
(IARC) as probable human carcinogens (41–43). Combined with their tendency
to bioaccumulate, PAHs pose risks to both environmental organisms and humans
(44). Table 3 lists the analyte PAHs measured in this study, their associated
abbreviations, molecular structures and internal standards of quantitation.

31
Table 3. List of analyte PAHs (including abbreviations and molecular
structures) measured in this study

32
 Passive air samplers (PAS) were used in this study to measure the
concentration of PAHs at each site. These samplers, characterized and used
in many previous studies of ambient concentrations of gas-phase persistent
organic pollutants, are low cost and require no power during sampling, and
have not yet been deployed in the Atlanta metropolitan region. The PAS (Tisch
Environmental; Cleves, OH) have been thoroughly characterized and their
method of operations previously described (45, 46). In brief, the PAS includes a
polyurethane foam disk (PUF, ½” height x 5 ½” diameter; part number TE-0114)
held inside of a stainless steel dome used for protection against precipitation,
deposition of particulate matter, UV light, and the influence of wind speed (47).
They operate based on the air-side mass transfer coefficient and the PUF-air
partitioning coefficient of each analyte (45), and thus, require no outside power
source for a pump, are quiet and non-invasive, and are a relatively inexpensive
way to increase spatial resolution of gas-phase PAH concentrations. PAS are
ideal for this type of study, in which spatial resolution of samples is important,
compared to traditional samples methods (such as high volume air samplers),
because PAS allows for simultaneous measurements at several different sites at a
time, generally prohibited with tradition sampling methods due to high cost and
person-hours needed to change sampling media. Similar PAS systems have been
used in several large-scale studies to measure atmospheric PAH concentrations
(46–52).

Figure 3. PAS deployed at Site C using non-invasive measures (zip ties and
hose clamps).

Prior to deployment, sample domes (Figure 3) were cleaned with acetone

and PUFs were pre-cleaned via Soxhlet extraction in a 50/50 acetone and hexane
mixture (Fisher Scientific, Optima) for 24 hours. Samplers were deployed at sites
selected by students starting in January 2017, and hung at heights ranging from
166 cm – 182 cm to represent a ‘human height’ exposure concentration. Dates
of deployment ranged from January 10, 2017 to March 17, 2017. Preliminary
analyses estimated the average sampling rate of these samples to be 5.0 m3d-1 (46,
47, 51, 52). Table 4 shows deployment characteristics for each site.

33
 Table 4. Deployment characteristics for each site
Date Total #
Site Latitude Longitude Site Type Deployed Sample Days
A 34.075402° -83.87047° School 1/17/2017 37.0
B 33.571235° -84.61902° School 1/10/2017 51.9
C 33.828622° -84.11447° Residential 2/4/2017 31.0
D 33.963097° -84.06922° GA EPD 1/11/2017 54.0
E 34.299359° -83.8134° GA EPD 1/13/2017 41.9
F1, F2 34.257762° -83.84541° Forested 1/13/2017 42.0
G 33.729485° -84.37091° Residential 2/4/2017 40.8

Method blank extracts were collected by subjecting clean PUFs to the same
laboratory and analytical procedures as sample PUFs. Two field blanks were
collected by packaging clean PUFs in aluminum foil, plastic bags and mason jars,
transporting them to the sampling site in the same manner as the sample PUFs,
placing the field blank PUFs in the stainless domes for approximately one minute,
and then storing under similar conditions as sample PUFs until extraction and
analysis. It should be noted that the only site where replicates were measured
was Site F (samples F1/F2). All PUFs were stored in aluminum foil, plastic bags,
and mason jars at 30°C until extractions were performed.
PUFs were spiked with a mix of deuterated internal standards (NAP-d8,
ANT-d10, FLA-d10, and BaA-d12, Supelco, TraceCERT) for quantitative purposes
and Soxhlet extracted in 50/50 hexane/acetone (Fisher Scientific, Optima) mix
for 24 hours. Samples were then concentrated under rotary evaporation and
eluted through silica solid phase extraction (SPE) columns (Discovery DSC-Si,
Sigma Aldrich) using a 50/50 mixture of hexane and dichloromethane (DCM,
Fisher Scientific, Optima) mix. Extracts were brought to a final volume of ~
200 µL using nitrogen flow (53). All PUF extracts were analyzed with gas
chromatography- mass spectrometry (GC-MS) using a Shimadzu QP2010S,
operated with EI ionization and SIM mode. Samples were injected at 280° C in
splitless mode, and separations were completed on a 30 m x 250 µm i.d. (film
thickness 0.25 µm) SHRXI-5 MS column (Shimadzu). The initial temperature
of the column was held at 70°C for three minutes, and then increased at 20°
min-1 to 315°C and held for 30 minutes. Retention times confirmed with a PAH
mix standard solution (EPA 610 PAH mix, Supelco) and concentrations were
calculated relative to the added deuterated internal standards.

Student Deliverables
Blog
Student reflection helps facilitate learning and keeps students fully engaged
(54). It is therefore important to find ways that help students reflect on the material
they learn. Blogs are a great tool for classroom use since they require students to
34
reflect on their work in a digital environment familiar to today’s student. Blogging
also allows students to create an online portfolio that highlights their work that
they can share with family, friends, potential graduate schools, and employers. As
a result, this project required students keep a weekly blog updating the progress of
the project and the specific work they performed.
Students began their blog by summarizing the goals of the project and
discussing the importance of investigating issues related to environmental justice.
After the initial post, students shared their experience selecting site locations,
the new skills they learned in the laboratory, the knowledge they gained related
to environmental policy, their experience visiting site locations and placing the
air samplers, as well as meeting with members of the community. In addition
to reflections on their work, students also posted photographs and supplemental
information to enhance the substance of their reflections. The result was a
professional online portfolio useable to display skills and accomplishments when
applying for graduate school or employment.
Students also reflected on the experiences they had at their meeting with the
external advisor, GreenLaw. Students not only discussed the substance of the
meeting, but also reflected on how the classroom and laboratory work transferred
to real world professional endeavors to solve issues of environmental justice. The
connection with what they learned and how it applied to future career possibilities
is particularly useful since it helps students see beyond the classroom experience
to how these skills can transfer to their future career goals.

Site Reports
Students’ site reports made it easy to record and organize data for later
analysis to determine what, if any, factors may contribute to the amount of
pollution in an area where samplers were placed. The reports included basic
geographic information, demographic statistics, and identification of polluting
businesses and industry located in the area of sample placement. For this project,
each student was assigned a particular location for which they generated the
site report. The reports were divided into several sections. The first section
covered basic location and geographic information about the sampler location.
Demographic information, such as population levels, percentage of individuals in
different minority groups, income levels, and education levels were included. In
addition to basic demographic information, the report included a section to record
health statistics of individuals living in the area. The third section of the report
included information about area pollution. The percentile of PM2.5, NATA Diesel
PM, and NATA RHI were estimated using the EJSCREEN information (38).
Information about current and past industries that may contribute to pollution
surrounding the sampler placement was also included. Details about these
industries included the name and address of the business, the type of industry,
and a summary of possible pollutants created by that particular industry. The
final section of the report included the actual data collected from the air samplers
placed in the field by the students.
To gather information for the report, students conducted on-site visits to
survey the geography of the area and determined present conditions where
35
samplers were placed. USGS and Google Maps were also used to learn more
about the topography of the sampler location. An examination of municipal and
county planning files as well as searches with local public agencies were checked
for prior and current land usage and permits in the area. This information helped
students locate current and past polluting industries. The Health Department
provided statistics about the health of individuals within a county, though this
information proved to be more difficult to find for most students, and was not
spatially resolved to the level of our chemical measurements. Demographic
information was primarily collected using statistics provided by the EJSCREEN,
but also compared to census data when available.
In some cases, students gained information on history of a location through
informal interactions with community members. For example, through interaction
with community members in Gainesville, GA, students learned of the Newtown
story and the Newtown Florist Club (55). The predominantly African American
residents living in the Newtown neighborhood exist alongside 14 polluting
industries within a 1-mile radius of their community. Members of this community
have suffered from high incidences of lupus, and specific types of mouth, throat,
and lung cancers. The Newton Florist Club is a grassroots organization that has
organized to bring awareness to their fight for environmental justice. This is
a community who has historically struggled with issues of environmental (in)
justice and brings light to the complex nature of proving and solving these types
of issues. These sources provided information for the environmental justice
struggles of a community less than 30 miles from GGC, giving the students a local
context with respect to the need of sound measurements and policies regarding
environmental justice.
When site reports were completed, students met to discuss their findings and
analyze the results. They also shared their reports on their individual blogs. Not
only were the reports useful for helping students organize the data they needed to
collect for analyzing the sampler results and drawing conclusions about the sources
of pollution and its impacts, but they also provided a deliverable that students can
share with potential employers and graduate schools.

Presentations and Outreach

Students took part in multiple presentations during the project. The first
was given to the community-based external advisor, GreenLaw. At this meeting,
students were hosted for the morning at the non-profit environmental law firm in
downtown Atlanta. Students met with several attorneys and interns to discuss the
project and relevant environmental justice case law, history, and current policies
existing in Georgia. Students provided a formal presentation to the attorneys,
sharing the overall goal, project plan, and the research design they developed
for this study. When completed, students received advice for improving their
research design and discussed how collaboration would take place during the
remainder of the project.
Students were also invited to present at the 2016 Energy Symposium held at
Georgia Gwinnett College. Although the focus of this event was energy security,
the hosts felt the work the students were doing not only related to the importance
36
of finding clean energy alternatives, but also wanted to highlight alternative
means by which the topic of energy security can be taught. Specifically, students
discussed the relationship of fossil fuels and air pollution and its impact on the
health of individuals. They shared demographic data related to areas affected
by air pollution, and argued that certain communities were disproportionately
disadvantaged compared to others because of the current reliance on fossil
fuels. After discussing their experimental design and hypotheses (since, at the
time, data collection was not complete), the students discussed the benefits of
clean renewable energy solutions and the greater impact it would have on those
communities more likely to suffer from the externalities of fossil fuels. Not only
was this experience beneficial because it helped students relate their project to
larger environmental issues, but several prominent scholars, including a member
from the United Nations, were present. Thus, students were able to network
with professionals in academia as well as in high-level government positions, an
experience not typically granted students in a traditional classroom setting.
Two senior biochemistry students traveled to present preliminary results at
the annual Spring American Chemical Society (ACS) meeting in San Francisco,
CA. This was the first national meeting at which either student had either attended
or presented. One of these students is currently pursuing a Ph.D. in Chemistry
at University of Georgia, and the other is in the process of applying for graduate
school. In addition, the entire group of students presented at the annual Georgia
Gwinnett College CREATE Symposium. The CREATE Symposium gave students
an opportunity to share their work on the project with their fellow students as well
as other faculty members on campus. During this presentation, students explained
the purpose and goals of the EJ-CIP project. Most of the presentation, however,
shared the results of the research and discussed the importance of the project to
the Atlanta metropolitan region.
The students also had the opportunity to communicate the goals and results
of their project to middle-school age campers at the Elachee Nature Science
Center during the summer of 2017. Two students from the project attended an
afternoon of summer camp to lead a group of 12-14 campers in the activity of
making Schoenbein paper. This relatively inexpensive activity allows participants
to create their own colorimetric measurement of tropospheric ozone (considered a
criteria pollutant by the EPA) using the oxidation of iodine (clear to purple/brown
color change). This outreach activity allows for the discussion of the importance
of air quality, the effects of air quality on the health of sensitive populations
(children and elderly populations), and well as the introduction of environmental
justice pertaining to air quality. In the future, the goal of such projects will be
to hang PAS at elementary and middle schools, and have the students at such
schools participate in ozone data collection using Schoenbein paper during the
time that the PAS is hung on their property. This type of outreach collaboration
will include K-12 students helping to collect semi-quantitative data in an active
research project.
Each of these presentations gave students an opportunity to not only share the
project goals and results, but also their experience working on an interdisciplinary
project and the benefits this type of collaborative approach had on their overall
educational experience. In addition, students gained exposure presenting in a

37
professional setting and were able to network with business professionals as well
as community and global leaders.

Preliminary Data Generated by Undergraduates

PAHs quantified included NAP, ACY, ACE, FLU, PHEN, ANT, FLA, PYR,
BaA, CHR, B(b+k)F, B(a)P, I123P + DBA, and BgP. Separation of 14 out of 16
analyzed PAHs were achieved with the method, with B(b)- and B(k)F reported as
a sum of the two isomers, as well as I123P and DBA. Retention times of analytes
in sample extracts were confirmed by retention times of standards (see Figure 4).

Figure 4. Chromatograms of standard PAH mixture (top), and site A extract

(bottom). Peaks are labeled according to Table 3 with (-dx) representing a peak
of a deuterated internal standard.

38
 Preliminary results from the analysis of six sites in the Atlanta metropolitan
region regarding total PAH concentrations using PAS techniques are shown
in Figure 5. While statistical analysis of variance could not be performed on
single samples (replicates were only measured at one site), upon initial analysis,
concentrations of PAHs at site A were two times greater than the average
concentration of all other sites. This sampler was hung on a fence bordering the
parking lot of an elementary school, where it was thought that buses idled prior to
loading students for transport at the end of each school day. Although a height of
166 cm was used to approximate exposure for an average adult, it may not havee
allowed for complete mixing of an air parcel prior to sampling. As a result, the
data for this site was considered as an outlier and was not used in the combined
chemical concentration and demographic analysis (shown in Figure 7).

Figure 5. Total PAH concentrations (pg m-3) for six sites in the Atlanta
metropolitan region. Samples F1 and F2 represent replicate samplers hung at
site F. These were the only replicate samples taken during this pilot project.

Replicate samples at F1 and F2 demonstrated a small amount of variability,

showing the importance for providing replicates at each sampling site. Upon
analysis of the distribution of PAHs at each site, preliminary analysis shows
differing compositions of the samples for different sites (Figure 6). The most
prominent PAH in each sample was PHEN, followed by varying contributions
from FLU, FLA, PY, and ACE. Preliminary analysis notes that Site F, our most
forested site (Elachee Nature Science Center) contained more ACE than other
sites, and Sites B and C have similar PAH profiles, despite being located over
40 miles from one another. It should also be noted that several semi-volatile
and non-volatile PAHs were measured with the PAS. Although these sampling
devices operate based on partitioning of analytes between the gas- and PUF-
phases, it has been shown previously that particulate matter can be collected
(46, 56). The difference in distributions of PAHs amongst sites suggests that
further investigation is needed into source differences or distances from sources
(photodegradation during atmospheric transport).

39
 Figure 6. Distribution of PAHs for Site A (top left), Site F (top right), Site B
(bottom left) and Site C (bottom right). PAHs that appear in over five percent are
represented structurally, according to pie chart color.

Students compared total sum of PAHs (pg m-3) to the demographic

information collected at each site for a preliminary environmental (in)justice
analysis. Preliminary regression analysis gives the respective coefficients of
determination shown in Figure 7. However, possibly due to our small number of
samples (n = 6 in this analysis) and the lack of replicate measurements, the data
shown in Figure 7 are inconclusive to the presence or absence of environmental
(in)justices regarding PAHs (p > 0.05). Therefore, these correlations can be
considered insignificant with respect to this study. However, this preliminary
analysis is meant to demonstrate a proof of concept that these PAS could be
used to increase spatial resolution of HAP concentrations on a large scale, thus
increasing the strength of the dataset for exposure to the chemicals for different
communities. For future studies containing a higher number of sampling sites (n
> 50), sample sites should not only vary in demographic parameters, but also in
distance from freeways and point-source contributions. Higher resolution GIS
measurements should also be used for more conclusive interpretation of results.

Influence of Interdisciplinary Community-Based Research on

Student Outcomes
Students (n = 7) were presented with a survey of attitudinal opinions using
an experience gains scale with question styles modeled after the survey of
undergraduate research experiences (SURE) (57). The students were presented
with the survey approximately six months after the conclusion of the project
and all seven students responded to the survey. Of these students, 71.4% had
not previously participated in an undergraduate research project at GGC, 42.9%
40
were from the SST and 57.1% were from the SLA. Students were asked to rate
different parameters based on their experience during the EJ-CIP project as either
a negative change, no change, small positive change, moderate positive change,
or large positive change. The results from this survey are displayed in Table 5.

Figure 7. Correlation plots showing relationships between total sum of PAH

concentration for each site as a function of % minority population (top), % low
income (middle), and % linguistic isolation (bottom).

41
 Table 5. Results of student survey after EJ-CIP participation
Parameter assessed % Participant Response
Perception that scientific inquiry can be applied in 71.4% Large change
everyday life 28.6% Moderate change
Understanding of how scientists work on real 57.2% Large change
issues/problems 28.5% Moderate change
14.3% Small change
Perception that research questions can be 85.7% Large change
successfully applied to address community issues 14.3% Moderate change
Confidence in your laboratory techniques 71.4% Large change
14.3% Moderate change
14.3% Small change
Confidence in communicating with researchers 85.7% Large change
outside of your major 14.3% Moderate change
Confidence in working on a project in which some 71.4% Large change
areas are outside of your expertise 28.6% Moderate change
Ability to work as part of a collaborative group 85.7% Large change
14.3% Moderate change
Understanding of the history of environmental 85.7% Large change
justice and current policies in place 14.3% Moderate change

The parameters that saw the greatest percent of students reporting a “large
positive change” included:

• Perception that research questions can be successfully applied to address

community issues;
• Confidence in communicating with researchers outside of your major;
• Ability to work as part of a collaborative group; and
• Understanding of the history of environmental justice and current policies
in place.

Thus, the survey suggests that goals were met with respect to increasing the
knowledge of undergraduates that academic research can be applied to community
issues, the confidence and ability of students to communicate and work outside of
their areas of expertise, and increasing awareness of environmental justice history
and issues in the state of Georgia. Students generally reported an increase change
for all parameters given, with the exception of “understanding that scientific
assertions require supporting evidence.” Several students, when asked to express
additional comments on the project offered:

• “It gave me (a social science major) the ability to understand that in

leadership positions where legislation is being implemented, it is very
important to merge with other disciplines and majors to gain as much
information as possible to make the best decisions;”

42
 • “The CIP made me realize the depth of work that can be done within the
legal profession to help society at large. As a result, I am better able to
focus more specifically on the type of legal career I wish to pursue”;
• “Working with other students with different majors, striving for the same
goal was inspiring as well as educational;” and
• “So grateful to have been able to work with a team from varying degree
programs.”

These comments suggest that the interdisciplinary nature of the project

was well received by students, and encouraged them to persist throughout the
term of the project. Based on these results, this project could be considered for
implementation at other institutions interested in leveraging student interest in
environmental and social issues to develop interdisciplinary research projects.

Future Goals
Several students have suggested that this research project be offered as
an official course, instead of just a faculty advised research project. The
interdisciplinary nature of the project lends itself to the newly developed
Environmental Science major here at GGC, which includes both a social science,
and a natural science track. Political science students have also expressed an
interest in participating in an official course such as this. They argue the active
learning approach as well as the integration with other fields like chemistry help
provide real world experiences that better connect the theories they study with
their application. In continuing this project, it is expected to increase the sample
number, number of replicates, and extend analyte analysis to include specific
polychlorinated biphenyl (PCB) congeners. This theme will be used as a full
semester long course integrated research project for the Environmental Science
Capstone Course (ESNS 4900) offered at GGC in Spring 2018.

Acknowledgments
We would like to thank our seven student researchers for their participation
and energy put forth into this project. We would also like to thank Mr. Lee
Irminger (Elachee Nature Science Center), Mr. Ken Buckley (GA Environmental
Protection Division), Evoline C. West Elementary, and Duncan Creek Elementary
School for their cooperation with hanging sampling devices. Special thanks to
our external advisor, GreenLaw, for hosting our students and providing valuable
feedback on their project plan. Faculty and support who were influential in
discussing and promoting this project include Dr. Charles Pibel, Dr. Brian
Etheridge, Dr. Aldolfo Santos, and Dr. Thomas Mundie. We thank the Georgia
Gwinnett College Community Innovations Project program and the School of
Science and Technology for funding. The results and contents of this publication
do not necessarily reflect the views and opinions of the external advisors or
collaborating partners.
43
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 Chapter 3

Undergraduate Research Experience

in Remote Sensing
A. Kahl*

Environmental Engineering, Penn State Greater Allegheny,

4000 University Dr., McKeesport, Pennsylvania 15132, United States
*E-mail: afk12@psu.edu.

The Multi-Campus Research Experience for Undergraduates

(MC REU) is an initiative to increase undergraduate research
at the Pennsylvania State University (Penn State), Greater
Allegheny. The MC REU program supports Penn State
undergraduate engineering students to conduct research with
Penn State faculty. Students participating in the program
complete a proposed engineering research project in conjunction
with two Penn State faculty members; one from the student’s
home campus and one faculty member based at University
Park. The objectives of the MC REU are: (1) to promote
undergraduate students participating in research early in their
academic program to broaden their education and increase
their chances of entering graduate studies; and (2) to promote
mutual awareness and collaboration among faculty across the
Commonwealth. This chapter details the results of two sessions
of undergraduate research in remote sensing, with special
emphasis on student engagement outside of the classroom and
collaboration with faculty.

© 2018 American Chemical Society

 Introduction

The purpose of the research is to build and establish a network of data loggers
across Western Pennsylvania to monitor water quality and observe salinization
trends. Data loggers are simple sensors that collect and store information over
time for a particular location. The problem with current water quality research
is the lack of data across a focus area. If a large network can be easily and
inexpensively built along streams and rivers in a focus area (in this case Western
Pennsylvania), more insight can be found on the causes of poor water quality in
drinking water sources. To do so, salinization measurements will give insight on
overall water quality. Salinization can be found with a measure of conductivity,
directly related to the concentration of total dissolved solids in the water (1).
The problem with recent brand name data loggers is that they are too intricate
and expensive for simple research purposes. What is needed to advance the
current state of knowledge is a simple yet robust sensor that is cheap to build and
easy to operate. Results from deploying this sensor will give an understanding
on the behaviors of the dissolved solids present in surface water such as salt.
Over time, the inexpensive data loggers have the potential to lead to a network
of sensors blanketing Western Pennsylvania, therefore increasing awareness of
water contamination issues. As the project is in its early stages, mapping the area
where these sensors will be deployed has not yet occurred.
Water quality data coupled with the emerging field of data science has the
potential to expedite scientific research and inform decisions about resource
allocation. One of the areas with the most potential for growth and innovation is
that of the water sensing. Current water sensors are large, cumbersome to use and
require specialized maintenance in order to gain reliable data sources. This limits
the number of sensors citizen groups can deploy as well as the duration that they
can be maintained. Smart systems, such as the internet of things (IOT) sensor
network in this work can help track contaminants at the backyard level and act
as first line avenues for data collection. The niche that citizen groups fill within
the water quality data nexus is currently small due to the limited availability and
accessibility of water quality sensors. Increasing data yields in a measurable way
through inclusion of IOT sensors and optimization can build out the footprint of
those community groups in a sustainable way. This in turn will build capacity
within the network and provide a jumping off point for community revitalization
efforts. Sensors for the IOT are growing in prevalence and availability. A Wall
Street Journal article last year estimated that the IOT market could reach $1.7
trillion by 2020 (2). IOT technology has moved beyond indoor space and into
the outdoors recently with a number of products and services such as the Edyn
watering sensor. The Edyn garden sensor has 5 sensors. It measures temperature,
humidity, light levels, soil moisture and soil nutrition (3). The Edyn probe
functions by sending an electrical pulse into the soil and detecting how that pulse
is affected by fertilizer and water using a technique that is identical to that used in
commercial farming. It also includes extensive digital dictionaries indexing the
compatibility, preferred conditions, and seasonal watering needs for thousands of
plants. The current version of the Edyn is produced commercially and costs $99

50
per sensor, which is still a substantial amount of money, particularly for a large
network of sensors.
There are currently open hardware low-cost data loggers for turbidity, but not
other water-quality parameters such as salinity. An NSF-sponsored critical zone
observatory (CZO) also includes multiple data loggers built with open-sourced
hardware (Arduino) and monitoring equipment, but to our knowledge no
conductivity measurements are recorded regularly and no sensor design was
included in the design.
The MC REU project is in its third year of existence. The REU program
connects faculty and students early in their careers to help build a foundation
of undergraduate research. Students spend most their time at their home
commonwealth campus, with two weeks out of the ten-week experience in
workshops with the entire cohort at University Park. Having two faculty mentors
(one from each campus) allows students to make bridging connections and extend
their research networks early in their undergraduate careers.
It has been shown that students that participate in undergraduate research
show increased interest in graduate study (4). A survey of researchers participating
in NSF REUs showed a 29% increase in interest of students in pursuing a PhD
after graduation following their undergraduate research experience (4). An
emphasis of the MC REU program is for students to participate in the culture of
research by experiencing faculty mentorship, presenting at the end of experience
conference and writing about their research work. In this way, students broaden
their education and increase their awareness of pathways to graduate education.
Another emphasis of the MC REU program is to connect faculty from
Commonwealth campuses to other faculty within Penn State. Faculty mentors
collaborating on shared research goals with shared student workers promote
awareness of Penn State resources and avenues for collaboration. A goal of the
program is to spawn new research collaborations as well as to promote the use
of shared resources for research.

Methods
This project is based on the Arduino platform and uses Arduino Unos as its
basis due to their wide availability and ease of use at an entry level. Arduino is
an open source platform for building electronics. The Arduino system consists
of a microcontroller or small circuit board, and software that is used to write and
upload code to the microcontroller. Arduino code is based on C++, and is simple
to learn and use, making it an ideal choice for an undergraduate research project.
Two student teams worked over the course of two summer term periods to refine
and test a basic sensor design. For the purpose of this exercise, each design was
focused on sensing conductivity as the main goal.
The first iteration of the sensor is a simple Arduino Uno that has three power
sources, built in temperature sensor diodes, and a customizable protoboard. This
sensor, called the Riffle, was originally produced by PublicLab as part of the
Open Water Project. The Riffle can also be attached to a protoboard to increase

51
its sensing capability. Both the Riffle and associated protoboard are shown in
Figure 1.
The Riffle can be powered with a lithium-ion battery, a button-cell battery, or
a USB/microUSB port. The temperature is automatically logged on a microSD
card for the Riffle. In order for the Riffle to measure conductivity, a circuit design
capable of doing so was soldered onto the protoboard attachment. In order to
make the Riffle compatible with a conductivity probe, the protoboard was adapted
to include a sensor array called the Coqui. The Coquí (Figure 2) is designed with
a probe that acts as a variable resistor.

Figure 1. Riffle Arduino board (top) and associated proto board (bottom).

Figure 2. Coqui sensor on protoboard.

52
 When the electrodes are placed into a solution, the solution has a specific
conductance; therefore, acting as a resistor. Depending upon the voltage going
through the circuit, the pitch of the piezo speaker varies. For example, if the probe
is placed into water with high conductance, the pitch of the sound released from
the piezo speaker increases. The speaker can be replaced with an LED light that
will act similarly to the speaker. The light shines brighter the more conductive the
sample is. The LED that is already in the circuit diagram in Figure 2 acts as an
‘on/off’ power indicator.
To adapt the Coquí to the Riffle attachment, the piezo speaker is replaced with
the analog read pin. The protoboard is designed where the top two rows are labeled
connections that run to the data logger. The rest of the pins on the protoboard
are connected vertically down the board. A diagram of the Coquí design for the
protoboard can be seen in Figure 2. The LED is still used as a power indicator
in the protoboard design. The protoboard is then connected to a simple nichrome
wire probe which can be used to test the water sample. This simple device was then
tested by the student to determine how well it performed compared to a traditional
conductivity probe.
The students then used these tools to evaluate prepared water samples. The
prepared water sample consisted of tap water that had varying levels of salt present.
During this challenge, students were required to answer the following questions:

Does the new conductivity probe give good data compared to a traditional
probe?

Is the new conductivity probe easy to use?

Could the design of the probe be improved? In what way?

What are potential community uses for the conductivity probe?

Questions were posed in oral form, following project discussion with faculty
mentors in the eighth week of the REU experience. Students responded to these
questions both orally and in the written form of a report. It was found that the
Arduino based probe did not perform as well as the traditional probes within a
reasonable margin of error (10-15%), likely due to interferences on the nichrome
wire probe which lead to variation in the cell constant. As the comparison test
was only performed one time, data is not included here. Students in future
undergraduate research experiences will perform the comparison test multiple
times to generate a larger data set for analysis, including statistics. Anecdotally,
collecting and analyzing data helped to stimulate and sustain student interest in
research, as students involved in the project were able to see their efforts manifest.
Students made several suggestions regarding the design of the probe, the
most common response being to make the probe more robust. This response
was a valuable insight as the project continues to develop. For future work,
undergraduate researchers will fabricate a housing to better protect the probe
and reduce interferences. Regarding potential community uses for the probe,

53
monitoring water quality downstream of industrial discharges and within local
water bodies for fishermen were two popular responses.
Students involved in the MC REU program were asked to produce weekly
reports about their research experience, blog about topics related to undergraduate
research and present a final poster at the closing research forum.

Discussion
Close collaboration with faculty is one of the main goals of the program,
which is fostered by the structure of the REU. As part of student engagement
within the MC REU program, each student spends 8 weeks at their home campus
and 2 weeks at the University Park Penn State campus. During this time, students
visit laboratories on campus, attend sessions about career development and
teambuilding, and meet with additional faculty and graduate students. Although
working independently on a research project, students receive faculty support and
instruction for several hours each week to help achieve their goals. This close
collaboration is cited by students as the most valued asset of the program.
Both sessions that have engaged with this program cite the close collaboration
with faculty as well as the hands-on nature of the research activity as stimulating
their interest in research. More specifically, the students were surveyed if they
would continue doing undergraduate research. All responses were either agree or
strongly agree. One commented that participating in the project “…helped me to
see research as an avenue for a possible career that I had not considered before.”
It was also noted in the comments portion of the poll that presenting their research
in the closing forum helped them to better understand not only the material but
to stimulate the interest of others in the audience in the growing field of remote
sensing.

Conclusions
This research experience has resulted in an engaged student experience that
provides in-depth topic exploration and familiarity with complex material as
well as providing greater engagement between faculty and students. Students
benefited from the interaction with real world research problems as well as their
own discoveries to provide enhanced understanding of the research process.
Students responded overwhelmingly positively to this activity, and it is planned to
continue to offer this research experience for students. For future work, students
will map the area of Western Pennsylvania for sensor placement, and collect and
interpret relevant water quality data using the sensors.

Acknowledgments
The author would like to acknowledge the support of the Penn State Greater
Allegheny community during preparation of this submission.
54
 References

1. Thomas, A. G. Specific Conductance as an Indicator of Total Dissolved

Solids in Cold, Dilute Waters. Hydrol. Sci. J. 1986, 31 (1), 81–92.
2. Norton, S. Internet of Things Market to Reach $1.7 Trillion by 2020. The
Wall Street Journal, June 2, 2015.
3. Flatow, I. The Blossoming Internet of Things for Your Garden. Science
Friday, April 29, 2016.
4. Russell, S. H.; Hancock, M. P.; McCullough, J. Benefits of Undergraduate
Research Experiences. Science (Washington) 2007, 316 (5824), 548–549.

55
 Chapter 4

Trends in Atmospheric Ammonia: An

Environmental Chemistry Class Project
Vivian C. Ezeh*

Department of Chemistry, Kenyon College, 200 N. College St.,

Gambier, Ohio 43022, United States
*E-mail: ezehv@kenyon.edu.

An environmental chemistry class managed an ammonia

monitoring station as a class project. The ammonia station
was part of the National Atmospheric Deposition Program.
The pedagogy goal for the project was to improve quantitative
reasoning skills, such as data management and visualization.
The data obtained during the fall 2017 semester was used to
teach data management, graph making and mapping with a
GIS program. Evaluation of submitted project assignments and
students’ response to an end-of-semester survey support an
improvement in quantitative reasoning skills.

Introduction
How do we know if an environmental policy to reduce pollution is effective?
Answers can be obtained from environmental data collected by a network of
monitoring stations. There are several environmental networks dedicated to
measuring, collating, and archiving various environmental data. An example
is the “Ammonia Monitoring Network (AMoN)” which as part of the National
Atmospheric Deposition Program (NADP) monitors ammonia gas concentration
in the atmosphere (1). This and other networks are very important to our
understanding of the trends in various environmental data.
Ammonia (NH3) is a compound that exists as a gas in the atmosphere at
atmospheric pressure and temperature. Agriculture practices such as farming and
animal husbandry are primary sources of NH3 to the atmosphere (2). Acting as a
basic gas in the atmosphere, NH3 reacts with acidic species to form ammonium
salts which contribute to aerosol formation as particulate matter (PM) (3, 4).

© 2018 American Chemical Society

When the ammonium salts fall back to land and water, they contribute to
acidification and nitrogen eutrophication (3). NH3 in the atmosphere also reacts
with secondary organic aerosols contributing to photochemical smog (5). The
concentration of NH3 in the atmosphere is increasing and there is currently no
policy to regulate the gas (Figure 1) (6, 7). Some gases regulated by the United
States Clean Air Act show decreasing concentration trend. For example, sulfur
dioxide (SO2) and nitrogen dioxide (NO2) levels in the atmosphere are declining
(Figure 1) (7). Tracking atmospheric NH3 is important to understanding trends
and effects of the gas in the environment. The data can also inform policies
to regulate atmospheric NH3. With Kenyon College located in an agricultural
community, the atmospheric ammonia monitoring station is an important data
point in obtaining a better picture of the ammonia pollution problem. There are
six AMoN sites in the state of Ohio, the Kenyon College site (labeled OH32) is
the only one on a college campus.

Figure 1. National Emission Inventory (NEI, 2015), SO2 (reported as S), NOx
and NH3 (both reported as N) emissions from 2001 to 2014. NOx is assumed
to be in the form of NO2 (7). Reproduced with permission from reference (7).
Copyright 2016 Elsevier.
The AMoN project was incorporated as a course-based research experience
in an environmental chemistry class to improve the quantitative reasoning course
goal (8, 9). The hypothesis for the ammonia class project is that the process of
answering the research questions will improve problem-solving and quantitative
skills.
This book chapter is a description of involving a class in a network data
collecting experiment. The success, challenges, and feedback of beginning a
course-based research experience will be discussed. Also discussed will be a
personal reflection of an early career faculty on course design.
58
 Course and Project Description

Environmental Chemistry, CHEM 110, is a chemistry class designed for

students to fulfill the requirement to take a science-based course if they major in
humanities, arts and languages. The majority of the students are political science,
international studies, or economics majors. The course is also designated as a
quantitative reasoning (QR) course. A QR course focuses on the organization,
analysis, and implementation of numerical and graphical data. To enhance the
QR aspect of the course, the 2017 fall semester CHEM110 class (20 students)
managed an ammonia monitoring station on campus. The project was supported
by a grant from the Kenyon College faculty affairs committee. The project
goals were: 1) Write and execute a data management plan, 2) Collate and graph
ammonia concentration and weather data (temperature, pressure, humidity, wind
speed, visibility), and 3) Plot ammonia data on a geographic information system.
The secondary goals were: 1) to expose students to a field-based project and 2) use
data to make observations. Several activities and assignments were incorporated
into the course schedule to support the project goals. A workshop on data
management was facilitated by the Social Science and Data Librarian and then
each team wrote a data management plan. For project goal 2, each team designed
a Google sheet to collate project data. Also a workshop on plotting graphs with
Google sheets was facilitated by the Social Science and Data Librarian. At the
end of the semester, each student made graphs (line graph, scatter plot with trend
line and 2D plots) with their collated project data. The third project goal was
achieved by plotting data from the six sites in Ohio onto the Ohio state map by
using Google MyMaps. Finally, a project survey was carried out to gauge the
success of the project goals.
The National Atmospheric Deposition Program (NADP) - National Trends
Network (NTN) was established in 1977 with a mission to study atmospheric
deposition and its effects on the environment.1 The network has been collecting
data (amount, trends, and geographic distribution) on various atmospheric
pollutants such as acidic precipitation, mercury, and ammonia. Although initially
funded by the United States Department of Agricultural, NADP is now supported
by a network of researchers. Measurement of ammonia started in 2010, and the
network consist of approximately 100 monitoring stations (1). The data collected
are the only consistent record of atmospheric ammonia concentration in the
United States. Participating in the network consist of hosting a sampling site,
changing samplers according to protocol and mailing the samplers to the NADP
central analytical lab (CAL) for analysis. AMoN uses a Radiello (radial diffusive
or passive) sampler for the ammonia project. The Radiello sampler is made of
microporous polyethylene impregnated with phosphoric acid, NH3 is selectively
adsorbed from the atmosphere and is trapped as ammonium salts (10). The
sampler deployment is on a two-week cycle; which means a sampler is installed
on a Tuesday, removed on a Tuesday two weeks later and mailed to the CAL
for chemical analysis. Preliminary ammonia concentration (measured as µg/m3)
results are received about two weeks after the sampler is received at the CAL.

59
 Project Implementation

In preparation for siting the ammonia sampler on campus, several locations

on campus were evaluated during the summer of 2017. The chosen location
was in an open field, with low vehicle & human traffic, and greater than 1
km (0.62 miles) from agricultural activities. Geographical information such
as latitude (40.370055 N), longitude (82.395539 W) and altitude (312 m) was
recorded. A shelter to house the sampler was installed at the beginning of the
fall 2017 semester, and the first sampler was deployed on Aug 22nd 2017. After
introductions on the first day of class (Aug 24th 2017), the class visited the sampler
location to observe the setup. An article “Nitrogen from the Environment” was
assigned to the class to acquaint students with the class project (11). Students
then completed a brief survey designed to get the class invested in the project
(Survey 1, Table 1). Based on responses from the survey, 6 teams of 3-4 students
were formed. Also, the class wanted to explore how the following variables
would affect ammonia concentration trends: 1) weather (temperature, pressure,
wind speed & direction, humidity, and visibility), 2) vegetation change, and 3)
location of samplers around Ohio. In summary, the class decided to track weather
conditions by checking weather websites and record vegetation changes by taking
pictures of vegetation around the sampler. The bulk of the semester was spent
changing the sampler according to schedule and collating project data. Each team
sent a representative for the sampler change.

Table 1. Survey 1: Questions at the beginning of project

# Survey Questions
1 What are reactive nitrogen species
2 How will participating in this project benefit your college, personal or career goals
3 How would you organize this project to ensure that everyone benefits and
contributes to its success
4 Give one example of another environmental data (apart for concentration of
ammonia) that we could collect to enrich the project

Within the semester, two 30 min workshops were included in the class
schedule to teach data management and graphing skills. The concepts covered
in the data management workshop included: file naming strategies, options for
preserving data, and categories of data. Each team wrote a data management plan
and submitted via Google Docs. Students were able to articulate the class project
goals and plan with the data management plan assignment. Graphing with Google
sheets, classification of variables, and interpretation of R2 values were taught at
the second workshop.

60
 After 13 weeks of the monitoring project, the class project was completed
in an 80 min workshop. Using the collated data, students made several graphs
during the workshop to answer the project research questions. Examples of graphs
completed included; line graphs, scatter plots (with Trendline & R2 value), 2D
plot (line graph with 2 y-axes) and a matrix plot (graphical comparison of several
variables). Each graph was copied to a Google slide with a figure number and
short description. A mapping exercise with data from other sites in the state of
Ohio was also completed. Average ammonia concentration for the 6 sites in Ohio
was obtained from the AMoN website and mapped with the Google MyMaps
GIS. Finally, each student wrote a summary which included their observations
and discussion of the team’s results.

Project Results
By the project wrap date, we had five ammonia concentration data points.
The class decided that the best representation of ammonia data was to match
it to the Tuesday dates between the 2 weeks sampling period. For example,
one ammonia concentration value represented the two weeks from Aug 22nd
to Sept 5th. However, for the plotting assignment, that ammonia concentration
was matched to Aug 29th and the corresponding weather data for Aug 29th. A
plot of ammonia concentration and Tuesday dates showed a general increase in
ammonia concentration during Aug to Oct 2017 (Figure 2). Each student made
a plot of ammonia concentration as a dependent variable with their weather data
as an independent variable. Figure 3 is an example of a scatter plot of ammonia
concentration and temperature. Following a discussion of outlier data points,
linear regression analysis was performed with 4 data points, and R2 values were
obtained. On the question of weather conditions effect on ammonia trends, we
observed no correlation between ammonia concentration and pressure or visibility.
A positive correlation with temperature (Figure 4) and a negative correlation with
humidity or wind speed. Ammonia concentration data for the other sites in Ohio
was obtained from AMoN website. A geographical information system plot was
made with average ammonia data for Aug – Oct 2017 (Figure 5). We observed
that Cincinnati (OH27) site had the highest average ammonia concentration, while
the lowest was at the Deer Creek State Park (OH54) site. Finally, the highest
ammonia concentration (2.21 µg/m3) during the Aug – Oct sampling period for
Kenyon site (OH32) corresponded with a complete loss of leaves on trees close
to the sampler.

61
Figure 2. Scatter plot of ammonia concentration (µg/m3) vs date for Aug 22nd
– Oct 31st 2017.

Figure 3. Scatter plot of ammonia concentration (µg/m3) vs temperature (°F)

for fall 2017.

62
Figure 4. Scatter plot of ammonia concentration (µg/m3) vs temperature (°F) for
fall 2017 after removing the possible outlier data point.

Figure 5. GIS plot of average ammonia concentration (µg/m3) for sites within
the state of Ohio for fall 2017 (Aug 22nd – Oct 31st).

63
 Assessment

The class project was classified as a formative exercise in the class design and
accounted for 10% of the class grade. Students were allowed to make corrections
after feedback for the full possible point per activity.
A survey (Survey 2, Table 2) was used to evaluate the quantitative reasoning
skills gained from the project. Student response (15 students) showed a significant
number learned or gained the QR skills taught by the project.

Table 2. Survey 2: Questions at the end of project

# The ammonia project was included to enhance the quantitative reasoning
designation of CHEM110. Rate the following QR skills as 1 (I didn’t learn this
skill); 2 (I learned or improved on this skill); 3 (I knew this before) or N/A (didn’t
participate in this activity)
1 Designing and executing a data management plan
2 Organizing data on a spreadsheet and preserving the data
3 Plotting data on graphs
4 Plotting data on a map

Figure 6. Response to survey 2.

64
 Discussion

The project was successfully implemented and having the class project
enhanced the communal feel of the class. Use of passive samplers and chemical
analysis conducted at CAL made the project easier to incorporate into the course
schedule without significant change to course content. Students practiced asking
research questions and agreeing on which inquires to pursue. As they were
searching for answers, they learned data management, graphing and visualization
skills. Although we had a small data set, some observations on ammonia
concentration trends were made. The effect of nearby agricultural activities,
leaves loss and decomposition, and urban heat were discussed in summary
submitted by students. In summary, the class project provided a great platform to
enhance the QR designation of the environmental chemistry class.
The time commitment to manage the project was low. After the time required
for initial planning, the bi-weekly sampler change takes about 10 min to complete.
The small time commitment made it easier to juggle with the busy schedule of
academic life. Implementing the project provided an opportunity to collaborate
with colleagues outside of my department in designing pedagogy activities. Most
of the schedule went as planned; we just required an extra half class time to
complete the graph and mapping assignment. In all, it was a successful class
project.

Conclusion and Future Directions

Data from ammonia monitoring on campus was used to teach graph and
visualization skills. Observation from our limited data was similar to trends
reported from analysis of larger data sets tested with rigorous statistics tools (7).
The monitoring project will continue and by the next class there will be more data
points to work with. With a larger data set, more statistics skills will be included
in the class project.

Acknowledgments
I thank the faculty affairs committee of Kenyon College for awarding the
teaching grant that provided funding for this class project. Nathan Wolfe, Social
Science and Data Librarian at Kenyon College, was valuable to the successful
implementation of the class project. He provided expertise in data management
and visualization. I am grateful to colleagues that provided support for the smooth
running of the class project. Steven Vaden, constructed the shelter for the sampler.
Emily Wise managed the finances for the project. Mrs. Shannon Hashman assisted
by making sure that the samplers are mailed back to CAL. Mrs. Carolyn Waggoner
helped by receiving the sampler. Prof. Simon Garcia provided support as the
alternate site manager.

65
 References

1. NADP National Atmospheric Deposition Program, Ammonia Monitoring

Network (AMoN). http://nadp.isws.illinois.edu/AMoN/ (accessed January
14, 2018).
2. Warner, J. X.; Dickerson, R. R.; Wei, Z.; Strow, L. L.; Wang, Y.; Liang, Q.
Increased atmospheric ammonia over the world’s major agricultural areas
detected from space. Geophys. Res. Lett. 2017, 44 (6), 2875–2884.
3. Sutton, M. A.; Tang, Y. S.; Dragosits, U.; Fournier, N.; Dore, A. J.; Smith, R.
I.; Weston, K. J.; Fowler, D. A spatial analysis of atmospheric ammonia and
ammonium in the U.K. Sci. World J. 2001, 1, 275–286.
4. Meng, Z.; Lin, W.; Zhang, R.; Han, Z.; Jia, X. Summertime ambient ammonia
and its effects on ammonium aerosol in urban Beijing, China. Sci. Total
Environ. 2017, 579, 1521–1530.
5. Liu, Y.; Liggio, J.; Staebler, R.; Li, S.-M. Reactive uptake of ammonia
to secondary organic aerosols: kinetics of organonitrogen formation.
Atmospheric. Chem. Phys. 2015, 15 (23), 13569–13584.
6. Walker, J.; Nelson, D.; Aneja, V. P. Trends in Ammonium Concentration in
Precipitation and Atmospheric Ammonia Emissions at a Coastal Plain Site
in North Carolina, U.S.A. Environ. Sci. Technol. 2000, 34 (17), 3527–3534.
7. Butler, T.; Vermeylen, F.; Lehmann, C. M.; Likens, G. E.; Puchalski, M.
Increasing ammonia concentration trends in large regions of the USA derived
from the NADP/AMoN network. Atmos. Environ. 2016, 146 (Supplement
C), 132–140.
8. Russell, J. E.; D’Costa, A. R.; Runck, C.; Barnes, D. W.; Barrera, A. L.;
Hurst-Kennedy, J.; Sudduth, E. B.; Quinlan, E. L.; Schlueter, M. Bridging
the Undergraduate Curriculum Using an Integrated Course-Embedded
Undergraduate Research Experience (ICURE). CBE Life Sci. Educ. 2015,
14 (ar4), 1–10.
9. Brownell, S. E.; Hekmat-Scafe, D. S.; Singla, V.; Seawall, P. C.; Conklin
Iman, J. F.; Eddy, S. L.; Stearns, T.; Cyert, M. S. A High-Enrollment Course-
Based Undergraduate Research Experience Improves Student Conceptions
of Scientific Thinking and Ability to Interpret Data. CBE Life Sci. Educ.
2015, 14 (ar21), 1–14.
10. Radiello - The Radial Diffusive Sampler. http://www.radiello.com/english/
nh3_en.htm (accessed October 25, 2017).
11. NADP Nitrogen from the Atmosphere. http://nadp.isws.illinois.edu/lib/
brochures/nitrogenAtmos.pdf (accessed January 14, 2018).

66
 Chapter 5

Using DNA Barcoding To Identify

Duckweed Species as Part of an
Undergraduate Ecology Course
Stokes S. Baker*

Biology Department, University of Detroit Mercy,

4001 West McNichols Road, Detroit, Michigan 48221, United States
*E-mail: bakerss@udmercy.edu.

DNA barcoding identifies species by sequencing polymerase

chain reaction (PCR) amplicons and comparing the amplicon
sequence to sequences found in databases. There are many
applications of this technology that support environmental
investigations. As part of an inquiry ecology laboratory course,
undergraduate students at the University of Detroit Mercy
conducted nutrient response experiments with duckweed,
floating aquatic plants. The students used DNA barcoding
to identify their wild collected plants because duckweed are
extremely small and do not possess distinctive morphological
features. The results of barcoding with the chloroplast
atpF-atpH intergenic region showed that a cove in Lake Saint
Clair, Michigan, USA, hosted a duckweed community that
contained at least four species. One of the species, Lemna
obscura, has never been reported in Michigan waters. This
paper describes how primer design, a robust DNA extraction
procedure, software use, and database utilization can be
incorporated into laboratory instruction.

© 2018 American Chemical Society

 Introduction

For over two decades, national organizations (1–4) have called for reform
of undergraduate science, technology, engineering and mathematics (STEM)
education by replacing content driven curriculum with curricula that focuses
on teaching core concepts and developing skills that support modern scientific
research. Recently, the American Association for the Advancement of Science
has called for revisions of biology curriculum to teach scientific skills by
integrating major principles, such as information flow, with activities that develop
competency in mathematics and provide undergraduate students experiences
in accessing large data sets (5). Ecology, a subject that has always been
interdisciplinary, has placed growing reliance on the use of molecular tools (6)
and the utilization of large databases (7). Unfortunately, most ecology laboratory
teaching manuals do not contain exercises that provide students experience
with molecular ecology, nor exposure to database utilization. [For example,
see Vodopich (8)] DNA barcoding is a technique well suited to ecological
investigations. Species are identified by homology searches of DNA databases
like GenBank (9). Thus, student investigations that utilize DNA barcoding
provide them an introduction to molecular ecology and exposure to publicly
available supercomputing resources. An inquiry investigation was implemented
in the Ecology Laboratory (BIO4490) course taught at the University of Detroit
Mercy (Detroit, MI, USA), where undergraduates conducted nutrient response
experiments with wild duckweed.
DNA barcoding is a technique that is used to identify species by sequencing
short (400 to 800 bp) regions of genomes (10). This strategy involves using
polymerase chain reaction (PCR) primers that are homologous to evolutionarily
conserved regions that flank a variable region. The resulting amplicon sequence is
determined by combining Sanger sequencing with capillary electrophoresis (11).
The resulting sequence is used to search nucleotide databases such as GenBank
(9, 12).
Ecologists use DNA barcoding in several applications such as identifing
species from small fragments collected from environmental samples, identifying
microorganisms, and identify species from individuals that do not contain
definitive morphological features (10). Though there is no single primer pair
that can be used to barcode all of life, a limited collection of primer pairs have
emerged that can be used to identify broad collections of taxonomic groups (10,
13). For plants, primers that hybridize to the plastid genome are widely used
because each plant cell contains several copies of its plastid genome (14). Two
commonly used primer pairs are rbcL which amplifies a 654 bp portion of the
gene encoding the large subunit of ribulose bisphosphate carboxylase/oxygenase
(RuBisCO) and atpF-atpH which amplifies 578 to 707 bp intergenic region of
the ATP synthase locus (15, 16).
Duckweed plants were used in the Ecology Laboratory course because it
is becoming an excellent model system. They are small free-floating plants
that proliferate in the 48 contiguous states, Hawaii, and southern Canada
(17). Duckweed plants grow easily in the laboratory (18), have rapid clonal
reproduction (19) and are extensively used in toxicology testing (20). Duckweed

68
are monocots in the clade Lemnoideae (21). Unfortunately, because of its small
size and infrequent flowering, it is a difficult plant to identify at the species level
(22). In the past, biochemical assays, such as chromatography, were used to
confirm species identification (22). DNA barcoding is now the tool of choice for
duckweed identification. For example, the Rutgers Duckweed Stock Cooperative
only accepts germplasm donation that has been identified by DNA barcoding (23).
A standard practice in field ecology is to identify species found in field
collections. Typically, this is done with the aid of dichotomous keys and field
guides. Unfortunately, reliable identification of duckweed based solely on
morphology is not possible. Thus, a modified version of the DNA Learning
Center’s Barcoding 101 curriculum was used to identify duckweed species (13).

Materials and Methods

Plant Material

During the month of September (2014, 2015 and 2016), duckweed

populations (Figure 1, Panel A) were field-collected from an abandoned marina
in Lake Saint Clair, Michigan, USA (Latitude 42.56141, Longitude -82.84313).
To assess the species diversity of the population, students were asked to choose
plants that had different morphological features. The plants were photographed
with an SLR digital camera with a 100 mm macro lens or with a dissecting
microscope with a built-in digital camera (Figure 1, Panels B - D). A DNA sample
was also isolated from a coleus plant (Plectranthus amboinicus). The plant was
obtained from a retail outlet. The resulting coleus DNA sequence was used as an
outgroup for making dendrograms.

DNA Isolation

Total DNA was isolated using the Wizard Genomic DNA Purification Kit
(Promega Corporation, Madison, Wisconsin, USA). Splash goggles and plastic
gloves were worn during the procedure because some of the reagents in the kit
contain chaotropic agents. The work-flow is illustrated in Figure 2. Forceps were
used to transfer clonal duckweed clusters into 1.5 mL microcentrifuge tubes. Up
to 40 mg (fresh weight) of plant materials was homogenized in 100 μL of Nuclei
Lysis Solution using plastic pestles design to fit inside the microcentrifuge tubes.
The material was ground by hand until the plant materials were well macerated.
An additional 500 μL of Nuclei Lysis Solution was added to each tube and mixed
by inverting. The manufacturer’s protocol was followed for the remainder of the
DNA isolation process.

69
 Figure 1. Wild population of duckweed. Panel A: A mixed species community
growing in Lake Saint Clair, Michigan. The arrow points at a water lily, a
member of the Nymphaeaceae. Close-up photographs of Spirodela polyrhiza
(Panel B), Lemma minor (Panel C), and Wolffia columbiana (Panel D). The bars
are 2-mm size standards. (see color insert)

Figure 2. Workflow of DNA extraction protocol.

70
Barcoding Primers

For this study, oligonucleotides that could hybridize to plastid DNA

were used as PCR primers. For most applications, the rbcL primer pair are
suitable (15, 16). However, for the identification of duckweed species, the
atpF-atpH primer pair should be used (24). More details will be presented
in the Instructional Prospective section. For the rbcL locus (13) the primer
sequences are 5′-ATGTCACCACAAACAGAGACTAAAGC-3′ (forward
primer, tm = 59.6 °C) and 5′-GTAAAATCAAGTCCACCRCG-3′ (reverse
primer, tm = 52.8 °C). For the atpF-atpH locus (24) the primer sequences are
5′-ACTCGCACACACTCCCTTTCC-3′ (forward primer, tm = 59.6 °C) and
5′-GCTTTTATGGAAGCTTTAACAAT-3′ (reverse primer, tm = 50.1 °C).
To facilitate automated DNA sequences, oligonucleotides that fused plastid
DNA primer sequences with M13 universal sequencing primer sequences were
synthesized. The M13 forward (-21) universal sequencing primer sequence
is 5′-TGTAAAACGACGGCCAGT-3′ and the M13 reverse (-27) universal
sequencing primer is 5′-CAGGAAACAGCTATGAC-3′(25). The M13 universal
primer/rbcL fusion primers (13) used were 5′-TGTAAAACGACGGCCAGT/
ATGTCACCACAAACAGAGACTAAAGC-3′ (forward fusion primer),
and 5′-CAGGAAACAGCTATGAC/GTAAAATCAAGTCCACCRCG-3′
(reverse fusion primer). The M13 universal primer/atpF-atpH locus fusion
primers used were 5′-TGTAAAACGACGGCCAGT/ACTCGCACACACT
CCCTTTCC-3′ (forward fusion primer) and 5′-CAGGAAACAGCTATGAC/
GCTTTTATGGAAGCTTTAACAAT-3′ (reverse fusion primer). The
oligonucleotides were purified by high-performance liquid chromatography
(HPLC) by the manufacturer (Bio Basic, Markham, Ontario, Canada). They were
diluted and combined to make primer mixtures containing 0.5 pmoles/μL forward
primer and 0.5 pmoles/μL reverse primer.

PCR Conditions

Illustra PuReTaq Ready-To-Go PCR Beads (GE Healthcare Life Sciences,

Pittsburgh, Pennsylvania, USA) were used for all sequencing reactions. This
system uses freeze-dried pellets that contain a hot-start Taq DNA polymerase,
deoxynucleotides, buffers, and co-factors. Only DNA template and primers are
needed to complete the mixture. To perform the PCR reaction, the following was
added to each 200 μL Ready-To-Go PCR Beads tube: 6.63 pmoles of each primer,
~50 ng plant DNA, and enough PCR grade water to bring the final volume up to
25 µL. The thermocycling conditions used are described below.
For tubes containing the M13 universal/rbcL gene fusion primer, initial
template melting was at 94 °C for 180 s, followed by 35 cycles of template
melting at 94 °C for 15 s, template priming at 54 °C for 15 s, and polymerization
at 72 °C for 30 s. The final polymerase extension was performed at 72 °C for 300
s (13). The PCR product was stored overnight at 4 °C.
For tubes containing the M13 universal/atpF-atpH locus fusion primer, initial
template melting was at 94 °C for 120 s, followed by 35 cycles of template melting

71
at 94 °C for 15 s, template priming at 50 °C for 15 s, and polymerization at 72 °C
for 45 s. The final polymerase extension was performed at 72 °C for 300 s (26).
The PCR products were stored overnight at 4 °C.
If there were poor PCR product yields with either primer set, the following
PCR protocol was attempted. Genomic DNA and primers were combined as
described previously. Initial template denaturation was at 95 °C for 180 s,
followed by 40 cycles of denaturation at 95 °C for 60 s, annealing at 55 °C for
45 s, and primer extension at 72 °C for 45 s. The final polymerase extension was
performed at 72 ○C for 300 s.

Analysis of PCR Products and Sequencing

To determine if appropriate PCR amplicons were produced, 5 μL of the PCR

reactions were fractionated by 2% agarose 1X TBE gel electrophoresis (25).
After electrophoresis, gels were stained with 1X GelGreen Nucleic Acid Stain
(Phenix Research, Candler, North Carolina, USA) and illuminated with a blue
light emitting diode transilluminator (Figure 3). The remaining 20 μL of PCR
products were held in reserve for DNA sequencing.

Figure 3. Example results of a 2% agarose showing PCR products from the

atpF-atpH locus and the rbcL locus. The numbers identify DNA samples
extracted from individual plants.

The PCR reaction that produced appropriate amplicons were sent to a

commercial sequencing faculty (GENWIZ, South Plainfield, New Jersey, USA).
The core facility performed amplicon purification and Sanger sequenced the
amplicon using M13 universal primers. Both the forward and reverse strands
were sequenced.
72
Sequence Quality Control

Students evaluated the quality of their DNA sequences by visual inspection

of the capillary electrophoresis chromatograph traces. To do so, the students
downloaded Chromas 2.6.4 (27) (Technelysium Proprietary Limited, South
Brisbane, Australia), free software that shows the four color channel traces and
deduced DNA sequence (Figure 4). Ambiguous sequences from the 3’-end and
5’-end were trimmed, and internal sequences that were called “N” were changed
to the correct base when the peaks could be reliably evaluated by inspection. The
corrected sequences were exported as FASTA files.

Figure 4. Four channel chromatograph of Sanger sequencing product visualized

with Chromas 2.6.4.

If the DNA sequences were correctly identified, the nucleotide sequence of

the forward strand and the reverse-complement sequence of the reverse strand
should be identical. To evaluate their sequence reliability, the students used
web-based software (28) that uses a Needleman-Wunsch alignment algorithm
(29) to align their forward and reverse sequences. The chromatograph peaks
corresponding to the non-complementary nucleotides were re-evaluated and
corrected with Chromas 2.6.4.

Species Identification

Species were identified by their homology to atpF-atpH or rbcL sequences

posted in the GenBank (12) database. To help students handle the bioinformatic
workflow, the DNA Subway pipeline (30) created by CyVerse (31) was utilized.
DNA Subway provides a collection of web-based bioinformatics tools that allow
students to utilize resources hosted on the eXtreme Science and Engineering
Discovery Environment (XSEDE) supercomputer cluster (32). The students
uploaded their sequences onto the DNA Subway Blue Line (13). On the Blue
Line, the sequences were processed through quality control tools, which trimmed
ambiguous sequences and paired the sense and antisense strand of the barcode
sequences. After quality control, the GenBank database was queried by BLASTn
(33). An example output is shown in Figure 5.
73
 Figure 5. Example BLASTn output from homology search with an atpH-atpF
amplicon sequence.
An additional feature of the DNA Subway Blue Line is it provides tools to
create dendrograms. Students created alignments of multiple DNA sequences
using the MUSCLE computer program (34). From the resulting matrix,
the students created maximum likelihood dendrograms and neighbor-joining
dendrograms using PHYLIP (35).

Results and Discussion

Both the rbcL and the atpF-atpH fusion primers (Figure 3) were able
to produce amplicons of the correct sizes (15, 24). Unfortunately, the rbcL
sequencing data did not meet the class’ needs because there was not enough
sequence divergence to identify the plants to the species level (Personal
observation and (24)). The results from the BLASTn searches of the atpF-atpH
barcodes indicated that there were at least four species of duckweed (Figure 6)
growing in the anthropogenic cove. According to range maps produced by US
Department of Agriculture (17) and the Flora of North America (36), Lemna
minor, Spirodela polyrhiza, and Wolffia columbiana are all native plants to
Michigan. In contrast, one student isolated DNA that produced a barcode for L.
obscura (Figure 5). The 587 nucleotides sequenced showed 99.8% homology
to GenBank sequence GU454235.1 (24). This plant is listed as “absent” from
Michigan (17, 36) though native to Ohio. Both natural and anthropogenic
mechanisms could explain the migration of L. obscura to Lake Saint Clair. The
lake is part of a major migratory flyway (37). Therefore, L. obscura may have
been deposited by waterfowl. Alternately, the lake is part of the Great Lakes
Waterway (37). Thus, boat traffic may have facilitated movement.
When the barcode sequences were arranged into a maximum likelihood
dendrogram (Figure 6) or a neighbor-joining dendrogram (not shown), the
resulting trees produce monophyletic clades. Members of the same species share
terminal nodes. Members of the same genus were found in common clades. The
organization of the genera (Lemna, Spirodela, and Wolffia) were consistent with
the taxonomy published in the NCBI Lifemap (38), Encyclopedia of Life database
(21), the Tree of Life database (39), and Wang et al. (24). These three genera are
in the clade Lemnoideae.
74
Figure 6. Maximum likelihood dendrogram from atpF-atpH barcode sequences.
The numbers are arbitrary plant identification numbers. The photographs of the
plants are inserted. Plants 9, 10, 13, and 18 are top views. Plants 5, 11, 12, and
14 are underside views. Images are not to scale. (see color insert)

The dendrograms were rooted by setting a dicot (P. amboinicus) atpF-atpH

barcode sequence as the outgroup. Monocots and dicots represent two distinct
clades of angiosperms (40). There is a growing collection of evidence indicating
that monocots evolved before dicots (40). If the goal of the dendrogram is to
perform cladistical analysis, then the outgroup should be basal to all other taxons
in the analysis (41). In future student investigations, a basal angiosperm, water
lilies (Nymphaeaceae) (42), will be sampled and used as the outgroup. Fortunately,
water lilies often grow alongside the studied duckweed community, as shown in
Figure 1 (Panel A).

Instructional Perspective and Conclusions

The described undergraduate investigation supports STEM curriculum
reform. The barcoding activity was part of an inquiry curriculum where students
conducted nutrient pollution experiments on wild collected aquatic plants.
Students learned a state-of-the-art technology to identify their experimental
organism. Species identification is part of the community of practice (4) in
ecology. By using DNA barcoding, the students focused on the key concept
of information flow, a learning outcome identified in the Vision and Change
recommendations (5). The students apply another key concept, organic evolution
(5) when they used their sequence data to create dendrograms.
One of the revolutions in ecology is the growing importance of big data
(i.e., data sets larger than 1 terabyte (7)). Because of the size of the datasets
and the complexity of the data, big data analysis is an interdisciplinary process
involving statistics and computer science to elucidate biological information.
Since specialized skills are needed to perform these analyses, several web-based
resources have been developed that allow non-specialists to access and process
75
big data sets. In this investigation, the students accessed several large databases
and used algorithms to process their sequence information. Specifically, the
supercomputing resources of NCBI were used to perform BLASTn queries (33)
of the GenBank database (9) to identify plant species. Additional large databases
were used to enrich the students learning experience. The USDA Plants Database
(17) was accessed to obtain species range maps, and phylogenetic databases (21,
38, 39) were utilized to help the students interpret their dendrograms.
The barcoding exercise can be modified to support many classroom
investigations. For example, students can use similar procedures to identify
difficult to classify organisms like green filamentous algae or identify small
non-distinct plant fragments, like roots found in soil samples. Because of the
diversity of material that can be used (10), DNA barcoding can be integrated into
many inquiry settings. Unfortunately, there is no single universal sequence for
barcoding (10, 15, 16). In this study, the atpF-atpH intergenic spacer locus was
used because it could identify members of the Lemnoideae down to the species
level (24). However, the number of barcode entries in GenBank for this locus
is relatively small as compared to rbcL barcode. As of December 2017, there
were 244,837 nucleotide records labeled as rbcL in GenBank while only 3998
nucleotide records labeled as atpF-atpH intergenic spacer. As a result, the rbcL
barcode may be better suited in many investigations.
Using DNA sequencing in species identification is a strategy that is likely to
be utilized for many years to come. The technology behind DNA sequencing is
rapidly advancing, especially with next-generation sequencing (NGS). This has led
to metagenomics, an investigative approach where whole microbial communities
are barcoded (43–45). In the past, NGS was limited to relatively short reads (46).
For example, an Illumina MiSeq produced reads of only 350 base pairs. Recently,
an inexpensive long-read technology has become available (47). By sequencing
longer stretches of DNA, long-read NGS may lead us closer to the goal of having a
small set of “universal” barcodes. Our instructional approaches will need to evolve
to take advantage of this rapidly changing science.

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 Chapter 6

Synthesis of a Novel Series of

Nitrogen-Containing Ligands for Use as
Water Remediators, All Incorporating
Long-Chain Aliphatic Moieties
Justin Pothoof, Michele Bhagwagar, Grace Nguyen, Sara Tinawi,
Sara Makki, and Mark A. Benvenuto*

Department of Chemistry & Biochemistry, University of Detroit Mercy,

4001 W. McNichols Rd., Detroit, Michigan 48221-3038, United States
*E-mail: benvenma@udmercy.edu.

A series of symmetrical, highly multi-dentate podand ligands,

all incorporating terminal, long-chain aliphatic moieties and
a centrally-positioned series of nitrogen atoms, have been
synthesized and characterized. These ligands were produced
in a continuing effort to find effective, useful, inexpensive
water remediators that are able to function as chelates and
remove metal ions indiscriminantly from aqueous solutions.
The ligands were complexed with a variety of metal ions, to
determine the solubility of the resulting complexes in water.
They were also examined to determine if they could retain
metal cations in non-aqueous solvent.

Introduction
Throughout the history of civilization, humankind has almost always lived
near water. Even desert dwellers knew exactly where water was to be found,
precisely because the presence of water meant life. Yet for as long, brackish water,
saline water, and water that has in any other way been contaminated with some
foreign matter has been of concern to people, precisely because it is either difficult
or impossible to use (1–12). Saline water is certainly still useful for fishing and
for waterborne traffic, but is routinely far too salty to drink.

© 2018 American Chemical Society

 What can be called this degradation of water has become a more acute
problem in the last 75 years than it has for almost all of the recorded history
prior to that time, because of the explosion in human population worldwide
(13–16). For example, the loss of the Aral Sea is one of the largest man-made
catastrophes dealing with a freshwater source that has ever been recorded (17,
18). The pollution of the Gulf of Mexico near the mouth of the Mississippi River
with agricultural waste and farm run-off is another large-scale degradation of a
significant part of the world’s water that has become a major regional concern (4,
19). And the recently enhanced salinity of the aptly named Dead Sea, as its waters
are used by companies in Israel and Jordan for mineral extraction, is a further
issue of concern for peoples of the region who have used the sea for centuries
(20). In these three cases and several more, the presence of larger numbers of
people near water sources, and depending on water, stresses those water sources
more than at any previous time in history.
Clearly, the need for materials to clean polluted or degraded water is
important. Numerous different chealting molecules have been used in some way
to extract unwanted ions or organic matter from water, with ethylene diamine
tetraacetic acid (EDTA) being arguably the widest known chemical used for this
purpose, at least on a small scale (21–26). But the existence of a class of chelators
does not prevent further, similar molecules from being produced and examined
in the hope that they too may function as inexpensive, efficient remediators of
environmentally degraded waters.
This paper is the result of a research project utilizing undergraduate
researchers, in which a novel series of ligands have been produced, under ambient
temperature and pressure conditions, resulting in organic molecules having three
or five nitrogen atoms in their central portion. These nitrogen atoms act to form
a dative bond non-specifically with a variety of metal ions, forming coordination
complexes. They function much as molecules such as EDTA and other established
chelators, and should prove useful in remediating water containing a wide variety
of cations.

Results and Discussion

Synthesis and Characterization of Ligands
The amines diethylene triamine (N3) and tetraethylene pentaamine (N5), as
well as the two aldehydes: octanal and dodecanal, were all purchased from Aldrich
and used as received. A single 1H NMR was run of each starting material to
ensure purity of the material. Solvents, monoglyme and toluene, were purchased
commercially and used without further purification.
To synthesize the target ligands, two molar equivalents of an aldehyde were
reacted with one molar equivalent of an amine at room temperature (25°C),
with either monoglyme or toluene as a solvent, with mechanical stirring, for
approximately 16 hours. Starting solutions were uniformaly clear, with the
resulting solutions after stirring being very slightly yellow.
Figure 1 shows the basic reaction chemistry for the production of the target
ligands.
82
 Figure 1. General route for ligand synthesis.
The reaction schmeme illustrated in Figure 1 was used to produce Ligands 1
and 2, and represents a wider scheme that can be used to produce numerous other
long-chain ligands. Figure 2 shows both ligands that were produced in this study,
and Table 1 indicates the sample sizes and molar ratios of materials used in the
syntheses.

Figure 2. Shortest (Ligand 1) and longest ligand (Ligand 2).

The ligands were examined by 1H NMR, and as expected, displayed a
very cluttered, crowded aliphatic region. The reaction though, a Schiff’s base
condensation, produces molecules that in these cases contain two imine sites.
These double bonds are the only functionality the target ligands have besides
the nitrogen atoms, and importantly, the imine proton appears as a singlet in the
region δ 8.2 – 8.8. This is definitely different from the aldehydic proton of the
starting material, which appears slightly above δ 11.0. It is also several ppm away
from the -CH2- saturated methylene signals from those protons two bonds away
from each nitrogen atom. In short, the imine singlet of each target ligand serves
as a diagnostic that the ligand has been produced. The presence of the imine
singlet, and the complete loss of the aldehyde singlet, were used as indicators that
the ligands formed quantitatively.

Evaluation of Ligand Complexing Abilities

In a traditional manner, for each trial, a solution of Ligand 1 or 2 was added
to a separatory funnel, then an aqueous solution of a metal salt was added (results
are summarized in Table 2). Precipitation of material essentially occurred upon
contact, with only a few seconds of shaking of the separatory funnel.
Simply adding a sample of a dry salt to the non-aqueous solution of either
Ligand 1 or 2 produced some unexpected results. This experimental approach
was chosen because it was felt that it would be straightforward to separate any
precipitate, dry it, and determine the overall conversion to the target coordination
complex. But it can be seen in Table 2 that four of the five metal salts added directly
to the non-aqueous ligand solution of Ligand 2 stayed in solution. While such
83
behavior is not unheard of, it is not common. Reported examples of organic ligands
that solvate ionic materials in non-aqueous solutions always involve more complex
ligands than those produced here (27–29). It appears then that in the case of Ligand
2 – a molecule that can be termed α,ω-bis-dodecyl-tetraethylene-pentaamine – a
very simply chelator has been found that will hold hundredth molar concentrations
of several cations in non-aquoeous solution.

Experimental Section
Diethylene triamine and tetraethyelene pentaamine were purchased from
Aldrich and used with no further purification, as were octanal and dodecanal.
Solvents were purchased and used without distillation.
The formation of all ligands was performed in monoglyme, and in toluene,
with the amine first measured out and dissolved in the solvent. The aldehyde was
added only after the amine was completely solvated.
All solutions were stirred for a minimum of 16 hours, during which time
minimal color changes occurred from clear to a very pale yellow.
Samples of each ligand were dried by rotary evaporation, followed by a
minimum of 16 hours on a Schlenk line, and solvated in CDCl3 for characterization
via NMR. Both ligands were examined by 1H NMR using a Jeol 300 MHz
instrument, at 25°C.
Table 1 lists the amounts of amine and aldehyde used in production of Ligands
1 and 2.

Table 1. Ligand Synthetic Data

Amine Amine Aldehyde, g Molar Product
mass, g (mole) mass of – Ligand
(mole) amine Number
(g/mol)
Diethylenetriamine (N3) 1.104 2.533 (0.021), 103.0 1
(0.011) octanal
Tetraethylenepentaamine (N5) 2.031 3.962 (0.022), 184.32 2
(0.011) dodecanal

Two different techniques were used to form metal-ligand coordination

complexes.
The first technique involves dissolving in distilled water a stoichiometric
equivance of a metal salt to the ligand solution, then adding this to a separatory
funnel containing the stoichiometric equivalence of the ligand in non-aqueous
solvent. In all such trials, a precipitate formed immediately.
The second technique involved measuring out the proper amount of a dry
metal salt, routinely a molar equivalence to the ligand solution in non-aqueous
solvent. The dry salt was then added to the ligand solution directly. In several
cases, the coordination complex that formed remained in solution. Results are
summarized in Table 2.
84
 For both techniques, 0.044 M solutions of Ligand 1 were used, and 0.033 M
solutions of Ligand 2 were used. This allowed for an easy-to-measure, highly
reproducible set of starting samples and experimental size.

Table 2. Metal – Ligand Complex Formation

Ligand Ligand mass, Salt mass, g Visible Result, Visible Result,
g (mole x10-3) (mole x 10-3) technique 1 technique 2
1 0.118 (1.144) 0.198 (0.726) Brown precipitate Dark precipitate
Fe(ClO4)2·H2O
1 0.118 (1.144) 0.279 (1.02) Grey precipitate Grey precipitate
ZnClO4·6H2O
1 0.118 (1.144) 0.283 (0.870) Grey precipitate Grey precipitate
Pb(C2H3O2)2
1 0.118 (1.144) 0.187 (0.511) Blue-brown Brown precipitate
Co(ClO4)2·6H2O precipitate
1 0.118 (1.144) 0.058 (0.142) Grey precipitate Grey precipitate
Nd(NO3)3·6H2O
2 0.103 (0.198) 0.0504 (0.198) Brown precipitate Dark brown
Fe(ClO4)2·H2O solution
2 0.103 (0.198) 0.073 (0.198) Grey precipitate Yellowish solution
ZnClO4·6H2O
2 0.103 (0.198) 0.072 (0.198) Brown precipitate Brown solution
Co(ClO4)2·6H2O
2 0.103 (0.198) 0.075 (0.198) Grey precipitate Whitish-grey
Pb(C2H3O2)2 precipitate
2 0.103 (0.198) 0.088 (0.198) Whitish White solution
Nd(NO3)3·6H2O precipitate

Conclusions
This duo of multi-dentate ligands is both very easy and straightforward to
synthesize, requiring no specialized reaction apparatus. Because of a single,
diagnostic imine peak in an otherwise cluttered 1H NMR, the ligands can be
characterized without ambiguity, and without having to resolve the aliphatic
region of the 1H NMR spectrum.
The ligands produced here all have minimal functionality, yet possess enough
that they have proven to be excellent chelators. Their syntheses have been
accomplished by multiple undergraduate researchers.
The formation of metal-ligand complexes that precipitate readily from water
indicate that these ligands may find use as an inexpensive form of water remediator.
The fact that one of these ligands is capable of solvating metal salts into
non-aqueous media when dry metal salts were added directly to non-aqueous
solutions of the ligands was unexpected. It is an intriguing phenomenon however,
85
one that may hold promise for the use of these ligands in previously unexpected
applications.

References
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Program’s Science Plan; National Academies Press: Washington, DC, 2011.
2. Letter Report Assessing the USGS National Water Quality Assessment
Program's Science Framework; National Academies Press: Washington,
DC, 2010.
3. Vickers, A. The Handbook of Water Use and Conservation; WaterFlow Press,
2001; ISBN: 1-931579-07.
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(accessed December 11, 2017).
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6. Gould, R. F., Ed.; Saline Water Conversion − II; Advances in Chemistry 38;
American Chemical Society, January 1, 1963.
7. Ghaffour, N.; Missimer, T. M.; Amy, G. L. Technical review and evaluation
of the economics of water desalination: Current and future challenges for
better water supply sustainability. Desalination 2013, 309, 197–207.
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Characterization, Fate, Effects, and Removal; Advances in Chemistry 189;
American Chemical Society, November 1980.
9. Baker, A. Ed.; Environmental Chemistry of Lakes and Reservoirs; Advances
in Chemistry 237; American Chemical Society, May 05, 1994.
10. Urban Stormwater Management in the United States; National Academies
Press: Washington, DC, 2009.
11. Binnie, C. Basic Water Treatment 4th ed.; Royal Society of Chemistry:
London, 2009l ISBN 9781847558787.
12. Benvenuto, M. A. Industrial Chemistry; DeGruyter, Berlin, 2014.
13. Gray, J. Ed.; Water Contamination Emergencies: Can We Cope?; Royal
Society of Chemistry: London, 2006; ISBN 9780854046287.
14. Thompson, K. C. Ed.; Water Contamination Emergencies: Enhancing
our Response; Royal Society of Chemistry: London, 2006; ISBN
9780854046584.
15. Barber, N. L. Summary of Estimated Water Use in the United States in 2005;
U.S. Geological Survey Fact Sheet 2009-3098; U.S. Geological Survey,
2009.
16. Liquid Assets 2000; EPA-840-B-00-001; Office of Water, United States
Environmental Protection Agency: Washington, DC, 2000.
17. Dewan, N., Majestic, B. J., Ketterer, M. E., Miller-Schulze, J. P., Shafer,
M. M., Schauer, J. J., Solomon, P. A., Artamonova, M., Chen, B. B.,
Imashev, S. A., Carmichael, G. R. Tracing Dust Sources Using Stable Lead
and Strontium Isotopes in Central Asia. In Trace Materials in Air, Soil,

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 and Water; ACS Symposium Series 1210; American Chemical Society:
Washington, DC, 2015; Chapter 4, pp 79−98.
18. Bennett, K. Disappearance of the Aral Sea. World Resources Institute. http:/
/www.wri.org/blog/2008/05/disappearance-aral-sea (accessed December 11,
2017).
19. Nutrient Control Actions for Improving Water Quality in the Mississippi River
Basin and Northern Gulf of Mexico; National Academies Press: Washington,
DC, 2009.
20. Nissenbaum, A. The Dead Sea – An economic resource for 10,000 years.
Hydrobiologia 1993, 267, 127–141.
21. Jin, Y.; Wang, Q.; Taynton, P.; Zhang, W. Dynamic covalent chemistry
approaches toward macrocycles, molecular cages, and polymers. Acc.
Chem. Res. 2014, 47 (5), 1575–1586.
22. Izatt, R. M. The synthesis and ion bindings of synthetic multidentate
macrocyclic compounds. Chem. Rev. 1974, 74 (3), 351–384.
23. Bradshaw, J. S.; Izatt, R. M. Crown ethers: The search for selective ion
ligating agents. Acc. Chem. Res. 1997, 30 (8), 338–345.
24. Gordon, A. E. V.; Xu, J.; Raymond, K. N.; Durbin, P. Rational design of
sequestering agents for plutonium and other actinides. Chem. Rev. 2003,
103 (11), 4207–4282.
25. Sessler, J. L.; Melfi, P. J.; Dan Pantos, G. Uranium complexes of multidentate
N-donor ligands. Coord. Chem. Rev. 2006, 250, 816–843.
26. Hayes, C. E.; Leznoff, D. B. Actinide coordination and organometallic
complexes with multidentate polyamido ligands. Coord. Chem. Rev. 2014,
266–267, 155–170.
27. Hancock, R. D.; Martell, A. E. Ligand design for selective complexation of
metal ions in aqueous solution. Chem. Rev. 1989, 89 (8), 1875–1914.
28. Osakai, T.; Ogata, A.; Ebina, K. Hydration of ions in organic solvent and its
significance in the gibbs free energy of ion transfer between two immiscible
liquids. J. Phys. Chem. B 1997, 101, 8341–8348.
29. Kemsley, J. Extracting inorganic ions, organically. C&EN Global Entrep.
2016, 94, 18–19.

87
 Chapter 7

Analysis of Cosmetic Mineral Eyeshadows and

Foundations with a Handheld
X-ray Fluorescence Analyzer
Tiffany Tieu Ngo, Sara Thomas, Diamond Stokes, Mark A.
Benvenuto, and Elizabeth S. Roberts-Kirchhoff*

Department of Chemistry and Biochemistry, University of Detroit Mercy,

4001 W. McNichols Rd., Detroit, Michigan 48221, United States
*E-mail: robkires@udmercy.edu.

Twenty-five consumer cosmetic mineral makeups purchased

from local stores and three soil standard reference materials
(SRMs) obtained from the National Institute of Standards and
Technology (NIST) were analyzed using a handheld X-Ray
fluorescence (XRF) analyzer. The soil standards were used to
access the accuracy of the XRF analyzer. The XRF analysis
allowed for efficient analysis of the elemental composition of
several samples in a short amount of time. The results from
the analysis with the handheld XRF were within 15% or less
of the reported values for all three of the SRMs for aluminum,
potassium, iron, zinc, and strontium; and for two of the SRMs
for titanium, manganese, copper, rubidium, and lead. Common
elements in all makeup samples included potassium, aluminum,
iron, titanium, and rubidium. Lead was not detected in any of
the samples. In conclusion, XRF provides a fast, efficient, and
accurate method for elemental analysis of cosmetics.

© 2018 American Chemical Society

 Introduction

The first use of cosmetics dates to the ancient Egyptians in 4000 BC

(1). According to the Federal Food, Drug, and Cosmetic Act, cosmetics are
defined as “articles intended to be rubbed, poured, sprinkled, or sprayed on,
introduced into, or otherwise applied to the human body or any part thereof for
cleansing, beautifying, promoting attractiveness, or altering the appearance”
(2). Cosmetic products are used by many people of different races and ages,
and new products are continually introduced into the market. For this reason,
ongoing studies on the composition and effects of cosmetics are of importance.
Mineral foundations, specifically, have become increasingly popular and offer
an alternative to traditional powder foundations. These mineral foundations are
assumed to be natural-based cosmetics, formulated using natural, finely ground
minerals. However, there is little and confusing information on what formulates
a “true” mineral foundation since manufacturers have different ideas (3).
Although the skin is a barrier and thus beneficial for preventing exposure to
harmful substances, there are some trace elements or ingredients in cosmetics that
can penetrate the skin and produce systemic exposure (4–6). These trace elements
could include heavy metals such as lead. Long term exposure to lead has been
known to be toxic to children and pregnant women (7). Contact dermatitis can
result from exposure to metals such as nickel through cosmetics or jewelry (5,
6). In cosmetics, the FDA has established limits of less than 20 ppm for lead,
less than 3 ppm for arsenic and less than 1 ppm for mercury in ingredients and
colors, and less than 65 ppm mercury in cosmetics intended for use only in the
area of the eye (2). Because of the harmful effects of certain trace elements and
popularity of using cosmetics, the contents of cosmetics should be investigated
on a regular basis. Studies have been reported that used methods such as X-
Ray fluorescence (XRF), ICP-MS, and instrumental neutron activation to perform
elemental analysis of cosmetics (8–11). Neutron activation and X-Ray methods
are advantageous since they are nondestructive and do not require the sample to
be in solution. In addition, McIntosh, et al. recently reported that the results from
two XRF analyzers using the soil fundamental parameter method reliably detected
many elements and gave semi-quantitative estimates of the elements present at
higher levels in spices, herbal medicines and cosmetics as compared to Inductively
Coupled Plasma Optical Emission Spectrometry (ICP-OES) (11).
XRF is a powerful, non-destructive technique with a wide range of
applications including geological, chemical, environmental, industrial, forensic,
biological, and others (12–18). XRF has been used to study a variety of
substances including consumer products, food products, and dietary supplements
(19–35). XRF offers analysis on multiple elements, low cost, little to no sample
preparation, and high throughput. In X-ray spectroscopy, primary gamma rays
or X-rays expose a sample to radiation. This radiation ejects electrons from an
atom’s first (K) and second (L) inner shells. Electrons from higher shells fill the
vacancy to stabilize the atom. When the electrons fill the vacancy, a characteristic
fluorescence is emitted. The L to K transition is designated Kα, the M to K
transition is named Kβ, and the M to L transition is designated Lα. In each case, a
characteristic photon is released. The Kα and Kβ photons correlate to the Kα and

90
Kβ lines seen on the spectrum. (36–38). In this study, three standard reference
materials and twenty-five makeup samples were analyzed with a Bruker S1 Titan
handheld XRF analyzer to compare their elemental compositions.

Experimental Methods
Standard reference materials (SRMs) were obtained from the National
Institute of Standards and Technology (NIST). SRM 2586 is the Trace Elements
in Soil standard containing lead from paint (Nominal 500 mg lead/kg). This soil
standard has reported certified mass fractions for arsenic, cadmium, chromium,
and lead. It also has reported reference mass fractions for other elements
including aluminum, copper, iron, manganese, potassium, titanium, strontium,
and zinc (39). SRM 2709a, a San Joaquin Soil standard, has certified mass
fractions reported for several elements including iron, aluminum, potassium,
manganese, and strontium, and has reported reference mass fractions for many
elements including zinc and rubidium (40). SRM 2711a is a Montana II Soil
standard. It has reported certified mass fractions for many elements including
aluminum, potassium, titanium, iron, strontium, lead, copper and zinc (41). It
also has reported reference mass fractions for other elements including rubidium.
A Bruker S1 TITAN 600-800 handheld XRF analyzer was used to analyze the
samples and SRMs. For each SRM, five separate samples (3.0 g per sample)
were analyzed five times each for 120 s. The instrument was mounted on the
TITAN bench-top stand. Each sample was placed on the safety platform to ensure
the samples were analyzed from an equal distance. Before each analysis, each
sample cup was removed from the safety platform and rotated. The instrument
used a voltage of 45 kV and a current of 10 µA, with an Al/Ti filter. A Dell laptop
computer with Bruker S1sync software was used to control the instrument, and
data were collected and analyzed with the soil calibration fundamental parameters
(FP) method. The soil calibration method provided a basic set of excitation
conditions that could target most of the elements of interest. This calibration
has been optimized for a SiO2 matrix. The reported elements with this method
include Mg, Al, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr,
Y, Zr, Nb, Mo, Rh, Pd, Ag, Cd, Sn, Sb, Ba, La, Ce, Hf, Ta, W, Pt, Au, Hg, Tl, Pb,
Bi, Th, and U (42). Characteristic peaks for each element were identified using
S1PXRF software from Bruker. The SRMs, used as provided, were placed into
Chemplex Spectrocertified® Quality XRF sample cups (31.0 mm × 22.4 mm)
and were covered with Chemplex Spectromembrane® perforated thin film mylar
polyester sample support carrier films (3.6 µm) with a sealing ring. For each of
the standards, the concentrations (averages and standard deviations) of various
elements were determined and compared to the NIST standard values. The Limit
of Detection (LOD) and Limit of Quantitation (LOQ) for each the analyzed
elements using the soil calibration method were provided by Bruker (42). Those
reported in this study are shown in Table 1. Twenty-five mineral eyeshadow
and foundations were analyzed with a Bruker S1 TITAN 600-800 handheld XRF
instrument as described for the SRMs. Each of the eyeshadow samples were
measured out to one sample (6.0 g per sample) and analyzed five times for 120
91
s. Each of the foundation samples were measured out to five samples (7.0 g per
sample) and analyzed for five times each for 120 s. Results are reported in ppm
as average concentration ± standard deviation.

Table 1. Detection limits for selected elements with the S1 TITAN handheld
XRF analyzer using the soil calibration method (42)
Al K Ti Mn Fe Cu Zn Rb Sr Pb
LODa 960 41 20 18 13 5 3 3 4 11
(ppm)
LOQb 4800 205 100 90 65 25 15 15 20 55
(ppm)
a LOD, Limit of Detection. b LOQ, Limit of Quantitation.

Results and Discussion

All NIST standards and cosmetic samples were analyzed with the soil
calibration method with the handheld XRF analyzer. Since it is difficult to
calibrate the XRF analyzer for a variety of cosmetic matrices, the soil calibration
mode and its employment of Compton Normalization helps to correct for some
matrix effects. SRM 2586 is the Trace Elements in Soil standard containing
lead from paint (Nominal 500 mg lead/kg). SRM 2709a is the San Joaquin Soil
Standard, and SRM 2711a is the Montana II Soil standard. The concentrations
of each element are expressed in ppm (averages ± standard deviation), and the
percent relative standard deviations (%RSD) are also given. The averages of
each XRF analysis were compared to the reference or certified values for SRMs
2586, 2709a, and 2711a and expressed as percent error. Results from elements of
interest where all three standards had reported certified or reference values above
the LOQ for the instrument and the XRF results showed less than 15% error are
shown in Table 2. The concentrations obtained by XRF analysis are compared
to the reported values of the NIST standards for strontium, zinc, iron, aluminum,
and potassium. The percent error for strontium was less than 2% for all standards,
while for iron, aluminum, and potassium, the percent error was less than or equal
to 10.0%. For zinc, the percent error was between 11.5 and 13.7%. The values
of the %RSDs for almost all the elements are less than 10% and for most are
less than 5% showing that there is not a large spread of data points around the
mean. Shown in Table 3 are elements of interest where at least two of the soil
standards reported certified or reference values above the LOQ of the instrument
and the XRF results showed less than 15% error. The concentrations obtained
by XRF analysis are compared to the reported values of the NIST standards for
lead, manganese, titanium, copper, and rubidium. The percent error for lead was
less than 7% with SRMs 2586 and 2711a. The concentration was not reported
for SRM 2709a since the reported value was below the LOQ for the instrument
of 55 ppm Pb. For manganese, the percent error was 10% or less with two of the
standards and at 15.8 % with 2711a. For titanium, the percent error was 10% or
92
less with two of the standards and at 17.0 % with 2709a. For copper, the percent
error ranged from 5-13% for the standards that had copper levels well above the
LOQ of 25 ppm for the instrument. With SRM 2709a, the error was 26%, but
the value of 33.9 ppm is very close to the instrument’s reported LOQ of 25 ppm
which is determined with single element calibration standards. The percent errors
for rubidium were determined to be 6.8 and 10.2 %.
Twenty-five consumer cosmetic mineral makeups were purchased from
various stores. All were analyzed with the soil calibration method with the XRF
analyzer. The method was selected because of the similarities between the two
matrixes (soil and powdered makeup) and it reports results from 44 elements.
Each mineral makeup was assigned a sample identification designation (Table 4).
Makeup samples varied between color and shine. For example, the eyeshadow
M41 was lime green and M3 was an ocean blue. All foundations differed in the
shade of brown.
The results for the strontium and rubidium concentrations in the makeup
samples are shown in Figure 1. Two foundation makeups, M4 and M50, had the
highest strontium concentrations, while M28, M35, and M40 contain between 40
and 100 ppm of strontium. Results for rubidium are also shown in Figure 1, and
all the samples had some measurable concentrations of this element. Samples
M43 and M50 showed the highest amounts. Rubidium does occur naturally in
several potassium ores/salts as well as some alumino-silicate ores/salts (43), and
thus, may be contained in these samples due to the presence of potassium and/or
aluminum. None of the samples showed concentrations of lead above the LOD.
The results for the zinc concentration in the samples are shown in Figure 2. The
two samples with the highest concentrations of zinc are the foundation samples
M4 and M50. Zinc oxide and titanium oxide are used as protection from UV
light in some cosmetics (44). These two foundations which supply UV protection
apparently use zinc oxide for the advertised sun protection factor (SPF) since they
show high zinc concentrations and as shown later, lower titanium concentrations.
Results for aluminum, potassium, and iron are shown in Figure 3. All samples
showed the presence of aluminum and potassium. There was a greater difference
in the amount of iron in the samples with M6, M20 and M49 showing the highest
concentrations.
The results for the titanium analysis are shown in Figure 4. Many of the
samples contained titanium which is not unexpected since titanium dioxide is used
in various personal care products including sunscreens and loose face powders for
protection from UV light and as a whitening agent (44). This makes sense since
three of the samples with the highest values, M47, M48, and M49, are foundations
with lighter shades of brown or tan. The results for manganese are shown in
Figure 5. Samples M5 and M9 had high levels of manganese. These are both
eyeshadows with a purple color and manganese violet is often used as a purple
color in cosmetics (45). One cosmetic sample M17, a green eyeshadow, showed
a high concentration of copper at 92,600 ppm. Two other samples, M5 and M43,
had 93 and 161 ppm of copper, respectively. Several others M6, M7, M8, M16,
M17, M20, M28, M35, M39-42 and M44-46, had measurable levels of copper
under 50 ppm.

93
 Table 2. Concentrations of strontium, zinc, iron, aluminum, and potassium from analysis with the handheld XRF compared to the
NIST reported values for the SRMs where the analysis of three soil standards reported less than 15% errora
%
Sr (ppm) Zn (ppm) % Error Fe (ppm) % Error Al (ppm) % Error K (ppm) % Error
Errorb
2586 83 ± 2 311 ± 8 46410 ± 280 71648 ± 1557 10627 ± 154
XRFc (2.3)d (2.7) (0.6) (2.2) (1.5)
1.2 11.5 10.0 7.7 8.8
2586 84 ± 8 352 ± 16 51610 ± 890 66520 ± 760 9760 ± 180
SRM (9.5) (4.5) (1.7) (1.1) (1.8)
2709a 243 ± 4 88 ± 2 31676 ± 281 71379 ± 16000 20607 ± 810
XRF (1.5) (6.2) (0.9) (22) (6.6)
1.7 13.7 5.7 3.1 2.3
2709a 239 ± 6 103 ± 4 33600 ± 700 73700 ± 16000 21100 ± 600
SRM (2.5) (3.9) (2.1) (22) (2.8)
94

2711a 245 ± 4 358 ± 8 24083 ± 295 75168 ± 2268 24971 ± 668

XRF (1.8) (2.2) (1.2) (3.0) (2.7)
1.4 13.6 1.3 1.3 1.3
2711a 242 ± 10 414 ± 11 28200 ± 400 67200 ± 1000 25300 ± 1000
SRM (4.1) (2.7) (1.4) (1.5) (4.0)
a SRM values are certified or reference values as reported in Experimental Methods. b Percent error between measured XRF value and NIST reported

value. c Values (average ± standard deviation) for XRF analysis with handheld instrument. d Percent relative standard deviation.
 Table 3. Concentrations of lead, manganese, titanium, copper, and rubidium from analysis with the handheld XRF compared to the
NIST reported values for the SRMs where the analysis of two soil standards reported less than 15% errora
Ti Cu Rb
Pb (ppm) % Errorb Mn (ppm) % Error % Error % Error % Error
(ppm) (ppm) (ppm)
2586 450 ± 9 901 ± 18 6763 ± 117 77 ± 2
N.D.g
XRFc (2.1)d (1.7) (1.7) (2.6)
4.1 9.8 10.0 5.0
2586 432 ± 17 17070 ± 840 6050 ± 660 81
N.D.
SRM (3.9) (4.9) (11) (0)
2709a Below 484 ± 20 3930 ± 220 43 ± 3 89 ± 2
XRF LOQe (4.2) (5.6) (7.0)f (2.1)
8.4 17.0 27 10.2
2709a 17.3 ± 0.1 529 ± 18 3360 ± 70 33.9 ±0.5 99 ± 3
SRM (1.0) (3.4) (2.1) (1.5) (3.0)
95

2711a 1492 ± 28 568 ± 38 3161 ± 61 122 ± 4 112 ± 2

XRF (1.9) (6.7) (1.9) (3.0) (1.5)
6.5 15.8 0.3 12.9 6.8
2711a 1400 ± 10 675 ± 18 3170 ± 80 140 ± 2 120 ± 3
SRM (0.4) (2.7) (2.5) (1.4) (2.5)
a SRM values are certified or reference values as reported in Experimental Methods b Percent error between measured XRF value and NIST reported value. c

Values (average ± standard deviation) for XRF analysis with handheld instrument. d Percent relative standard deviation. e LOQ, level of quantitation of
55 ppm. f Near LOQ of 25 ppm for Cu. g N.D., not detected.
 Table 4. Consumer mineral makeup analyzed by XRF
Designation Makeup Identifier Type
M2 Danzig Eye Shadow
M3 Paranoid Eye Shadow
M4 Tan Foundation
M5 Water Lily Eye Shadow
M6 Sex Kitten Eye Shadow
M7 Wild Flower Eye Shadow
M8 Soiree Eye Shadow
M9 Berry Flambe Eye Shadow
M16 Pink Eye Shadow
M17 Green Eye Shadow
M20 Red Eye Shadow
M28 Gray Eye Shadow
M 35 Beige Eye Shadow
M39 Raw Power Eye Shadow
M40 Black No.1 Eye Shadow
M41 Electric Warrior Eye Shadow
M42 Synergy Eye Shadow
M43 Liberty Eye Shadow
M44 True Gold Eye Shadow
M45 Bare Skin Eye Shadow
M46 Queen Tiffany Eye Shadow
M47 Fairly Medium Foundation
M48 Golden Tan Foundation
M49 Medium Deep Foundation
M50 Deep Foundation

96
Figure 1. Concentration of strontium and rubidium in the makeup samples as
determined by XRF analysis.

Figure 2. Concentration of zinc in the makeup samples as determined by XRF

analysis.

97
Figure 3. Concentrations of aluminum, potassium and iron in the makeup
samples as determined by XRF analysis.

98
Figure 4. Concentration of titanium in the makeup samples as determined by
XRF analysis.

Figure 5. Concentration of manganese in the makeup samples as determined

by XRF analysis.

99
 Conclusions
A soil calibration method with a handheld XRF was used to analyze three soil
standard reference materials and twenty-five consumer mineral makeup samples.
The results from the soil method can be used to quickly compare the elemental
composition of the different makeup samples Comparing the reported results with
the certified and reference values of the standard reference materials was used to
verify that an element was present and the XRF’s precision and accuracy. There
were five elements identified in some or all the makeup samples which were
strontium, zinc, iron, aluminum, and potassium. These elements were verified
with all three soil standard reference materials. In contrast, there were five other
elements that were verified with two soil standard reference materials. These five
elements were lead, manganese, titanium, copper, and rubidium. Of these five,
all but lead were found in some or all the samples. None of the cosmetic samples
analyzed contained levels above the FDA allowable levels of toxic metals (Pb,
As, or Hg) (2). The XRF method is a quick way to analyze several samples. An
instrument-supplied calibration method such as the soil calibration allows quick
analysis of multiple elements to compare between samples. If more labor, time,
and cost-intensive investigations are to be performed, this method provides an
efficient way to quickly and accurately screen candidates before further analysis.

Acknowledgments
Work reported in this publication was supported by the National Institutes
of Health Common Fund and Office of Scientific Workforce Diversity under
three linked awards RL5GM1189XX, TL4GM1189XX, 1UL1GM1189XX
administered by the National Institute of General Medical Sciences, the University
of Detroit Mercy’s McNichols Faculty Assembly Internal Research Fund, and the
College of Engineering & Science at the University of Detroit Mercy.

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 Chapter 8

Arctic Communities as Sites of Local Field

Work in Environmental Chemistry
Mark H. Hermanson*,1 and Sydney Le Cras2
1Hermanson & Associates, LLC, 2000 53rd St. W.,
Minneapolis, Minnesota 55419, United States
2Department of Natural Resources Management & Environmental Sciences,

California State Polytechnic University, 180 North Poly View Drive,

San Luis Obispo, California 93407, United States
*E-mail:markhermanson@me.com.

The Arctic is remote from major population centers and

industrial or agricultural activities and is often assumed to be
“pristine”. Considering that it is cold, dry and seasonally dark,
the usual environmental processes affecting distribution or
accumulation of contaminants is clearly different. However,
since the late 1980s, various investigators have found that
contamination levels of industrial and agricultural chemicals
are sometimes very high in the Arctic. In some cases, the
contaminants have traveled to the Arctic through the atmosphere
as gasses or associated with particles in a process known as
long-range atmospheric transport, or LRAT. These contaminants
may be deposited on glaciers or ocean surfaces and in the case
of the latter, will enter the food chain, including humans who
rely on wild sources of food from the marine environment.
In other cases, contaminants may arrive in the Arctic through
imported construction or other materials. In the case of energy
production, the emissions are the same as in any populated
place. Here we discuss the early history of contamination in
the Arctic and the more recent sampling, analysis and results
of different environmental chemistry campaigns in the Arctic.
Resident university students have been involved in sampling
and data gathering for the analysis of atmospheric mercury
released from coal combustion, and the apparent emissions
of various flame retardants into the atmosphere from local

© 2018 American Chemical Society

 building materials or LRAT. The site is in Longyearbyen, on
Svalbard, which was organized as a coal-mining town in 1906,
and continues to operate today as a tourist site with a small
university offering courses relevant to the Arctic. Electricity has
been generated in Longyeaarbyen by coal combustion for about
100 years, and the effect during sampling in 2016 showed a
daily atmospheric mercury cycle, with an average concentration
similar to “European polluted air”, and average air in Detroit,
USA. Our investigation of flame retardants showed that the
organophosphorus flame retardants (OPFRs), considered to
be replacements for now-banned brominated flame retardants
(BFRs), have a concentration similar to non-urban areas in the
U. S. Great Lakes region. The average content of the OPFRs
was at least one order of magnitude greater than the BFRs.
Using an Arctic community for investigations of environmental
chemistry leaves students with a strong background about
the impacts of urban and industrial pollution on the Arctic
environment, demonstrating that the Arctic is part of the global
contaminant distribution system, and is not “pristine”.

Introduction: Why Environmental Chemistry in the Arctic?

The study of environmental chemistry involves the reactions, movements
or accumulations of chemicals in various environmental compartments. Rarely
do investigators know in advance what they are looking for because chemicals
observed are seen only by using analytical instruments. The analyte list is often
developed from policy agreements about chemicals in the environment, such as
the Stockholm Convention (www.pops.int). And the result is often identification
of pollutant chemicals with unknown sources except at sites of well-known
contamination. The typical image of the Arctic is of bright white, clean snow,
clear, uncontaminated skies, very few people, and no trace of any known
contamination. Why is there a need to investigate environmental chemistry in a
pristine environment? Especially considering that it is too cold, too dry, and in
the winter, too dark to support many common chemical reactions or movements.
The concept of the Arctic as a pristine place, cut off from the rest of the world,
and particularly from the contaminating effects of human activity because of its
remote (and usually unknown) location, has persisted for decades. Some opinions
about this began to change as early as the 1950s when spring-time weather flights in
Alaska (the Ptarmigan flights) observed what was characterized as the Arctic haze,
an optical effect of high-altitude “smoke” observed from aircraft. The origin of the
“smoke” was unknown, and the reason for its appearance only at high altitude was
also unknown (1). One assumption was that the material in the “haze” may have
originated with forest fires, not considering that urban or industrial particles could
move to the Arctic. That view began to change when Murozumi et al. (2) measured
a 200-times greater Pb concentration in surface ice and snow over pre-industrial
background levels from an ice core collected near Camp Century, a remote glacier-
106
covered site in Greenland. The increase in glacial Pb concentrations was attributed
to growth of Pb smelting before World War II and use of tetra-ethyl Pb in motor
fuel, which began in 1924, and had rapid growth after World War II. A transport
mechanism of atmospheric dust, contaminated with industrial and urban Pb from
urban/industrial areas to Greenland, was proposed.
Even though the Pb results from Murozumi et al. (2) were generally well
received, the magnitude of movement and accumulation of contaminants to the
Arctic was not appreciated for nearly 20 years.
The observations of Arctic Haze and Pb in Greenland ice led to emphasis
on effects of long-range atmospheric transport (LRAT) to the Arctic from
urban/industrial and agricultural areas. This approach has dominated
investigations of environmental chemistry in the Arctic for decades. Studies
have shown accumulated polychlorinated biphenyls (PCBs), pesticides, and
brominated flame retardants (BFRs) in glaciers where these compounds were
obviously never manufactured or used. The attraction for LRAT studies arises
from the low human populations in the Arctic and the general lack of industrial
or agricultural activity meaning that the contaminants must travel long-distances
through the atmosphere. And long travel means that the contaminants must be
persistent and undergo transformation from gas to condensed phases under the
influence of cold Arctic air temperatures. Persistence is often associated with the
reaction rate of a substance with hydroxyl radicals (OH.) produced by photolytic
reactions and which are considered to be the most important atmospheric
substance to oxidize many different contaminant gases. But it is also known that
contaminants can travel to the Arctic associated with particles and in that form
are less likely to be oxidized by OH., intensifying their persistence.
The earliest observation of direct human effect by contaminants in the
Arctic appeared in 1989 when Dewailly et al. (3) published the results of a
survey of organic industrial contaminants in breast milk in an Inuit community
in northern Quebec. The intent of the study was to use the Inuit community as
a “background” amount for comparison to samples from Quebec City which
were assumed to show the effects of typical urban/industrial living. It turned
out that the Inuit concentrations were several times higher than the Quebec City
samples, and after confirmation with further samples, it was discovered that
the difference was attributable to the Inuit diet which was largely comprised
of community-harvested sea food, particularly seal and fish. This should have
been no surprise because it was earlier noted that seals and fish in the Arctic
were affected by bioaccumulation of contaminants that condensed into the
marine environment from the atmosphere, showing that LRAT of semi-volatile
industrial chemicals was having a significant effect on contamination of marine
ecosystems in the Arctic (4). The biomagnification of contaminants from
fish to seals was significant, and in hindsight, it should have been clear that
biomagnification from seals to humans would be large as well. In the Dewailly
et al. study, the contaminant class was polychlorinated biphenyls (PCBs)
which were not manufactured anywhere in North America after 1977 and
Europe after 1983. Immediately, the issues of environmental persistence and
bioaccumulation/biomagnification were considered to be important, and have
been ever since.

107
 The difficulty with a study like Dewailly et al. (3) was how to address the
contamination issue with the local community where it was found. How does one
report a high level of PCB contamination in human breast milk to a population
which has no industry, may not have any PCB sources in the community, and not
know – or even not care – what PCBs are? After all, nobody can see environmental
chemical contaminants in most cases, so how does one convince anybody that they
really are present?

Atmospheric Mercury from a Coal-Fired Power Plant

on Svalbard
Longyearbyen, on Svalbard, is the location of the only operating coal power
plant in a Norwegian territory and has depended on this form of energy throughout
its history (Figure 1). Unilike the community where Dewailly et al. conducted
research on organic contaminants in breast milk, Svalbard has no indigenous
population. Everyone there, including environmental chemistry students and
scientists working in the community, is from elsewhere. As a result, students
and researchers have a direct role in understanding the environmental impacts
that they and others in the community create simply by living and working there
and consuming energy or constructing buildings in the process. One outstanding
feature in Longyearbyen is the coal plant, one of only two that we know of in
the Arctic. This plant creates an opportunity to measure the impact of energy
production on the environment in a way that people living in a larger community
elsewhere in the world would not consider. The interest in investigating a coal
plant in this situation arises from the image of the Arctic as “pristine”, and
therefore a place where, with no coal plant, the residues of energy production
would not expect to be found, unless delivered by LRAT. While combustion
chemistry is not often related to investigations in environmental chemistry, one
learns that researching the effects of living in such close proximity to a coal plant
that expanding into new areas of chemical investigation becomes a necessity if
one is to comprehend the real environment.
Energy production in Arctic towns involves use of fossil fuels, usually
transported there from elsewhere. In most towns, diesel fuel is used. The residues
of combustion will always leave a chemical imprint on the community, and the
magnitude of that imprint depends on the fuel and how it is managed. Since
mercury is a significant neurotoxin to humans, and can move easily between
environmental compartments, we decided that it would be useful to learn more
about it for our courses at the University Center on Svalbard. Unlike the Inuit
community where Dewailly et al. (3) worked, having a resident student population
in the Arctic creates the opportunity to make local contaminant issues part of the
curriculum.
Mercury analysis in the Arctic atmosphere has focused on long-term
measurements of elemental mercury (Hg0(g)) at Alert, on Ellesmere Island
in Canada (5), at Zeppelin Observatory on Svalbard (6) and at Station Nord
in northeast Greenland (5). Studies at these sites are characteristic of many
contaminant investigations in the Arctic, including Svalbard, that focus on
108
the effects of LRAT and deposition with few, if any, observations of local
contaminant sources. Some investigators have concluded that there are no
anthropogenic mercury emissions in the Arctic (7). However, Svalbard has two
potential emissions sources, both coal-burning power plants in Longyearbyen and
Barentsburg (Figure 1), which need to be considered.

Figure 1. Svalbard map highlighting Longyearbyen (78.22°N 15.65°E). From

the Norwegian Polar Institute.

Hg0(g) has an estimated atmospheric lifetime of about 1 year6 so it is well

mixed in the atmosphere and distributed globally in concentrations that average
between 1.5 – 1.7 ng m-3 (6, 8, 9). Anthropogenic emissions are dominated by coal
combustion and these emissions are highly correlated to the amounts of mercury in
the coal that is burned, suggesting that the process will convert mercury to the gas
phase (9). Mercury in coal and combustion systems can be found in three different
forms, as HgS found in pyrite (see below), as Hg2+(aq) after oxidation, and as
Hg0(g), the latter being the most common form of atmospheric emissions. Mercury
in coal is normally HgS and is a contaminant in pyrite (FeS2) commonly found
in bituminous coal (10–12). Modern coal plants wash bituminous coal before
combustion in order to remove pyrite because it does not support combustion (13).
Washing removes variable amounts of mercury ranging from 10 – 50%, depending
109
on the coal (11, 13). For unwashed coal, sulfur from both iron and mercury will
oxidize to SO2, the discharge of which is regulated in some countries. After HgS is
oxidized, mercury will be released in some form, perhaps as an HgCl2 or as Hg2+(aq)
in the presence of water in contact with combustion gases. Mercury may remain
as Hg2+(aq), but in the presence of SO32-(aq), a strong Hg2+(aq) ligand, it will accept
unshared electrons from SO32-(aq) to form Hg0(g) and move in to the atmosphere
following a series of intermediate reactions (14, 15).
In 2016, a guest lecturer in one of our university courses on Svalbard deployed
a portable mercury analyzer at our site during her visit in early May. The intent
was to measure the concentrations of Hg0(g) at a site where it has not been measured
before but where the concentration might be influenced by the local coal-burning
power plant. This research during our course is the first that we are aware of
to measure Hg0(g) concentrations generated from an anthropogenic source in the
Arctic. Atmospheric contamination in Longyearbyen by substances other than
mercury has been documented, showing that the community is affected by some
typical urban contaminants (see section about flame retardants, below).
In Longyearbyen we collected continuous air samples, with 5-second interval
sampling and 10-minute reporting interval, from 2 to 10 May 2016 (Monday
to Monday) using a Lumex 915+ atomic fluorescence spectrophotometer. The
sampling site was 725 m upwind (to the east) from the coal-burning power
plant. The device, which was on loan to us during this time, was located inside
the Svalbard Research Park (Svalbardforskningsparken) with a sampling tube
extending outside. It was calibrated against a mercury saturated cell before being
put into operation. It was reset to zero by drawing air through a dedicated inlet
with a black carbon absorbant at the beginning of alternate sample reports (every
20 minutes). As a spectrometer packaged in a small field-ready case, it was
typical of several modern instruments available for measurement of trace gases
in the atmosphere.
Movement of Hg0(g) could be affected by meterological variables, so the class
collected air temperature data (hourly averages) from the Adventdalen weather
station, located 1.02 km ESE from the Svalbard Research Park. Wind direction
and speed data (hourly averages) were from Svalbard Lufthavn (airport), located
2.36 km northwest. The variability of these meteorological data over time were
associated with Hg0(g) variability in an effort to determine if weather conditions
had an effect on our observations.
Three notable results are apparent in the Hg0(g) data set from Longyearbyen.
First is a large daily cycle of Hg0(g) with the highest daily concentrations, 5.7 ng
m-3, occurring around midday and the lowest values, about 1.0 – 1.5 ng m-3, within
three hours of midnight (Figure 2). The low end of the range is consistent with the
lowest average concentration, 1.23 ng m-3, observed during a cruise in the Arctic
Ocean (16). This range is a factor of about 5.7 every day showing the effect of a
large, active source, which we assume is the coal-burning power plant. All Hg0(g)
investigations that we have found in the literature show ranges, but not on a daily
basis: At the Arctic sampling site at Alert, the average annual range of Hg0(g)
was a factor of 2 between 1995 and 2007 (17), less than half the daily range at
Longyearbyen. The second result is the extreme event on 9 May, with a jump
in concentration up to 42 ng m-3 lasting 20 minutes during a series of obserations

110
over about 90 minutes from beginning to end (not shown). Following this, the daily
cycle was once again observed. The cause of this event is unknown but assumed to
be associated with power plant emissions. Including the extreme event, the range
of values in Longyearbyen is 1.0 to 42 ng m-3. Without including the extreme
values on 9 May, the third major result is the average value of 2.7 ng m-3 (+/- 0.87,
n = 1131), between 70% and greater than 100% more than the average Arctic
background amounts that range from 1.23 to 1.56 ng m-3 (5–8, 16).

Figure 2. Daily Hg0(g) concentration cycles from Longyearbyen 2 to 10 May 2016

without peak values on 9 May. Dates are at 00:00 each day.

The Longyearbyen average is greater than the “European polluted air”

average concentration of 2.5 ng m-3 from Mace Head, Ireland (18, 19), where
the maximum did not exceed 3.5 ng m-3, well below the Longyearbyen daily
maximum. Mace Head was among the longest active atmospheric Hg0(g) sensors,
and is near the western-most part of Europe (excluding Iceland), away from
European pollution sources unless easterly winds prevail (18). The Mace
Head average for “European polluted air” is about the same as the average
observed in Detroit, USA (2.47 ng m-3) during 2004, a site known to be affected
by many industrial/urban sources (20). The Detroit values range from 0.36
– 25.6 ng m-3, the maximum about 60% of the peak concentration observed
in Longyearbyen. The peak value in Longyearbyen is similar to the lower
concentrations of highly contaminated air events observed in East St. Louis USA
from October to December 2002, which ranged from 50 – 220 ng m-3 Hg0(g) (21),
111
the latter value approaching the no-effect reference concentration of 300 ng m-3.
These comparisons show that Longyearbyen is affected by a strong, continuous
anthropogenic source of Hg0(g).
A comparison of the daily Hg0(g) cycle with air temperature, wind direction
and speed did not show an association with any of these variables. Air temperature
variation (Figure 3) and wind direction or speed variation (not shown) did not show
daily variability consistent with Hg0(g) trends. In fact, our Hg0(g) sampling location
was upwind from the power plant during almost the entire sampling period with
wind speed greater than 5 m s-1 most of the time.

Figure 3. Hourly average air temperature at Longyearbyen during Hg0(g)

sampling, 2 – 10 May 2016.

The Longyearbyen power plant, which we assume is the source of the high
average and daily cycle of Hg0(g), began operating in 1983. It is a 10 MW plant
that burns about 25 000 MT of bituminous coal per year (2015) taken from Mine 7,
about 12 km east from the plant. This coal has a high pyrite (FeS2) content, which
is known to be contaminated with HgS (11, 12), noted above. As far as we know,
FeS2 is not washed from Mine 7 bituminous coal, so associated Hg becomes part
of the combustion residue. In general, older coal combustion systems, like the one
in Longyearbyen, cannot be adapted to operate with washed coal (13).

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 High values of Hg0(g) have been observed in the emissions of bituminous coal
plants in China, and those emissions have been highly correlated with the amounts
of mercury found in the coal that is burned (9).
In December 2015, the Longyearbyen plant was required to install air
pollution control devices (APCD) to reduce emissions of NOx, particles, and
SO2. Other monitored emissions included CO2, O2, temperature, and airflow (m3
per hour) (22). The first step in the APCD process treats NOx using urea. This
is followed by an electrostatic precipitator to remove particles. The third step is
wet flue gas desulfurization (FGD) using sea water. Most wet FGD processes in
coal combustion systems employ a limestone-gypsum system (13, 23, 24), but
the cost of this would likely be prohibitive in Longyearbyen because there is no
local limestone source, while sea water is plentiful and free.
In the FGD step using sea water, reaction of dissolved SO2 with H2O will first
produce SO32-(aq) because the S in both SO2 and SO32-(aq) has the same oxidation
state (4+). Protons resulting from this reaction are neutralized by natural seawater
alkalinity (23). The SO32-(aq) will react readily with Hg2+(aq) either from the flue
gas (including pyrite residues) or seawater itself, with S contributing unshared
electrons to form Hg0(g) which will move to the atmosphere after a series of
intermediate reactions (14, 15).
The process of chemical reduction of Hg2+(aq) by SO32-(aq) has been observed at
coal-fired power plants using sea water FGD in China (10, 25). The result is high
Hg0(g) concentrations ranging up to 13.5 ng m-3, approximately 8 times greater
than the global average, above the aeration ponds where FGD takes place or at
discharge points of FGD water back in to the ocean.
Combustion literature also suggests that Hg0(g) emissions from coal
combustion may result from SO32-(aq) added for deoxygenation to prevent
corrosion in the combustion system (26). Again, SO32-(aq) will reduce Hg2+(aq) to
Hg0(g), especially at high temperatures (14, 15).
This short Hg0(g) sampling campaign from Longyearbyen clearly shows the
presence of both high emissions and daily trends of Hg0(g) in an Arctic settlement
relying on coal combustion for local energy. The local and regional impacts of
these emissions have not been studied. However, Dastoor and Durnford (27) noted
that Hg0(g) concentrations at the Zeppelin Observatory in Ny-Ålesund (Figure 1)
in 2007-2008 were 1.6 – 1.7 ng m-3, and significantly higher than at Alert, in the
far northern Canadian Arctic, from 2005 – 2009 (1.4 - 1.6 ng m-3). They attributed
this higher concentration to seawater emissions from the West Spitsbergen Current
near Svalbard that originated near North America (and possible industrial mercury
sources) with the Gulf Stream. The higher concentrations at Zeppelin than at both
Station Nord and Alert were also noted by Angot et al. (5) and were attributed to
the fact that Zeppelin during summer is surrounded by open water – presumably
emitting Hg0(g), while Station Nord and Alert are surrounded by multi-year sea
ice during most years, preventing emissions from surface water. Hirdman et al.
(28) attribute peak Hg0(g) concentrations at Zeppelin during winter to transport of
comparatively contaminated air masses from Europe. An additional consideration,
based on our results, is that the source in Longyearbyen may contribute to higher
Hg0(g) at Zeppelin which is 114 km NW (downwind) from Longyearbyen (29).

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 Documentation of the effects of this Arctic coal-burning site on Hg0(g)
concentrations and distribution in the eastern Arctic is needed, along with
on-going measurements to observe seasonal and long-term concentration changes.

Particle-Associated Flame Retardants in Air in an Arctic Town

Beginning in 2010, we made an exercise of having students collect air samples
on the roof of the Svalbard research park in our environmental chemistry courses.
For both courses, it was necessary for students to understand how sampling air
differs from sampling other environmental matrices.
Collecting environmental samples for chemical analysis involves removing
the substrate, whether it is ice, snow, water, soil or organisms, from the native
system and putting it into a lower density matrix, the atmosphere, to measure
the volume or mass. This is followed by measurement of chemical analytes of
interest found in that volume or mass. An exception is collecting samples of the
atmosphere itself because there is no lower density system to accept the sample in
order to measure its volume. Air sampling requires a device to remove the analytes
of interest from the air. The issue then becomes a question of how to collect and
measure the volume of air from which the analytes have been removed.
This issue first appeared in the scientific literature in the 1930s when Drinker et
al. (30) performed toxicology experiments with rats to approximate the gas phase
chlorinated biphenyl concentrations in factory air which were thought to affect
workers at a manufacturing site. A major challenge became measuring the mass
of contaminant that would have toxic effects, requiring controlling the amount of
toxin released into the air but more importantly, calculation of the volume of air to
which the test organisms were being exposed in the experiments. The description
of the experiment refers to an orifice calibrator used to identify air flow (and thus
volume over a unit of time), and is the earliest mention of this that we have found
in the literature.
The need for high volume air sampling – and the need for calibration of
flow rate and volume using an orifice calibrator - became even more important in
the USA with founding of the American Conference of Governmental Industrial
Hygienists (ACGHI) which developed recommended concentration limits of a
variety of contaminants in air that in 1966 resulted in a list of 78 mostly organic
compounds (31). This list, along with limits proposed by Drinker et al. (30)
introduced an added complication with air sampling, which was that the volume
collected needed to be very large (typically greater than 500 m3) because of the
toxic effect of a small mass of contaminant in air. High-volume (Hi-Vol) air
sampler development soon followed the ACGHI limits with early designs in the
1960s that included use of vacuum pumps that could move large volumes of air
(32). Later development in the 1980s included systems that have proven to be
reliable in extreme weather conditions (33).
Once students were able to quantify the volume of air collected over a period
of time, we were able to analyze the samples for a series of particle-associated
flame retardants, including some BFRs and organophosphorus flame retardants
(OPFRs) that are often considered to be replacements for BFRs that are no longer
114
used or produced because of restrictions or bans by government agencies or treaties
such as the Stockholm Convention.
While we were able to conduct the sample collection as a course exercise,
the samples had to be sent elsewhere for analysis by gas chromatography / mass
spectrometry. Although the students were not able to experience the analytical part
of the work, they were able to understand the meaning of the results.
Earlier results on investigation of BFRs in an ice core from Svalbard
suggested that concentrations of some of them were high, particularly those that
were high production (34), leading us to realize that particles, with their associated
contaminants, were subject to LRAT to glacier surfaces in the European Arctic.
In this exercise, since the samples were collected on the roof of our building, we
had to assume that the presence of these contaminants could be from either LRAT
or from local emissions or from our building. Since this was the first investigation
of this type, we were comfortable with this assumption.
Organophosphate esters (OPEs) and BFRs are used in a large variety of
consumer and industrial products to delay ignition and slow the spread of fire in
order to comply with flammability regulations. Polybrominated diphenyl ethers
(PBDEs) have historically been the most widely used BFRs, but these compounds
now are off the market globally due to their persistence, bioaccumulation, and
toxicity. Several PBDE compounds were added to the Stockholm Convention
and are targeted for elimination of production and use.
To compensate for the restrictions placed on PBDEs, the production and
use of OPEs have increased. Halogenated (mainly chlorinated) OPEs, such as
tris(2-chloroethyl) phosphate (TCEP), tris(1-chloro-2-propyl) phosphate (TCPP)
and tris(1,3-dichloropropyl) phosphate (TDCPP), as well as non-halogenated aryl
OPEs, such as triphenyl phosphate (TPP) and tricresyl phosphate (TCP), are used
as flame retardants in building materials, electronics, plastics, and furniture and
textiles. Some of the non-halogenated alkyl OPEs are also used as plasticizers and
anti-foaming agents in hydraulic fluids, lacquers, and floor polishes. OPEs have
been in use for several decades, and their global consumption as flame retardants
was 270,000 tons in 2005. However, their production increased after the PBDE
phase out; for example, production volumes for TDCPP, TPP, and TCPP in the
United States increased from 450-4500 metric tons in 1990 to 4500-22500 metric
tons in 2006. In Western Europe, the OPE production increased at about 10%
between 2001 and 2006. Now OPEs constitute about 20% of the world’s flame
retardant consumption. Despite these rapid increases in the use of OPEs, data on
their environmental concentrations in the Arctic are rare, making new samples
and data especially valuable.
Like BFRs, OPEs are additive flame retardants and not covalently bound to
the material in which they are used; hence, they can leach into the environment.
Because of low vapor pressures, they are associated with particles in the
atmosphere, indicating that if influenced by LRAT, it will be different from
gas-phase compounds.
Figure 4A shows the concentrations of the individual OPEs in Longyearbyen.
The data are put in summary form as a class exercise showing, among other
things, how statistical interpretations can be made. The sum of the eight OPE
concentrations shown (ΣOPEs) ranged from 33 to 1450 pg/m3, with the mean

115
ΣOPE concentration of 426 ± 57 pg/m3. The non-chlorinated tri-n-butyl phosphate
(TnBP) and 2-ethylhexyl-diphenyl phosphate (EHDPP) were the most abundant
OPE congeners measured and were detected in all the samples at concentrations
ranging from 5.6 to 1000 pg/m3 for TnBP and 6 to 300 pg/m3 for EHDPP.
Mean tris(butoxyethyl) phosphate (TBEP) concentrations were statistically
indistinguishable from the TnBP and EHDPP concentrations, but TBEP was
detected only in ~25% of the samples with the concentrations ranging from 47
to 210 pg /m3. In addition, triphenyl phosphate (TPP) and tris(2-ethylhexyl)
phosphate (TEHP) were detected in all samples, but at lower concentrations
ranging from 1 to 52 pg/m3 and 1 to 42 pg m-3, respectively. Overall, the sum of
all non-chlorinated OPE concentrations was ~75% of the ΣOPE concentrations.
The sum of the three chlorinated OPEs, TCEP, TCPP, and TDCPP, was only ~25
% of the ΣOPE concentrations. The most abundant chlorinated OPE was TCPP,
which was detected in all samples with the concentrations ranging from 10 to
190 pg m-3. Average TDCPP concentrations were statistically not distinguishable
from the average TCPP concentrations, but this OPE was detected only in ~20%
of the samples at concentrations ranging from 2 to 290 pg/m3. Finally, TCEP
concentrations were the lowest among the levels of the chlorinated OPEs and
ranged from 4 to 63 pg/m3.
There are only two studies that have measured atmospheric OPE
concentrations in the Arctic environment: ΣOPE concentrations of ~120–1100
pg/m3 were reported in three particle phase samples collected at Ny-Ålesund,
and over the Arctic Ocean the reported ΣOPE concentrations ranged from 237
to 1270 pg/m3 in particle samples. Interestingly, both of these studies reported
that chlorinated OPEs dominated the ΣOPE concentration, which is different
from our findings. The OPE profile found in our samples agrees with the ΣOPEs
profiles measured at North American remote sites, where the non-chlorinated
OPEs, TnBP, TBEP and TPP, were found to comprise up to 85% of the ΣOPE
concentrations. Overall, our data, like that in the literature, clearly show that
OPEs are widely present in the atmosphere at remote regions throughout the
world, including polar regions. It has been shown that particle-bound OPEs
are persistent in the atmosphere with regard to OH. oxidation, with estimated
atmospheric lifetimes ranging from ~6 days for non-chlorinated OPEs to ~14 days
for TDCPP. Longer atmospheric lifetimes suggest that OPEs can undergo LRAT.
Along with the OPEs, we measured many BFRs and Dechlorane Plus (DP)
to compare to the OPE concentrations. Figure 4B shows the concentrations
of total BFRs (ΣBFRs, the sum of 34 PBDE congeners, tetrabromo-p-xylene
(pTBX), pentabromo-benzene (PBBz), pentabromoethylbenzene (PBEB),
hexabromo-benzene (HBB), 2-ethylhexyl-2,3,4,5-tetra-bromobenzoate (TBB),
bis(2-ethylhexyl)-tetrabromophthalate (TBPH), 1,2-bis(2,4,6-tribromo-
phenoxy)ethane (BTBPE), and decabromodiphenyl-ethane (DBDPE)), total
PBDEs (ΣPBDEs, the sum of 34 PBDE), BDE-47, 99, 209, pTBX, PBBz, HBB,
PBEB, and DP (the sum of the syn- and anti-DP). ΣBFR concentrations were in
the range of 3–77 pg/m3, with the average concentration of 16 ± 2.7 pg/m3. TBB
and TBPH were the dominant non-PBDE BFRs measured in these samples and
comprised ~46% and 17% of ΣBFR concentrations, respectively. TBB and TBPH
concentrations varied from 0.2 to 58 pg/m3 and 0.3 to 14 pg/m3, respectively and

116
were higher than concentrations previously reported for atmospheric vapor-phase
samples collected in the Canadian and European Arctic and over the Arctic Ocean
in 2006–2010. TBB and TBPH are major components of Firemaster 550, and
the presence of relatively higher concentrations in our Longyearbyen samples
could be related to a recent increase in the use of Firemaster 550. One way to
identify Firemaster as a parent product from observed concentrations is a ratio of
TBB to TBB+TBPH concentrations. We know that this ratio in the commercial
Firemaster 550 mixture was 0.77 ± 0.03. In this study, the ratio averaged 0.65
± 0.02, which is close enough to the Firemaster value to suggest that TBB and
TBPH measured in Longyearbyen may be related Firemaster 550 emissions to
the atmosphere.

Figure 4. (A) Concentrations (pg/m3) of OPEs and (B) BFRs and ΣDP in the
atmospheric particle phase at Longyearbyen, Svalbard. The black horizontal
line inside each box represents the median. The boxes represent the 25th and
75th percentiles. Error bars represent 5th and 95th percentiles. Note that the
concentrations scale is 10 times greater for panel A than for panel B. Reprinted
with permission from Salamova et al. (33) Copyright 2014, American Chemical
Society.

117
 ΣPBDE concentrations were ~37% of ΣBFR on average, and ranged from 1.0
to 31 pg/m3. The most abundant PBDE congener was BDE-209, which contributed
24% to ΣPBDE concentrations and was in the 0.1-6.7 pg/m3 concentration range.
The common penta-congeners, BDE-47 and BDE-99, were the second and third
most abundant PBDEs and contributed on average ~15% and ~12% to the ΣPBDE
concentrations. These PBDE concentrations generally agree with those previously
measured at Ny-Ålesund on Svalbard.
DBDPE and BTBPE were detected in most of these samples,but at lower
concentrations (0.04-2.2 pg/m3 and 0.01-0.09 pg/m3, respectively). Among the
bromobenzenes, HBB was detected in all samples with the concentrations ranging
from 0.01 to 1.7 pg/m3. PBEB, pTBX, and PBBz were detected in ~70% of the
samples with average concentrations lower than the HBB concentrations.
Finally, DP was also detected in all of the samples, and ΣDP concentrations
ranged from 0.05 to 5.0 pg/m3. The fractional abundance of anti-DP defined as a
fraction of anti-DP in ΣDP varied from 43-90%, with the mean value of 75 ± 2%,
which is consistent with the previously reported composition of the commercial
DP mixture.
Since OPEs are potential replacements for the discontinued PBDEs, we
compared ΣOPE, total chlorinated OPE (ΣCl-OPEs), and total non-chlorinated
OPE (Σnon-Cl-OPEs) concentrations with ΣBFR concentrations, as well
as with the most abundant BFRs (TBB, TBPH, and ΣPBDEs) measured in
the same samples (see Figure 5A). Overall, ΣOPE, ΣCl-OPE, Σnon-Cl-OPE
concentrations are ~150, 100, and 35 times higher (on average) than the BFR
concentrations, respectively (see Figure 5B). In other words, atmospheric OPE
concentrations measured are 1-2 orders of magnitude higher than corresponding
BFR concentrations, which is consistent with the OPE-BFR ratios found for the
North American Great Lakes basin and oceanic air over the Northern Pacific.
In fact, OPE concentrations measured in this study are 1-2 orders of magnitude
higher than any BFR (specifically, PBDE) concentrations historically measured in
the Arctic atmosphere, even those measured during the active PBDE production
period. Figure 6 shows literature data on PBDE concentrations measured at
various Arctic sites since the 1990s. With the exception of two high values found
at Alert and Tagish in 1994/1995, which were attributed to local waste incineration
sources and here assumed to be outliers, all of the previously measured ΣPBDE
concentrations are within 1-10 pg/m3, while OPE concentrations measured in this
study are generally between 10-1000 pg/m3.

Summary
The results from the Arctic studies and experiences we have discussed
demonstrate how small towns have been used as environmental chemistry
laboratories, where contaminant levels of mercury and organic contaminants,
from combustion, diffuse local emissions, or LRAT, are significantly affecting
environmental quality at the local level. In the case of mercury emissions from
coal combustion, the results show not only the importance of environmental
chemistry, but a significant bit of combustion and pollution control chemistry,
118
which will impress upon students the need to use a very broad approach when
attempting to understand the sources and processes involved in environmental
chemistry. Not all of the experiences, results or processes we have presented are
unique to the Arctic, but the fact that they are found there shows that the Arctic,
while far away in the experiences or even imaginations of most environmental
chemists, is part of the integrated world. The benefit to students is that the
outcomes of these research investigations can be taken anywhere in the world
with a broader understanding of the different processes affecting environmental
chemistry, and that even the remote parts of the world are not off-limits to the
effects of human processes.

Figure 5. (A) Concentrations (pg/m3) of ΣOPEs, Σnon-Cl-OPEs, ΣCl-OPEs,

ΣBFRs, ΣPBDEs, TBB, and TBPH in the atmospheric particle phase at
Longyearbyen, Svalbard. The red line represents the arithmetic mean, and the
black horizontal line inside each box represents the median. The boxes represent
the 25th and 75th percentiles. Error bars represent 5th and 95th percentiles. (B)
Ratios of ΣOPE, Σnon-Cl-OPE, ΣCl-OPE concentrations to ΣBFR, ΣPBDE,
TBB and TBPH concentrations. Reprinted with permission from Salamova et al.
(33) Copyright 2014, American Chemical Society.

119
Figure 6. Atmospheric concentrations (pg/m3) of ΣOPEs (purple, rightmost bar)
in Longyearbyen, Svalbard and historic ΣPBDEs (blue bars; gas phase, the sum
of di- to hepta-PBDE congener concentrations) measured at various Arctic sites
worldwide. See reference (33) for information on literature references of data
shown. Reprinted with permission from Salamova et al. (33) Copyright 2014,
American Chemical Society.

The results that we have presented, while showing examples of the effects
of human activity in the Arctic, are not known to be harmful to organisms in
the environment. The Hg0(g) concentrations are below the no-effect reference
concentrations, and the FRs do not have established reference concentrations in
air. While there are mechanisms producing or moving these toxic substances in
and to Longyearbyen, the immediate risk to the environment is low. However, for
a region with very few if any sources of these contaminants, the need to understand
the fates and effects, and in some cases the sources of these pollutants remains a
challenge for the environmental chemist.

120
 Acknowledgments
The research results reported here include experiences by both authors
as professor (MHH) and student (SLC) at the University Center on Svalbard.
The access to sampling opportunities resulting from courses AT-210 (Arctic
Environmental Pollution) and AT-331 (Arctic Environmental Pollution:
Atmospheric Distribution and Processes) are gratefully acknowledged. The
sampling instrument producing mercury data was supplied by Michelle Nerentorp
Mastromonaco, Chalmers Technical Univeristy, Götborg, Sweden. The section of
this chapter on flame retardants is adapted from Salamova et al. (33)

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31. Danielson, J. A. Air Pollution Control Manual. U.S. Public Health Service,
National Center for Air Pollution Control, 1967.
32. Jutze, G. A.; Foster, K. E. Recommended method for atmospheric sampling
of fine particulate matter by filter media-high-volume sampler. J. Air Pollut.
Control Assoc. 1967, 17, 17–25.
33. Salamova, A.; Hermanson, M. H.; Hites, R. A. Organophosphate and
halogenated flame retardants in atmospheric particles from a European Arctic
site. Environ. Sci. Technol. 2014, 48, 6133–6140, DOI: 10.1021/es500911d.
34. Hermanson, M. H.; Isaksson, E.; Forström, S.; Teixeira, C.; Muir, D. C. G.;
Pohjola, V.; van de Wal, R. Deposition history of brominated flame retardant
compounds to an ice core from Holtedahlfonna, Svalbard, Norway. Environ.
Sci. Technol. 2010, 44, 7405–7410, DOI: 10.1021/es1016608.

123
 Chapter 9

Mapping of Brownfield Properties in the

Detroit Community Using GIS
Alexa Rihana-Abdallah* and Yuncong Pang

Department of Civil &Environmental Engineering,

University of Detroit Mercy, 4001 W. McNichols Road,
Detroit, Michigan 48221, United States
*E-mail: rihanaa@udmercy.edu.

Brownfields are properties left abandoned or underused because

of a perceived contamination problem. They contribute to urban
sprawl, limit economic growth and reduce tax revenue. They
also contribute to environmental degradation and pose potential
risk to public health. For these reasons, brownfields are of
interest as prospective sites for redevelopment. In Detroit, the
motor city of Michigan, decades of industry and manufacturing
plants have left a number of properties contaminated with
organic and inorganic chemicals, heavy metals, and debris
from dilapidated buildings. This work describes a classroom
project in which brownfield sites were identified according to
pollutant types or industrial activities and then mapped using
the Geographic Information System software (GIS). Focusing
primarily on communities in Detroit, students were able to use
GIS to visually locate and map brownfield sites contaminated
with either lead, asbestos, or petroleum products. This work
further motivated them to research remediation teachniques for
potential redevelopment of these sites in their communities.

Introduction
The federal Environmental Protection Agency (EPA) defines brownfields
as “abandoned, idled, or underused industrial and commercial facilities where
expansion or redevelopment is complicated by a real or perceived environmental
contamination” (1). Brownfields differ in many aspects, such as location, size,

© 2018 American Chemical Society

age, past use, and degree of environmental contamination. These factors can pose
obstructions to redevelopment. There are many types of properties classified as
potential brownfields, including abandoned gas stations, landfills, old dry cleaning
operations, and vacant industrial plants. Old and vacuous office buildings, vacant
residential housing, warehouses, and commercial operations also can be classified
as brownfields. Most of these properties may have contaminants such as asbestos,
lead paint, or hazardous chemicals that must be cleaned up when redeveloping the
properties. The EPA estimates that the number of brownfield sites in the United
States exceeds 400,000 (2). This stagrant number stems from several factors
including the decline of the manufacturing industry sector, the passing of more
stringent environmental policies to protect public health and the environment, and
the continued struggle to balance public safety and economic growth. The tension
between motivations to ensure environmental quality and to promote economic
development is mostly noticeable in urban areas hit by the loss of industrial jobs
(3). During the 1970s and 1980s, in order to protect the public from brownfield
contamination, the US Congress passed several acts and the US EPA initiated its
Superfund program designed to list contaminated sites on the National Priority
List (NPL) and fund their cleanup process. This program sparked an interest in
brownfield redevelopment and helped revive economic life in urban communities.

Brownfields in Michigan

Brownfield classification encompasses a wide variety of pollutants and

various degrees of contamination. Students were asked to list industries and
manufacturing operations in Michigan that can be sources of accidental spills
and thus have the potential to produce contaminated sites. A list of industrial
activities was compiled. Then, using the EPA and Department of Environmental
Quality (DEQ) websites, brownfield sites by county were tabulated according to
the different activities and operations conducted on these sites (4–6). Students
then generated a list of typical pollutants expected to arise from the identified
activities. Table 1 displays the number of brownfields per county classified
according to the category of activities. This table is by no means an exhaustive
list of brownfields in Michigan. To better visualize the extent of contaminated
sites in the state, GIS was used to map the brownfields by county. GIS software
is designed to store, display, and analyze geographic and spatial data. GIS stores
data on geographical features and characteristics and allows the user to produce
maps and layer the statistical data on its geographical location. The software
used in this study is ArcGIS 9.3, a tool that helps visualize the data and enhance
users’ understanding of the data for further analysis. Figure 1 shows the number
of brownfields in each county. The colors on the map each are associated with a
range of numbers, with red representing the highest range. As seen in Figure 1,
most of the brownfields in Michigan are concentrated in Wayne County, which
contains the city of Detroit.

126
 Figure 1. Brownfields in Michigan. (see color insert)

Table 1. Brownfields in Michigan by contaminants (4–6)

Typical Activity Typical Contaminants County Number of
Found Brownfields
Oakland 8
Jackson 4
Some metals and metal Macomb 3
Automotive dust; various organic
refinishing and compounds; solvents; paint Wayne 2
repair and paint sludge; scrap
metal; waste oil Ionia 2
Allegan 1
Hillsdale 1
Continued on next page.

127
 Table 1. (Continued). Brownfields in Michigan by contaminants (4–6)
Typical Activity Typical Contaminants County Number of
Found Brownfields
Polynuclear aromatic
Coal gasification Monroe 1
hydrocarbons (PAH)
Volatile organic compounds Wayne 1
(VOCs) such as chloroform
Dry cleaning and tetrachloroethane;
various solvents; spot Ionia 1
removers; fluorocarbon 113
Dioxin; various municipal
Incinerators Wayne 2
and industrial waste
Oakland 4
Metals; VOCs; Monroe 2
polychlorinated biphenyl
(PCB); ammonia; methane; Newaygo 1
Landfills
household products and Macomb 1
cleaners; pesticides;
various wastes Wayne 1
Lenawee 1
Macomb 5
Wayne 2
Oakland 2
Shiawassee 1
Jackson 1
Machine Metals; VOCs; dioxin;
shops/metal beryllium; degreasing Bay 1
fabrication agents; solvents; waste oils
Ionia 1
Kent 1
Hillsdale 1
Lenawee 1
Clinton 1
Kalamazoo 1
Polymers; phthalates;
Plastics
cadmium; solvents; resins; Shiawassee 1
manufacturing
chemical additives; VOCs
Jackson 1
Pharmaceutical Lead; various organic
Wayne 1
manufacturing chemicals; organic solvents
Silver; solvents; acids; Oakland 1
Printing industry waste oils; inks; and dyes;
photographic chemicals Monroe 1
Continued on next page.

128
 Table 1. (Continued). Brownfields in Michigan by contaminants (4–6)
Typical Activity Typical Contaminants County Number of
Found Brownfields
Scrap metal Various metals (such as lead
Oakland 1
operations and nickel); PCBs; dioxin
Wayne 8

Petroleum hydrocarbons; Oakland 3

benzene, toluene, Kalamazoo 2
Petroleum
ethylbenzene, xylene
refining and reuse Shiawassee 1
(BTEX); solvents; fuels;
oil and grease Kent 1
Jackson 1
Various metals such as
Electroplating
cadmium, chromium, Wayne 1
operations
cyanide, copper, nickel

Brownfields in Detroit
The city of Detroit is steeped in history. Its industrial boom erupted in
the early part of the twentieth century with the advent of the automobile. The
automotive industry allowed the city to grow exponentially in a very short period
of time. Production boomed, jobs were abundant, thousands of homes were
built for workers, and the city grew and flourished (7). However, with better
technology, the industry began to replace and refine the workforce. Jobs once
numerous began to wane. Socioeconomic issues came to a head in 1967 when the
great race riots of Detroit raged for five days. Half-burned houses, empty factories,
and vacant land soon peppered the city’s landscape. About 30% of Detroit is now
vacant land, which accounts for about 40 square miles of the city’s total 138.77
square mile area. The city’s population has shrunken from a peak of 2 million in
the early 1950s to 900,000 today (8). With all of these dilapidated buildings and
decaying factories come several environmental problems. When most of these
buildings were erected, environmental regulations, building codes, acceptable
building materials and storage regulations were different from today’s standards.
Before codes, buildings might have been structurally unsafe and unsanitary and
emergency exits might have been inadequate. Building codes were developed
following disastrous situations to address societal concerns about public health
and safety by setting minimum requirements for building design, construction
and operation to protect the public and natural resources. For example,
current constructions must meet seismic design standards, flood-protection
and wind-bracing requirements (9). In earlier construction projects, builders
used asbestos for insulation due to its resistance to heat and fire. Before 1978,
paint and gasoline contained lead. Leaking underground storage tanks (LUST)
threatened to pollute groundwater with lead and gasoline. When improperly

129
utilized or disposed of, asbestos, lead and petroleum compounds present many
environmental challenges that contribute to the formation of browfields.
Primarily used for its natural fire-retardant properties, asbestos was used in
many applications, including insulation for pipes and furnaces, floor and ceiling
tiles, and textured paints. However, anytime asbestos is disturbed by sanding,
remodeling, or demolition, asbestos particles if inhaled can cause asbestosis and
eventually lead to lung cancer and mesothelioma (10). Lead contamination also
poses serious problems, particularly in Detroit. It can be found in houses built
before lead-based paint was banned in 1978, which includes almost 90% of all
low-income Detroit housing (11), and in soil contaminated by air deposition of
lead particles emitted before leaded gasoline was phased out. Digestion of lead
paint chips and inhalation of lead dust can cause lead poisoning (12). Finally,
petroleum contaminantion can arise from modern gasoline stations that use
underground storage tanks (UST) to store fuel products. When gasoline stations
are abandoned due to financial failure, these UST remain buried underneath the
stations and can begin leaking over time. Leakage can be caused by malfunction
or corrosion of the tanks, UST fill manholes, supply pipes, or dispensing pumps
(13). The release of a fuel product can contaminate surrounding soil, groundwater
and even surface water (14). Determining the source, extent and nature of the
release is crucial in containing and cleaning the spill.

Figure 2. Brownfield sites in Detroit. (see color insert)

130
 Since Detroit has the most brownfield sites of all cities in Michigan, the focus
was on locating brownfields contaminated with these three chemicals within the
city limits. From old gas stations to abandoned factories to vacant commercial
properties, these buildings are not only eyesores to the community but also health
hazards to those living near them. A total of 27 properties contaminated with
either lead, asbestos or petroleum chemicals were identified through the help of the
Department of Environmental Affairs for the city of Detroit (15). This department,
in collaboration with the US EPA and Michigan DEQ, formed the Redevelopment
of Urban Sites (REUS) committee to address current and future issues related to
brownfield sites as well as initiatives associated with environmental and economic
redevelopment. The 27 properties then were mapped using GIS; the result is shown
in Figure 2. Finally, students researched EPA recommendations for site cleanup.

Brownfield Remediation
The process of remediating a site contaminated by hazardous substances can
be complicated. Depending on the extent and nature of the contamination, the
remediation process can be costly and time-consuming. The EPA, in conjunction
with the State Response and Brownfield Program Operations Task Force, provides
a 3-step approach to brownfield remediation (16).
Step 1 is a basic assessment of the site, which is a two-phase process. The
first phase is establishing the probability of contamination. The second phase is
determining the planned future use of the site.
Step 2, which establishes which contaminants are actually present, also is a
two-phase process. The first phase requires a survey of the site and a review of all
historical records regarding past use and operations of the site. The second phase
involves collecting and analyzing soil, air and water samples, and estimating the
amount of contaminant and potential effects on public health.
Step 3 is cleaning up the site. The type of clean-up varies widely based on the
type and amount of contamination. Removal and treatment of contaminated soil
and groundwater are the most common approaches.

Conclusions
This paper describes a classroom project that aims to identify certain
industrial operations that cause site contamination in the state of Michigan.
These sites are known as brownfields. Once tabulated by county, these sites
then were mapped using the GIS software. Wayne county, home to the city of
Detroit, had the largest number of brownfields. Students then selected three
contaminants—asbestos, lead and petroleum—that are among the top three most
common contaminants found in Detroit brownfields. Twenty-seven properties in
Detroit were identified as contaminated by asbestos, lead and/or petroleum. The
mapping of the properties by the GIS software was reported in the paper. Locating
brownfields in their communities motivated students to research solutions for site
cleanup. The three steps of brownfield remediation recommended by the EPA
were identified. Overall, brownfield redevelopment poses challenges to major
131
cities like Detroit. Although it carries financial burden, it has enormous potential
to bring environmental, economic, and social benefits to the city.

Acknowledgments
The authors would like to acknowledge the help of the students who put
forth effort and energy into this work. The authors would like to thank Yan J.,
McCutcheon K., and Hancock C. for their contribution and assistance with the
data for this research project.

References
1. U.S. Environmental Protection Agency. Brownfields. https://www.epa.gov/
brownfields (accessed on November 19, 2016)
2. Fischer, T.; Rosenberg, B.; Kchao, V.; Sheahan, J. Detroit Hosts
EPA Brownfields 2008 Conference. http://www.usmayors.org/
usmayornewspaper/documents/05_19_08 (accessed October 11, 2016)
3. Brachman, L. Turning brownfields into community assets: Barriers to
redevelopment. In Recycling the city: The use and reuse of urban land.
Greenstein, R., Sungu-Eryilmaz. Y. Eds; Lincoln Institute of Land Policy:
Cambridge, MA, 2004, 67-88.
4. Michigan Department of Environmental Quality. A MDEQ Report on the:
Environmental Protection Bond Fund Cleanup and Redevelopment Fund
Clean Michigan Initiative Bond Fund. https://www.nrc.gov/docs/ML1126/
ML112620577.pdf (accessed October 1, 2016)
5. Michigan Department of Environmental Quality. Inventory on Facilites.
https://secure1.state.mi.us/facilitiesinventoryqueries/ (accessed October 5,
2016)
6. Contaminated Site Clean-Up Information (CLU-IN). Brownfields. https://
clu-in.org/cihandbook/CIOCpage/brown.htm (accessed on October 8, 2016)
7. Hyde, C. K. Detroit the Dynamic: The Industrial History of
Detroit from Cigars to Cars. https://www.jstor.org/stable/20173894?
seq=1#page_scan_tab_contents (accessed December 10, 2017)
8. Gallagher, J. Acres of Barren Blocks Offer Chance to Reinvent Detroit.
Detroit Free Press. http://www.cityfarmer.info/2008/12/23/acres-of-barren-
blocks-offer-chance-to-reinvent-detroit/ (accessed December 19, 2017)
9. Environmental Energy and Study Institute (EESI): The Value and Impact of
Building Codes http://www.eesi.org/papers/view/the-value-and-impact-of-
building-codes (accessed March 24, 2018)
10. U.S. Environmental Protection Agency. Asbestos. http://www.epa.gov/iaq/
asbestos.html#Sources%20of%20Asbestos (accessed December 21, 2017)
11. Detroit Environmental Agenda. https://detroitenvironmentaljustice.org/wp-
content/uploads/2017/07/DETROIT-ENVIRONMENTAL-AGENDA.pdf
(accessed March 21, 2018)
12. U.S. Environmental Protection Agency. Lead. http://www.epa.gov/lead
(accessed December 21, 2017)
132
13. U.S. Environmental Protection Agency. Underground Storage Tank.
https://www.epa.gov/ust/leaking-underground-storage-tanks-corrective-
action-resources (accessed March 21, 2018)
14. U.S. Environmental Protection Agency. Basic Information on Petroleum
Brownfields. http://www.epa.gov/OUST/petroleumbrownfields/pbbasic.htm
(accessed December 21, 2017)
15. Brownfield Listings: The Redevelopment Marketplace. https://
brownfieldlistings.com/
16. Davis, T. S. Brownfields: A Comprehensive Guide to Redeveloping
Contaminated Property; American Bar Association, 2002; pp 354−356.

133
 Editors’ Biographies
Elizabeth S. Roberts-Kirchhoff
Elizabeth Roberts-Kirchhoff received a B.S. in Chemistry from Texas A & M
University and a Ph.D. in Biological Chemistry from the University of Michigan.
After postdoctoral research at Wayne State University and The University of
Michigan, she joined the faculty at the University of Detroit Mercy in 1997.
Presently, Liz serves as Assistant Dean of Science in the College of Engineering
& Science at the University of Detroit Mercy.
Liz has taught courses in biochemistry, medicinal chemistry, and
environmental toxicology to science majors and general, organic, and
biochemistry to allied health majors. Liz has continued to develop and implement
innovative and evidenced-based teaching pedagogies in the classroom and
laboratory. This has included the development of modules in Process-oriented
Guided Inquiry Learning, the innovative use of technologies in the classroom, and
the implementation of project-based laboratories and course-based undergraduate
research experiences.
Her research focus on the analysis of metals and xenobiotics in food,
consumer products, and the waters of Southeastern Michigan contributes to the
growing body of knowledge about how we impact our environment and how our
environment impacts our health. Liz has interest in the analysis of metals and
xenobiotics including the X-ray fluorescence analysis of metals in food, dietary
supplements, and cosmetics, and the GC-MS and LC-MS analysis of pesticides
and pharmaceutical compounds in southeastern Michigan waterways.

Mark A. Benvenuto
Mark Benvenuto received his education at the Virginia Military Institute and
the University of Virginia (B.S. and Ph.D., respectively) and did a post-doctoral
fellowship at the Pennsylvania State University. He also served a four-year term
of service between his undergraduate and graduate education as a lieutenant in the
United States Army, spent mostly in Mannheim, West Germany.
He joined the University of Detroit Mercy as a faculty member in inorganic
chemistry in 1993 and has been department chair since 2001. Mark has taught
freshman-level chemistry to science and engineering students virtually every
semester since he has been at the University of Detroit Mercy and has been
voted the UDM Science Teacher of the Year by the students five times. He was
also awarded the Michigan College Science Teacher of the Year in 2003 by the
Michigan Science Teachers Association. He has been active in local and national
ACS activities for two decades and is a Class of 2015 ACS Fellow.

© 2018 American Chemical Society

 Mark maintains research interests in two broad areas: coordination chemistry,
specifically the development of multi-dentate ligands with unusual coordinating
abilities, and in the analysis of trace materials in archaeological objects as well
as food supplements and personal care products via energy dispersive X-ray
fluorescence spectrometry.

136
Indexes
 Author Index
Baker, S., 67 Nguyen, G., 81
Benvenuto, M., ix, 81, 89 Pang, Y., 125
Bhagwagar, M., 81 Pothoof, J., 81
Ezeh, V., 57 Rihana-Abdallah, A., 125
Guerard, J., 1 Roberts-Kirchhoff, E., ix, 89
Hayes, S., 1 Stokes, D., 89
Hermanson, M., 105 Thomas, S., 89
Kahl, A., 49 Tinawi, S., 81
Le Cras, S., 105 Woodard, K., 21
Makki, S., 81 Young, L., 21
Ngo, T., 89 Zimmermann, K., 21

139
 Subject Index
A course and project description, 59
discussion, 65
Arctic, environmental chemistry introduction, 57
conclusions, 15 National Emission Inventory, 58f
future work, 14 project implementation, 60
implementation questions at the beginning of project,
distance laboratory experiences, 9 60t
face-to-face or distance format, 7 project results, 61
lab manual and lab kit developed, 10f ammonia concentration, scatter plot
surface water and drinking water after removing the possible outlier
quality, paucity of data, 11 data point, 63f
tentative course schedule, 8t ammonia concentration, scatter plot
introduction for Aug 22nd-Oct 31st 2017, 62f
course-based undergraduate research, ammonia concentration, scatter plot
2 for fall 2017, 62f
distance learning, engagement average ammonia concentration, GIS
challenges, 3 plot, 63f
environmental chemistry, contextually
relevant framework, 2
rationale, 4 C
distance and on-campus modalities,
course, 5f
Community-based undergraduate research
faculty-guided research projects,
experimental methods, 29
theoretical framework, 6f
analyte PAHs, list, 32t
UAF, STEM core courses, 6
deployment characteristics for each
results, 12
site, 34t
course, formative and summative
each site, demographic data, 31t
evaluation, 13
EJSCREEN, 30
USPS, students, 13
non-invasive measures, PAS deployed
Arctic communities, 105
at site C, 33f
air in an arctic town, particle-associated
future goals, 43
flame retardants, 114
interdisciplinary community-based
OPEs, concentrations, 117f
research, influence, 40
atmospheric mercury, 108
EJ-CIP participation, results of student
chemical reduction, process, 113
survey, 42t
Longyearbyen, Daily Hg0(g)
PAH concentration, correlation plots,
concentration cycles, 111f
41f
Longyearbyen, hourly average air
introduction, 22
temperature, 112f
CIP program, 25
meterological variables, 110
employers that rated the described
svalbard map highlighting
skills, percentage, 24f
longyearbyen, 109f
interdisciplinary nature of the project,
introduction, 106
Venn diagram, 29f
summary, 118
interdisciplinary undergraduate
atmospheric concentrations, 120f
research, 26
atmospheric particle phase,
open access institution, experiential
concentrations, 119f
learning, 23
Atmospheric ammonia, trends
student population, demographic
assessment
distribution, 22t
response to survey 2, 64f
student deliverables, 34
survey 2, 64t
conclusion and future directions, 65

141
 annual Georgia Gwinnett College
CREATE Symposium, 37
basic demographic information, 35
presentations and outreach, 36
undergraduates, preliminary data
generated, 38
PAHs, distribution, 40f
standard PAH mixture,
chromatograms, 38f
total PAH concentrations, 39f
Cosmetic mineral eyeshadows, analysis, 89
conclusions, 100
experimental methods, 91
selected elements, detection limits,
92t
introduction, 90
results and discussion, 92
aluminum, potassium and iron,
concentration, 98f
lead, concentrations, 95t
manganese, concentration, 99f
strontium, concentrations, 94t
strontium and rubidium,
concentration, 97f
strontium and rubidium
concentrations, 93
titanium in the makeup samples,
concentration, 99f
XRF, consumer mineral makeup
analyzed, 96t
zinc in the makeup samples,
concentration, 97f
D
Detroit community using GIS, mapping of
brownfield properties
brownfield remediation, 131
conclusions, 131
Detroit, brownfields, 129
brownfield sites, 130f
introduction, 125
Michigan, brownfields, 126
brownfields, 127f
brownfields, contaminants, 127t
142
Duckweed species, using DNA barcoding,
67
instructional perspective and
conclusions, 75
DNA sequencing, technology, 76
introduction, 68
atpF-atpH barcode sequences,
maximum likelihood dendrogram,
75f
DNA extraction protocol, workflow,
70f
duckweed, wild population, 70f
homology search, example BLASTn
output, 74f
PCR conditions, 71
2% agarose, example results, 72f
Sanger sequencing product, four
channel chromatograph, 73f
N
Nitrogen-containing ligands, synthesis of a
novel series
conclusions, 85
experimental section, 84
ligand synthetic data, 84t
metal-ligand complex formation, 85t
introduction, 81
results and discussion, 82
ligand synthesis, general route, 83f
shortest and longest ligand, 83f
R
Remote sensing, undergraduate research
experience, 49
conclusions, 54
discussion, 54
introduction, 50
methods, 51
Coqui sensor on protoboard, 52f
REU experience, 53
Riffle Arduino board, 52f