NC0089087_Permit Modification_20151014

North Carolina Department of Environmental Quality
Pat McCrory Donald R. van der Vaart
Governor Secretary
October 14, 2015
Paul Young, VP Regulatory Affairs
Ergon Asphalt & Emulsions, Inc.
2520 Wilco Boulevard South
Wilson, North Carolina 27893
Subject: Issuance of NPDES Permit Modification
NPDES Permit NCO089087
EAE Wilson
2520 Wilco Boulevard South
Wilson County
Dear Mr. Young:
In response to your Change of Ownership notice and updated application to modify the subject permit
(received October 10, 2014), the Division of Water Resources (the Division or DWR) hereby issues the
subject discharge permit. We issue this permit pursuant to the requirements of North Carolina General
Statute 143-215.1 and the Memorandum of Agreement between North Carolina and the U.S. Environmental
Protection Agency (EPA) dated October 15, 2007 (or as subsequently amended).
Permit Modifications. The Division acknowledges Ergon's request to modify parameters of concern
(POCs) and their respective sampling frequencies (received October 10, 2014). We have further considered
that bulk storage of asphalt product poses less risk of escaping to the natural environment than less viscus
hydrocarbon products such as vehicle fuels. Therefore, we conclude:
• EPA Test Methods 624 (volatile organics) and 625 (semi -volatile organics) are no
longer required, based on data submitted to date.
• Total Suspended Solids (TSS) and Turbidity will remain in the permit, but the
monitoring frequencies are hereby relaxed from Monthly to Quarterly, based on data
submitted to date.
• Whole Effluent Toxicity (WET) testing will continue in the permit but, based on data
submitted to date, monitoring is hereby relaxed from Quarterly to Annually. [Should
any annual test fail, the Permittee shall immediately conduct follow-up testing [see
NOTE, Section A. (2.)] and revert to Quarterly monitoring.
Findings - DWR Site Visit/Inspection 16Apr2015:
1. Ergon facilities appear well run and well maintained.
2. The Division notes site -grading issues for stormwater:
• The ground -surface surrounding the truck -loading rack appears to drain eastward to
the property line. Here, catch -basins connected to sub -surface piping convey
stormwater southward, to include offsite drainage from adjacent neighbors east. DWR
suspects that this conveyance bypasses Ergon's stormwater-collection pond, thus
discharging offsite potentially impacted, untreated stormwater.
1617 Mail Service Center, Raleigh, North Carolina 27699-1617
Location: 512 N. Salisbury St. Raleigh, North Carolina 27604
Phone: [phone] FAX: [phone] Customer Service: 1-877-623-6748
Internet: www.newaterquality.org
An Equal Opportunity 1 Affirmative Action Employer

• DWR recommends that the Permittee re -grade and/or berm the truck -loading area to
confine or otherwise contain runoff onsite for treatment afforded by the pond.
2. Draining from the adjacent property west, DWR observed a storm -drain (?) outlet
inappropriately capped with a "trash -can lid" (?); this outlet apparently draining to Ergon's
onsite pond. DWR questions what impact this discharge may have on the permittee's
final -discharge compliance.
3. Site inspectors noted a temporarily effluent bypass of boiler blowdown installed to
facilitate sump -pump maintenance. DWR recommends that Ergon adopt new
facilities and/or a pollution prevention plan to prevent future effluent bypasses - a
permit violation.
Electronic Discharge Monitoring Reports (eDMR). Please be advised that the Division will implement an
electronic Discharge Monitoring Report (eDMR) program in accord with pending requirements by the
Environmental Protection Agency (EPA). We have included the details required to implement the eDMR
program in this permit [see Special Condition A. (4)].
Proposed federal regulations require electronic submittal of all DMRs and specify that, if North Carolina
does not establish a program to receive such submittals, Permittees must then submit eDMRs directly to
EPA. For information on eDMRs, registering for eDMR submittal, and obtaining an eDMR user account,
please visit our webpage: http•//portal ncdenr ore/web/wo/admin/bo ipu/edmr
For information on EPA's proposed NPDES Electronic Reporting Rule, please visit EPA's website:
If any parts, measurement frequencies or sampling requirements contained in this permit are unacceptable,
you have the right to an adjudicatory hearing upon written request submitted within thirty (30) days
following receipt of this letter. This request must take the form of a written petition, conforming to Chapter
I SOB of the North Carolina General Statutes, and filed with the Office of Administrative Hearings (6714
Mail Service Center, Raleigh, North Carolina 27699-6714). Unless such demand is made, this decision
shall be final and binding.
Please note that this permit is not transferable except after notice to the Division. The Division may modify,
revoke, and/or reissue this permit. This permit does not affect your legal obligation to obtain other permits
required by the Division of Water Resources, the Division of Land Resources, the Coastal Area
Management Act, or any other Federal or Local governmental permit.
If you have any questions, please contact Joe R.
duect line [phone].
cer y,
C
S. Jay Zimmerman, .G., Dir to
Division of Water Resources
L.G. at [e-mail]] or call his
Enclosure: NPDES Permit NC0089087 (modification issuance final)
he: RRO/SWPS Supervisor, Danny Smith
Central Files
NPDES Program Files
ec: RRO/SWPS Supervisor, Danny Smith
Aquatic Toxicity Branch (ATB), Atm. Susan Meadows
EAE, Inc., Austin Moody, Environmental Engineer [[e-mail]

Permit NC00089087
STATE OF NORTH CAROLINA
DEPARTMENT OF ENVIRONMENTAL QUALITY
DIVISION OF WATER RESOURCES
PERMIT
TO DISCHARGE WASTEWATER UNDER THE
NATIONAL POLLUTANT DISCHARGE ELIMINATION SYSTEM
(NPDES-)
In compliance with the provisions of North Carolina General Statute 143-215.1, other lawful standards
and regulations promulgated and adopted by the North Carolina Environmental Management
Commission, and the Federal Water Pollution Control Act, as amended,
Ergon Asphalt & Emulsions, Inc.
is hereby authorized to discharge wastewater from outfalls located at the
EAE -Wilson
2520 Wilco Boulevard
Wilson County
to receiving waters designated as an unnamed tributary to Contentnea Creek in the Neuse River Basin in
accordance with effluent limitations, monitoring requirements, and other conditions set forth in Parts 1,
H, III and IV hereof.
This permit shall become effective November 1, 2015.
This permit and authorization to discharge shall expire at midnight on June 3 012018.
Signed this day October 14, 2015.
S. ��immerman, P.G., Director•-' _,
Division of Water Resources
By Authority of the Environmental Management Commission
Page 1

Permit NC00089087
..
SUPPLEMENT TO PERMIT COVER SHEET
All previous NPDES Permits issued to this facility, whether for operation or discharge are hereby
revoked, and as of this issuance, any previously issued permit bearing this number is no longer effective.
Therefore, the exclusive authority to operate and discharge from this facility arises under the permit
conditions, requirements, terms, and provisions described herein.
Ergon Asphalt & Emulsions, Inc.
is hereby authorized to:
1. continue operating Surface -Water Pollution -Prevention facilities for stormwater and related
wastewater runoff(s) servicing distribution of petroleum hydrocarbons contained as surface bulk -
storage in excess of one (1) million gallons utilizing;
• railroad offloading facilities for liquid asphalt with spill -prevention
secondary containment
• above -ground storage tanks (ASTs), heated
• truck -loading rack with spill -prevention secondary containment
• pond (stormwater-.retention);
• 8-inch diameter discharge line with discharge valve, manually -operated,
lockable - normally closed
• effluent surface-spreader/diffuser
• sample point, up gradient of vegetative filter
located at the EAE - Wilson, 2520 Wilco Boulevard, Wilson, Wilson County, and
2. discharge from said treatment works via Outfall 001, at the location specified on the attached
map, into an unnamed tributary (UT) to Contentnea Creek [stream segment 27-86-(7)], a
waterbody currently classified C; SW; NSW within Subbasin 03-04-07 [HUC: 03020203] of
the Neuse River Basin.
Page 2

Permit N000089087
PART I
A. (1.) EFFLUENT LIMITATIONS AND MONITORING REQUIREMENTS
[15A NCAC 02B .0400 et seq.; 02B .0500 et seq.]
Beginning on the effective date of the permit and lasting until expiration, the Permittee is authorized to
discharge from Outfall 001. Such discharges shall be limited, monitored and reported 1 by the
Permittee as specified below:
EFFLUENT CHARACTERISTICS
[PARAMETER CODE]
, LIMITS
.: .
MONITORING RE UIREMENTS .1
Monthly
Average
Daily
Maximum
Measurement
Frequency
Sample
a
Sample
Location
Flow 2
50050
Episodic
2
Effluent
Total Suspended Solids 3
C0530
30.0 mg/L
45.0 mg/L
Quarterly
Grab
Effluent
Turbidity 3
00076
50 NTU
Quarterly
Grab
Effluent
pH (standard units) 3
00400
Not < 6.0 of > 9.0
Quarterly
Grab
Effluent
Oil & Grease 3
EPA 1664 [STG-HEM]
00556
Quarterly
Grab
Effluent
WET Acute Toxicity 4.
TAE6C
Annually 4
Grab
Effluent
Footnotes:
1. No later than 270 days from the permit effective date, begin submitting discharge Monitoring Reports electronically
using NCDWR's eDMR application system. See. Special Conditions A. (4.)
2. Flow shall be monitored with each discharge event. During periods of no discharge, the Permittee shall submit a monthly
Discharge Monitoring Report (DMR) indicating "No flow/No discharge." Flow may be monitored using any one of the
following methods:
a. measure flow continuously;
b. calculate flow based on total rainfall per unit area draining to the outfall [see Rational
Equation, Section A. (3)];
c. estimate flow at 20-minute intervals during the entire discharge event; or
d. report flow based on discharge pump logs.
3. This sample shall be collected concurrently with WET -test sampling.
4. WET Testing: The Permittee shall perform Annual Whole Effluent Toxicity (WET) testing; Acute Pass/Fail @ 90%
(Fathead Minnow, 24-hour static test), January, April, July, and October [see Section A. (2.)]. The Permittee has been
granted provisional Annual testing based on compliance. If any annual WET test should "fail" [LG-50 < 100%], the
Permittee shall immediately conduct follow-up testing [see NOTE, Section A. (2.)] and revert to Quarterly WET testing.
After five (5) consecutive Quarterly WET -test events showing "Pass" [LG-50 = 100%], the Permittee may petition the
Division to reevaluate the monitoring frequency, as data may warrant.
Conditions:
• The Permittee shall discharge no floating solids or foam.
• The Permittee shall discharge no tank solids, no tank bottom -water, no tank rag layer
• Following hydrostatic tank testing, the Permittee shall discharge no tank (or pipe) contents unless the benzene
concentration test less than 1.19µg/L and the toluene concentration test less than 11 µg/L.
Page 3

Permit NC00089087
A. (2.) ACUTE TOXICITY MONITORING - LIMITED (Annually)
[15A NCAC 02B .0200 et seq.]
The Permittee shall conduct acute toxicity tests Annually [Except reverting to Quartedy upon failure to
pass provisional Annual WET -testing], using protocols defined in the North Carolina Procedure Document
entitled "Pass/Fail Methodology For Determining Acute Toxicity In A Single Effluent Concentration"
(Revised -July, 1992 or subsequent versions). The monitoring shall be performed using a Fathead
Minnow (Pimephales promelas), 24-hour static test. The effluent concentration at which there may be at
no time significant acute mortality is 90% (defined as treatment two in the procedure document).
Effluent samples for self -monitoring purposes must be obtained during representative effluent discharge
below all waste treatment. The tests will be performed during the months of January, April, July, and
October.
The parameter code for Pimephales promelas is TGE6C. All toxicity testing results required as part of
this permit condition will be entered on the Effluent Discharge Form (MR-1) for the month in which it
was performed, using the appropriate parameter code. Additionally, DWR Form AT-2 (original) is to be
sent to the following address:
Attention: North Carolina Division of Water Resources
Environmental Sciences Section
1621 Mail Service Center
Raleigh, N.C. 27699-1621
Completed Aquatic Toxicity Test Forms shall be filed with the Environmental Sciences Section no later
than 30 days after the end of the reporting period for which the report is made.
Test data shall be complete and accurate and include all supporting chemical/physical measurements
performed in association with the toxicity tests, as well as all dose/response data. Total residual chlorine
of the effluent toxicity sample must be measured and reported if chlorine is employed for disinfection of
the waste stream.
Should there be no discharge of flow from the facility during any month, the Permittee will complete the
information located at the top of the aquatic toxicity (AT) test form indicating the facility name, permit
number, pipe number, county, and the month/year of the report with'the notation of "No Flow" in the
comment area of the form. The report shall be submitted to the Environmental Sciences Section at the
address cited above.
Should any test data from either these monitoring requirements or tests performed by the North Carolina
Division of Water Resources indicate potential impacts to the receiving stream, this permit may be re-
opened and modified to include alternate monitoring requirements or limits.
If the Permittee monitors any pollutant more frequently than required by this permit, the results of such
monitoring shall be included in the calculation & reporting of the data submitted on the DMR & all AT
Form submitted.
NOTE: Failure to achieve test conditions as specified in the cited document, such as minimum control
organism survival and appropriate environmental controls, shall constitute an invalid test and will
require immediate follow-up testing to be completed no later than the last day of the month following the
month of the initial monitoring.
Page 4

Permit NC00089087
A. (3.) RATIONAL EQUASION - FOR CALCULATING FLOW
[G.S. 143-215.3(a)(2)]
The Rational Equation is one method for calculating runoff; find references and information in DWR's
Stormwater BMP Manual, Chapter 3, "Stormwater Calculations," by addressing the following website:
http://i)ortal.NCDEQ.orp-/web/wo/ws/su/bmp-manual
The Rational Equation: Q=KuCIA, where:
Q = flow (peak flow rate (cfs or m3/sec)
Ku = units conversation factor =1.008 for U.S. standard units (usually ignored because
it is so close to 1), or 0.278 for SI units
C = dimensionless runoff coefficient for the watershed, loosely defined as the ratio of
runoff to rainfall
I = intensity of rainfall taken from the intensity -duration -frequency curves for the
specified design return period at the time of concentration, tc (in/h or mm/h). tc =
time of concentration (time after the beginning of rainfall excess when all portions
of the drainage basin are contributing simultaneously to flow at the outlet).
A = area of tributary watershed (acres or km2)
The rational equation is used to calculate the runoff from a region, given:
• runoff coefficient which accounts for infiltration and other potential losses in
the region, .
• rainfall intensity to the region,
• time it takes for runoff to travel from the region's upper reaches to its outlet,
and
• region's drainage area.
A. (4.) ELECTRONIC REPORTING - DISCHARGE MONITORING REPORTS
[G.S. 143-215.3(a)(2)]; [G.S. 143-215.66]
Proposed federal regulations require electronic submittal of all discharge monitoring reports (DMRs)
and specify that, if a state does not establish a system to receive such submittals, then Permittees must
submit DMRs electronically to the Environmental Protection Agency (EPA). The Division adopted and
implement these regulations in 2013.
NOTE: This special condition supplements or supersedes the following sections within Part II of this
permit (Standard Conditions for NPDES Permits):
• Section B. (11.) Signatory Requirements
• Section D. (2.)
• Section D. (6.)
• Section E. (5.)
Reporting
Records Retention
Monitoring Reports
Page 5

Permit NC00089087
Ir
1. Reporting (Supersedes Part II, Section D. (2.) and Section E. (5.) (a)1
Beginning no later than 270 days from the permit effective date, the Permittee shall report discharge
monitoring data electronically using the NC DWR's Electronic Discharge Monitoring Report
(eDMR) internet application.
Monitoring results obtained during the previous month(s) shall be summarized for each month and
submitted electronically using eDMR. The eDMR system allows permitted facilities to enter
monitoring -data and submit DMRs electronically using the internet. Until such time that the state's
eDMR application is compliant with EPA's Cross -Media Electronic Reporting Regulation
(CROMERR), Permittees will be required to submit all discharge monitoring data to the state
electronically using eDMR and will be required to complete the eDMR submission by printing,
signing, and submitting one signed original and a copy of the computer printed eDMR to the
following address:
NCDEQ / DWR / Information Processing Unit
ATTENTION: Central Files / eDMR
1617 Mail Service Center
Raleigh, North Carolina 27699-1617
If a Permittee is unable to use the eDMR system due to a demonstrated hardship or due to the facility
being physically located in an area where less than 10 percent of the households have broadband
access, then a temporary waiver from the NPDES electronic reporting requirements may be granted
and discharge monitoring data may be submitted on paper DMR forms (MR 1, 1. 1, 2, 3) or
alternative forms approved by the Director. Duplicate signed copies shall be submitted to the
mailing address above.
Requests for temporary waivers from the NPDES electronic reporting requirements must be
submitted in writing to the Division for written approval at least sixty (60) days prior to the date the
facility would be required under this permit to begin using eDMR. Temporary waivers shall be valid
for twelve (12) months and shall thereupon expire. At such time, DMRs shall be submitted
electronically to the Division unless the Permittee re -applies for and is granted a new temporary
waiver by the Division. -
Information on eDMR and application for a temporary waiver from the NPDES electronic reporting
requirements is found on the following web page:
http://portal.NCDEO.org/web/wq/admin/bog/ipu/edmr
Regardless of the submission method, the first DMR is due on the last day of the month following
the issuance of the permit or in the case of a new facility, on the last day of the month following the
commencement of discharge.
2. Signatory Requirements [Supplements Part II, Section B. (11.) (b) and supersedes Section B. (11.)
All eDMRs submitted to the permit issuing authority shall be signed by a person described in Part 11,
Section B. (I 1.)(a) or by a duly authorized representative of that person as described in Part H,
Section B. (11.)(b). A person, and not a position, must be delegated signatory authority for eDMR
reporting purposes.
Page 6

Permit NC00089087
For eDMR submissions, the person signing and submitting the DMR must obtain an eDMR user
account and login credentials to access the eDMR system. For more information on North
Carolina's eDMR system, registering for eDMR and obtaining an eDMR user account, please visit
the following web page:
http://portal.NCDEO.or web/wq/admin/boa/ipu/edmr
Certification. Any person submitting an electronic DMR using the state's eDMR system shall make the
following certification E40 CFR 122.221. NO OTHER STATEMENTS OF CERTIFICATION WILL
BE ACCEPTED:
"I certify, under penalty of law, that this document and all attachments were prepared under my
direction or supervision in accordance with a system designed to assure that qualified personnel
properly gather and evaluate the information submitted. Based on my inquiry of the person or
persons who manage the system, or those persons directly responsible for gathering the information,
the information submitted is, to the best of my knowledge and belief, true, accurate, and complete. I
am aware that there are significant penalties for submitting false information, including the
possibility of fines and imprisonment for knowing violations. "
I Records Retention [Supplements Part H, Section D. (Q]
The Permittee shall retain records of all Discharge Monitoring Reports, including eDMR submissions. These
records or copies shall be maintained for a period of at least 3 years from the date of the report. This period
may be extended by request of the Director at any time [40 CFR 122.41].
Page 7

11 US Hwy 301 7-
-IF
Approximate Property
6b
Boundary
X
Coon
tN
NAMOn Wild P
•
M.4
7
01
C
U'r to Contentnea Creek
Outfall 001
(flows South)
(flows south)
\4
09
Contentnea Creek
(flows cast)
P
Ergon Asphalt & Emulsions, Inc.
EAE-Wilson, 2520 Wilco Boulevard S., Wilson
State Grid/ USGS Quad: E27NW/Wilson, NC BUC:0302020307
Latitude: N35041'19" Drainage Basin: Keuse River Basin
Longitude: W77055'02" Receiving Stream: UTtoContentneaCreek (27-86-(7)]
Sub -Basin: 03-04-07 Stream Class: C; SW; NSW
Facility
Location
(not to scale)
NPDES Permit NCO089087
North Wilson County

an Site I tannery reclines • Pool • Fileess Center • Playground
Conveniently Located • Z, 2 & 3 Bedrooms
Appliances Furnished
Washer/DryerHookups
NelvlyRenrodeled AparhaenlsAvaiteble
1706•B Vineyard Dr.
Wilson, NC
py 252-291-2035 or visit us on the web:
Q T o w N n o u r s tirsteasternrentals.com
IMMEDIATE OPENINGS
For
Experienced Body Shop Technicians
Truck Part Counter Person
White's international Trucks
WStson, NO
Goldsboro, NO
New Bern, NC

r! ErgonAsphalt
y & Emulsions, Inc.
a company that works,
CERTIFIED MAIL 7008 1830 0000 5250 4144
July 28, 2015
Mr. Joe Corporon
North Carolina Department of Environmental and Natural Resources
Department of Water Resources
NPDES
RE: ErgonAsphalt&Emulsions —Wilson, NC (NCO089087)
Response to Draft NPDES Permit
Dear Mr. Corporon:
Ergon, Inc.
P.O. Box 1639
Jackson, MS
392154639 USA
601-9333000
ergon.com
RECEIVEDIDENROWR
AUG 0 2015
Water Quality
Permitting Section
Ergon Asphalt & Emulsions— Wilson, NC received the NPDES draft permit on July 9, 2C15. We are
submitting the following comments:
1. TSS and Turbidity will remain in the permit, but the monitoring frequencies are hereby relaxed
from Monthly to Quarterly, based on data submitted to date.
While the frequency of monitoring is being relaxed, we noticed that a TSS monthly average limit
was added to the permit. Please provide the justification for the addition of tits limit.
2. Based on data submitted to date, WET testing is being relaxed from q er to annually.
i
Per Part I.A.(1.) Footnote 4. of the current NPDES permit, "After five c i ous quarterly WET -
test events showing "Pass", the permittee may petition the division to reevaluate the
monitoring frequency". On April 21, 2015, the NCDENR notified Sean Randall of EAE — Wilson
that based on the results of the previous five WET -tests, there was no need tc collect additional
WET test data. The correspondence is being attached to this letter. Since the facility is currently
not subject to WET testing, we feel that requiring annual WET testing would be placing more
stringency on the facility rather than relaxing the requirement.
3. The frequency of DMR submittals is not indicated in the draft permit or rationale. Please
provide this information, as it is not clear since monitoring frequencies have been relaxed.
If you have any questions please contact me at [phone].

Sincerely,
Ergon Asphalt & Emulsions, Inc.
/ �� Crd�zj
Katelan Crain
Environmental Engineer
Office: 601-933-3122
Fax: [phone]
Mobile: [phone]
[e-mail]
Enclosures
CC: Sean Randall, EAE —Wilson
Steve Clark, EAE
File (220-E-02-14- )

Katelan Crain
From: Sean Randall
Sent: Tuesday, April 21, 2015 11:59 AM
To: Austin Moody; Katelan Crain
Subject: FW: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit
fyi
From: Corporon, Joe rmailto:ioe.corooron(c ncdenr.aov
Sent: Tuesday, April 21, 2015 12:15 PM AUG 1 U &k)
To: Sean Randall
Cc: Hennessy, John; Zhang, Cheng Water Quality
Subject: RE: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit Permitting Sectior
Thanks, Sean — received; by the way, I notice all five (5) quarterly tests indicate "pass," with the latest sample collected
April 7, 2015. Therefore, no need to collect additional WET test data discussed during our site visit.
Respectfully,
Joe R Corporon, L.G.
Compliance and Expedited Permitting
DWR
Division of Water Resources
NCDENR/ NPDES Program / Water Quality Permitting Section
919-807-6394; FAX [phone]
E-mail correspondence to and from this address may be subject to the North Carolina Public Records Law and may be disclosed to
third parties.
From: Sean Randall [mailto:Sean.Randall(cbergon.coml
Sent: Tuesday, April 21, 2015 12:04 PM
To: Corporon, Joe
Cc: Austin Moody; Katelan Crain
Subject: RE: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit
Files are attached this time.
From: Sean Randall
Sent: Tuesday, April 21, 2015 12:03 PM
To: 'Corporon, Joe'
Subject: RE: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit
sorry, I will resend.
From: Corporon, Joe rmailto:ioe.corporon(ancdenr.00v]
Sent: Tuesday, April 21, 2015 12:02 PM

To: Sean Randall
Subject: RE: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit
Sean — I don't find the files. Did you forget to attach?
Try again.
Respectfully,
Joe R. Corporon, L. G.
Compliance and Expedited Permitting
DWR
W.Uhsc4UmetRssa:mt Division of Water Resources
NCDENR/ NPDES Program / Water Quality Permitting Section
919-807-6394; FAX [phone]
E-mail correspondence to and from this address may be subject to the North Carolina Public Records Law and may be disclosed to
third parties.
From: Sean Randall [mailto:Sean. [e-mail]]
Sent: Tuesday, April 21, 2015 11:59 AM
To: Corporon, Joe
Cc: Austin Moody; Katelan Crain
Subject: RE: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit
Mr. Corporon,
Attached are Ergon A&E Wilson Toxicity Reports for January 2014 thru January 2015. We appreciate your help in this
process.
Sean Randall
252-991-4692 office
580-583-6618 cell
From: Corporon, Joe fmailto:[e-mail]]
Sent: Monday, April 20, 2015 7:48 AM
To: Sean Randall
Cc: Hennessy, John; Pickle, Ken; Zhang, Cheng; Smith, Danny; Bennett, Bradley; Austin Moodv; Bob Walley
Subject: NCO089087 Ergon Asphalt and Emulsions, Inc. - Site Visit
Mr. Sean Randall:
Sean, thanks again for the tour of your facility last Thursday. I enjoyed meeting with you and your dedicated crew. DWR
will soon provide feedback on your existing site conditions, and make its decision on your permit application(s). I look
forward to receiving your make-up Whole Effluent Toxicity (WET) test results in accord with your existing permit (and
any past results that may not have been submitted).
I will copy the home office and you on all future correspondence. Thanks also for your continued patience with our
backlogged permit -review process.
Respectfully,

. 4,
Corporon, Joe
From: Pickle, Ken
Sent: Thursday, April 16, 2015 5:09 PM
To: Corporon, Joe
Cc: Bennett, Bradley, Georgoulias, Bethany; Hennessy, John; Riddle, Rick L
Subject: Ergon Asphalt plant, Wilson
Hi Joe,
• First, most important: So far, I concur that there is no need here for a stormwater permit; the NPDES
wastewater permit can suffice. We are open to re-evaluating this if you think differently, or if we have
overlooked any aspect. It might be good to meet briefly to be sure we are all seeing the some thing. Just let
me know.
This opinion based on 40 CFR 443.11(c) Effluent Limitations Guidelines... Asphalt Emulsion Subcategory
provision that, "The term process wastewater pollutants shall mean any pollutants present in the process
wastewaters and rainwater runoff." My underlining. So, it looks like we have a basis to conclude that
the efficient bureaucratic approach here is to have just the one permit, the wastewater permit
As I reported earlier today, in the NPDES stormwater program we are using a narrower FOG test at sites where
we think the pollutants are likely to be exclusively derived from petroleum. Our new test is: Non polar oil and
grease by EPA Method 1664 (SGT-HEM) with a new stormwater benchmark of 15 mg/L. SGT HEM means'silica
gel transfer - hexane extraction method', I believe. As I understand it, it's important to qualify the Method with
the 'SGT HEM' to be sure that we are getting the narrower method.
The Stormwater Permitting Program went through an evolution over recent years in getting from 'O&G'to'TPH'
to 'Non -polar Oil and Grease by EPA Method 1664 (SGT-HEM)'. 'TPH' turned out to be confusing, and we are
removing it from all permits as they come up for renewal. As you are editing your own internal guidance on bulk
terminal NPDES permitting, we would suggest you learn from our experience, and just skip the confusing step of
'TPH'.
On the other hand, at sites where animal and vegetable fats, oils, and greases might also be present we are
continuing to use the previous O&G test with a stormwater benchmark of 30 mg/L. Bethany led our thinking on
these revisions a few years ago, and can perhaps advise further if you want to discuss. Either she or I would also
be a good one to review your revised guidance on Bulk Terminal permitting to be sure we are coordinated.
As we also discussed, I'm available for a quick review of your Ergon DRAFT NPDES wastewater permit renewal
when it's ready. Thanks for asking me.
Now, as to sharine my observations this mornine at Ereon:
o On -site staff confirmed the unpermitted discharge of boiler blowdown on an infrequent, or maybe just
once, maintenance problem basis within the last couple of days. Usually this flow goes to the city sewer,
but apparently not when the line backs up or the pump fails. Not a permitted flow, and so you may
consider amending the renewed permit to include this flow. As far as Chang and RRO, this is a permit
violation, and it's their call as to an NOV. But to my eye this falls in the "No harm, no foul, please don't
do it again' category, presuming that it has indeed been an infrequent occurrence of small magnitude.
We identified a previously unrecorded underground pipe entering the drainage piping from the property
to the east. Nearest development appeared to be a loading dock at a building —500' east of the
site. The connection was a surprise to the new Terminal Manager, Sean Randall. Upstream origin of the
pipe is unknown. Sean advised he would be trying to find out about this pipe.

o We identified a previously unrecorded underground pipe entering the western -most drainage ditch,
apparently from the Cargill dog food factory bordering on the west. By my observation the standing
water in the drainage ditch had a brownish color not observed anywhere else on site. Approximately
10" diameter pipe was sealed with duct tape, or similar tape, where it was exposed above the ditch:
probably not an effective seal; suspected source of brownish water in the ditch.
o Drainage from the eastern —15% (?) of the site bypasses the runoff pond. Thomas Dawson, lead
operator, reports taking the permit samples at a location that captures the pond discharge, but does not
include this flow. Sampling —60' further downstream would capture this flow, but would also capture
any flow from the mystery pipe from the east, previously mentioned above.
o Noted that three compressed air aerators were operating in the pond, as evidenced by surface
turbulence, and as confirmed by T. Dawson. Stated purpose of the aerators was to keep the grass carp
alive in the pond by providing DO to this typically stagnant pond. Light green color observed in the
pond, of unknown origin, possibly not indicative of anything special.
o One apparently blind sump between the two rail spur lines. If site personnel were familiar with the
purpose or function of this sump, I did not hear that explanation.
o Very nice level spreader on the discharge from the pond.
o Pretty good looking site, over all.
Let me know if I can help with confirming other observations on site.
114m,
Ken Pickle
Stormwater Program Specialist
NCDENR I DEMLR I Stormwater Permitting Program
1612 Mail Service Center, Raleigh, NC 27699-1612
512 N. Salisbury St, Raleigh, NC 27604
Phone: [phone]
Fax: [phone]
Email: ken. Pickle @ncdenr.00v
Website:—i)://oortal.ncdenr.org/web/Irlstormwater
** Email correspondence to and from this address is subject to the North Carolina Public Records Law and may be
disclosed to third parties unless the content is exempt by statute or other regulations.**

eCFR— Code of Federal Regulations http://www.ecfr.gov/cgi-bin/text-idx?SID=9d79b98d56b2d7ea12d5...
ELECTRONIC CODE OF FEDERAL REGULATIONS
e-CFR Data is current as of February 2, 2016
Title 40 —. Chapter I , Subchapter N Part 443 , Subpart A
Title 40: Protection of Environment
PART 443—EFFLUENT LIMITATIONS GUIDELINES FOR EXISTING SOURCES AND STANDARDS
OF PERFORMANCE AND PRE-TREAT-MENT STANDARDS FOR NEW SOURCES FOR THE
PAVING AND ROOFING MATERIALS (TARS AND ASPHALT) POINT SOURCE CATEGORY
Subpart A —Asphalt Emulsion Subcategory
Contents
§443.10 Applicability; description of the asphalt emulsion subcategory.
§443.11 Specialized definitions.
§443.12 Effluent limitations guidelines representing the degree of effluent reduction attainable by the
application of the best practicable control technology currently available.
§443.13 Effluent limitations guidelines representing the degree of effluent reduction attainable by the
application of the best available technology economically achievable.
§443.14 [Reserved]
§443.15 Standards of performance for new sources.
§443.16 Pretreatment standards for new sources.
t Back to Top
§443.10 Applicability; description of the asphalt emulsion subcategory.
The provisions of this subpart are applicable to discharges resulting from the production of asphalt
paving and roofing emulsions.
It Back to Top
§443.11 Specialized definitions.
For the purpose of this subpart:
(a) Except as provided below, the general definitions, abbreviations and methods of analysis set
forth in part 401 of this chapter shall apply to this subpart.
(b) The term "production area size" shall mean that area in which the oxidation towers, loading
facilities, and all buildings that house product processes we located. _
(c) The term "process wastewater pollutants" shall mean any pollutants present in the process \
wastewaters and rainwater runoff. %/ 1
t Back to Top
§443A2 Effluent limitations guidelines representing the degree of effluent reduction attainable
by the application of the best practicable control technology currently available.
Except as provided in §§125.30 through 125.32, any existing point source subject to this subpart
shall achieve the following effluent limitations representing the degree of effluent reduction attainable
by the application of the best practicable control technology currently available (BPT):
Effluent
characteristic
Effluent limitations
Maximum for any 1
day
Average of daily values for 30 consecutive days shall
not exceed—
Metric units (kg/cu m of runoff)
Oil and grease
0.020
0.015
pH
0)
(1)
English units (lb/1,000 gal of runoff)
Oil and grease
0.167
0.125
PH
0)
(t)
'Within the range 6.0 to 9.0.
1 of 3 2/4/2015 1:54 PM

eCFR — Code of Federal Regulations
http://www.ecfr.gov/cgi-bin/text-idx?SID=9d79b98d56b2d7ea l2d5...
[40 FIR 31191, July 24, 1975, as amended at 60 FIR 33969, June 29, 1995]
t Back to Top
§443.13 Effluent limitations guidelines representing the degree of effluent reduction attainable
by the application of the best available technology economically achievable.
The following limitations establish the quantity or quality of pollutants or pollutant properties,
controlled by this section, which may be discharged by a point source subject to the provisions of this
subpart after application of the best available technology economically achievable:
Effluent
characteristic
Effluent limitations
Maximum for any 1
day
Average of daily values for 30 consecutive days shall
not exceed—
Metric units (kg/cu m of runoff)
TSS
0.023
0.015
Oil and grease
0.015
0.010
pH
0)
(1)
English units (lb/1,000 gal of runoff)
TSS
0.188
0.125
Oil and grease
0.125
0.083
PH
M
(1)
lWithin the range 6.0 to 9.0.
t Back to Top
§443.14 [Reserved]
t Back to Top
§443.15 Standards of performancefor new sources.
The following standards of performance establish the quantity or quality of pollutants or pollutant
properties, controlled by this section, which may be discharged by a new source subject to the
provisions of this subpart:
Effluent
characteristic
Effluent limitations
Maximum for any 1
day
Average of daily values for 30 consecutive days shall
notexceed—
Metric units (kg/cu m of runoff)
TSS
0.0231
0.015
Oil and grease
0.0151
0.010
pH
(1)
0)
English units (lb/1,000 gal of runoff)
TSS
0.188
0.125
Oil and grease
1 0.1251
0.083
pH
I (1)
(1)
'Within the range 6.0 to 9.0.
t Back to Top
§443.16 Pretreatment standards for new sources.
Any new source subject to this subpart that introduces process wastewater pollutants into a
publicly owned treatment works must comply with 40 CFR part 403. In addition, the following
pretreatment standard establishes the quantity or quality of pollutants or pollutant properties controlled
by this section which may be discharged to a publicly owned treatment works by a new source subject
to the provisions of this subpart:
Pollutant or pollutant property
Pretreatment standard
BODs-
No limitation.
TSS
Do.
pH
Do.
Oil and grease
100 mgll.
[40 FIR 31191, July 24, 1975, as amended at 60 FIR 33969, June 29, 19951
2 of 3 2/4/2015 1:54 PM

1 Michael F. Easley
i Governor
r William G. Ross, Jr_ Secretary
-i North Carolina Department of Environment and Natural Resources
"�11 Alan W. Klimek, Director
Division of Water Quality
February 27, 2007
Pamela F. Faggert, /
Vice President and Chief Environmental Officer 7
Dominion
Glen Dominion Boulevard
Glen Allen, Virginia 23060 .q-V
Subject: Your Request to Rescind NPDES
Permit NCO079014
Rosemary Power Station
Roanoke Rapids, North Carolina
Halifax County
Dear Ms. Faggert:
The Division of Water Quality (the Division) has received and reviewed your letter dated December 20,
2006. We acknowledge your request to rescind both your permits for the subject site, one for a point
source discharge (NC0079014), and one for non -point -source stormwater (NCS000197).
The Point Source Branch hereby addresses only your NC0079014 permit. The Division will address your
request to rescind Non -Point Source permit NCS000197 under separate letterhead.
Your facility stores hydrocarbon fuels in bulk. The Division began its investigations of hydrocarbon bulk -
storage in 1986. These and subsequent investigations focused our permitting guidance through the last
three, five-year NPDES permit cycles. We investigated tank- and piping -maintenance activities,
contaminants of concern (COCs), best management practices (BMPs), and thereby evaluated the potential
of facilities like yours to imoact North Carolina surface waters.
Your facility requires an individual NPDES permit, and does not qualify for general stormwater General
Permit NCG080000 because:
1. onsite petroleum -hydrocarbon bulk storage capacity is equal to, or exceeds, one million
gallons, and;
2. secondary containment dikes (for product spills) confine stormwater in close proximity
to product tanks and appurtenant piping, potentially creating product -contact
wastewater [CWA Sec. 502(6), 33U.S.C. §1362 (6)], and;
3. routine operations require the manual discharge of stormwater (via a pipe through
secondary containment) to waterbodies of the state, i.e., the release constitutes a point -
source discharge [CWA Sec. 502(14), 33U.S.C. §1362 (14)].
North Carolina therefore concludes that this is a wastewater point source and as such, its discharge to the
natural environment must be permitted under the NPDES Program.
NCDEMY
®*&V
N. C. Division of Water Quality 1617 Mail Service Center Raleigh, NC 27699-1617 [phone] Customer Service
1 800 623-7748

Type.... Individual Outlet Curves Page 7.13
Name.... Outl 6 -81,
j File.... P:\_PROJECT FILES\Black Rock Resources\BROCK POST DT2.PPW
RATING TABLE FOR ONE OUTLET TYPE
Structure ID = CV (Culvert -Circular)
--------------------------------------
Mannings open channel maximum capacity: 1.31 cfs
UPstream ID's= 01, IB
DNstream ID = TW (Pond Outfall)
Pond WS. Device (into) Converge Next DS HGL 0 SUM DS Chan. TW
Elev. 0 HW HGL DS HGL DS HGL Error Error TW Error
ft cfs ft ft ft +/-ft +/-cfs ft +/-ft
-------------------------------------- ------ --------------------
117.10 2.56 117.10 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=S3.83ft Vh-.838ft HL=3.681ft
217.20 2.60 117.20 Free Free .000 .000 Free Outfall
FULL PLOW ... Lfull=53.85ft Vh=.861ft HL=3.782ft
117.30 2.63 117.30 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfu11=S3.86ft Vh=.884ft HL=3.882ft
117.40 2.67 117.40 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.87ft Vh=.906ft HL=3.981ft
117.S0 2.70 117.50 Free Free .000 .000 Free Outfall
FULL FLOW...Lfull-53.88ft Vh=.929ft HL=4.063ft
117.60 2.73 117.60 Free Free .000 .000 Free Outfall
FULL FLOW...Lfull-53.90ft Vh=.952ft HL=4.182ft
117.70 2.76 117.70 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.91ft Vh=.974ft HL=4.282ft
217.80 2.80 117.80 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.91ft Vh=.997f t HL=4.383ft
117.90 2.83 117.90 Free Free .000 .000 Free Outfall
FULL FLOW...Lfull=S3.92ft Vh=1.020ft HL=4.483ft
118.00 2.86 118.00 Free Free .000 .000 Free Outfall
FULL FLOW...Lfull=53.92ft Vh=1.043ft HL=4.583ft
118.10 2.89 118.10 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfullo53.94ft Vh=1.065ft HL=4.683ft
118.20 2.92 118.20 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.94ft Vh=1.088ft HL=4.782ft
118.30 2.9S 118.30 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfullr53.95ft Vh=1.110ft HL=4.882ft
116.40 2.98 118.40 Free Free .000 .000 Free Outfall
FULL PLOW ... Lfull=53.95ft Vh=1.133ft HL=4.982ft
118.50 3.01 118.50 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.95ft Vh=1.156ft HL-5.082ft
118.60 3.04 218.60 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.95ft Vh=1.179ft HLoS.184ft
118.70 3.07 118.70 Free Free .000 .000 Free Outfall
FULL FLOW...Lfull-53.95ft Vh=1.201ft HL=5.282ft
118.80 3.10 118.80 Free Free .000 .000 Free Outfall
FULL FLOW ... Lfull=53.95ft Vh=1.224ft HL-5.383ft
SIN: 121EOIC0709D Bartlett Engineering and Surveying, PC
PondPack Ver. 9.0041 Time: 10:17 AM Date: 10/29/2010

4.0f Type.... Individual Outlet Curves Page 7.14
Name.... Outl 6 -8"
0
6 File.... P:\_PROJECT FILES\Black Rock Resources\BROCIC POST DT2.PPW
RATING TABLE FOR ONE OUTLET TYPE
Structure ID = CV (Culvert -Circular)
--------------------------------------
Mannings open channel maximum capacity:
1.31
cfs
Upstream ID's= 01, IS
DNstream ID a TW (Pond Outfall)
Pond WS.
Device (into) Converge Next DS HGL 0
SUM
DS Chan. TW
Elev.
0 HW HGL DS HGL DS HGL Error Error
TW Error
ft
cfs ft ft ft +/-ft +/-cfs
ft +/-ft
118.90
3.13 118.90 Free Free .000
.000
Free Outfall
FULL FLOW ... Lfu11=53.96ft Vh=1.247ft
HL=5.483ft
119.00
3.15 119.00 Free Free .000
.000
Free Outfall
FULL FLOW ... Lfull=53.96ft Vh=1.269ft
HL=5.582ft
SIN: 121SOlCO709D Bartlett Engineering and Surveying, PC
PondPack Ver. 9.0042 Time: 10:17 AM Date: 10/29/2010

R�
Appendix A
A-1
Index of Starting Page Numbers for ID Names
---- O -----
Outl 6 -S"... 7.01, 7.04
----- P -----
POND 10... 6.01
---- S -----
SUBAREA 10... 3.01, 4.01, 5.01,
5.02, 5.03, 5.04, 5.05
SUBAREA 20... 3.03, 4.02
----- W -----
Watershed... 1.01
WILSON 2010... 2.01
SIR: 121E01CO709D Bartlett Engineering and Surveying, PC
PondPack Ver. 9.0041 Time: 10:17 AM Date: 10/29/2010

■
� � Ergon
Asphalt & Emulsions, Inc.
Certified Mail: 7012 3460 0003 4309 5315
Attn: John Hennessey
NC DENR / DWR / WQ Permitting Section
1617 Mail Service Center
Raleigh, North Carolina 27699-1617
RE: Ergon Asphalt & Emulsions, Inc. —Wilson, NC
NPDES Permit Change in Ownership
NC00089087
Dear Mr. Hennessy:
RECEIVED/DENRIDWR
OCT 10 2014
Water Quality
Permitting Section
Enclosed, please find the following forms:
• NPDES EPA Form 1
• NPDES EPA Form 2C
• NPDES EPA Form 2F
• Permit Name / Ownership Change Form for NPDES Permit Number NC00089087
• Sampling Results
• Chemical Leaching Studies
Also with this submittal, Per Regulatory Citation 15A NCAC 0213.0100, we request the Division
to reevaluate the current permit's sampling requirements and frequencies. The table below
outlines the current effluent limitations and monitoring requirements.
Table 1: Current Effluent Limitations and Monitoring Requirements
Effluent Characteristics
[Parameter Code]
Limits
Monitoring
Requirements
Monthly Average
Daily Maximum
Measurement
Frequency
Flow
50050
-
-
Episodic
Total Suspended
Solids
C0530
-
45.0 mg/L
1/Month
Turbidity
00076
-
50 NTU
1/Month
Volatiles Organics
EPA 624
-
-
1/Month
Semi -Volatile
Organics
EPA 625
-
-
1/Month
WET Acute Toxicity
TAE6C
Based on our industry knowledge and the attached supporting documentation the above effluent
and monitoring requirements are not representative for this facility's processes and products
stored. As stated by Joe Corporon during our May 12, 2014 meeting and as reported on the
past sampling reports (Attachment 5), the facility has not had any issues with meeting the above
requirements. Also included in the attachments are three studies (Attachment 6) conducted to
determine the probability of chemical leaching of asphalt. Through our own testing we have
found these studies to be accurate in the fact that asphalt has a very low probability of chemical
0)U A F (C-f_LV
An Ergon Company I P.O. Box 23028 1 Jackson, MS 39225ZO28 USA 1 601-933-3000 1 http://www.ergon.com

RErgon
Asphalt & Emulsions, Inc.
leaching. Therefore, Volatile Organics, Semi -Volatile Organics, and WET Acute Toxicity testing
are not representative testing parameters for this facility. Table 2 outlines our proposed effluent
limitations and monitoring requirements that are sufficient to accurately and effectively monitor
the facility's stormwater discharges.
Table 2: Pronosed Effluent Limitations and Mnnitnrinn RP.n111rerrlentS.
Effluent Characteristics
Units
Limits
Measurement Frequency
Flow
MGD
Annual Average and
Episodic
Daily Maximum
Total Suspended Solids
mG/L
Annual Average and
Semi-annual
Maximum
Oil and Grease
mg/L
Annual Average and
Semi-annual
Maximum
pH
6.0-9.0
Annual Average and
Semi-annual
Maximum
These proposed effluent limitations and monitoring requirements are consistent with the
sampling requirements at our similar asphalt storage and production facilities in Mississippi,
Texas, Tennessee, Oklahoma, and Kansas.
Should you have and questions or comments please contact me. RECEIVED/DENRIDWR
OCT 10 2014
Sincerely,
Water Quality
Ergon Asphalt & Emulsions, Inc. Permitting Section
Austin Moody
Environmental Engineer
Office: [phone]
Fax: [phone]
Austin. moodvna.ergon. com
Enclosures:
CC: Brad Dixon, EAE-Wilson
Chris Eldridge, Ergon Inc.
File (220-E-02-14- )
An Ergon Company I P.O. Box 23028 1 Jackson, MS 392253028 USA 1 601-933-3000 1 httpi/�.ergon.com

Schematic of Water Flow
EAE-Wilson
Wilson, Wilson County, North Carolina I
Storm Water Runoff 11,600 GIRD Retention Pond 11,800 GPD—y Outtall001 11,800
I
r'
II `1
.yZ—nsunc;rop.,U
h—
Unnamed
C1
d
Tributary
E,
�
C
+O+
O
=
O
U
Contentnea Creek

RECENEDIDENRDWR
Pat McCrory
Governor
A7
OCT 10 2014
±L141
NNCDEAM Water Q$e� on
R Permitting
North Carolina Department of Environment and Natural Resources
Division of Water Resources
WATER QUALITY PERMITTING SECTION
John E. Skvarla, III
Secretary
PERMIT NAME/OWNERSHIP CHANGE REQUEST
This form is for ownership changes or name changes of NPDES wastewater hermits.
"Permittee" references the existing permit Folder
• "Applicant" references the entity applying for the ox nership-'name change.
I. NPDES Permit No. (for tivhich the change is requested): N C 0 0 8 9 0 8 7
or
Certificate of Coverage #:
N C G 5
11. Existing Permittee Information:
a. Permit issued to (company name):
Black Creek Terminal, LLC
b. Person legally responsible for permit:
Paul Young
First MI Last
VP - Regulatory Affairs
Title
P.O. Box 1639
Permit Holder Mailing Address
Jackson MS 39215-
City State Zip
[phone] [phone]
Phone Fax
c. Facility name:
Black Creek Terminal
d. Facility's physical address:
2520 Wilco BLVD South
Address
Wilson NC 27893-
City State Zip
e. Facility contact person:
_ Brad Dixon [phone]
First / MI / Last Phone
111. Applicant Information:
a. Request for change is a result of: ® Change in ownership of the facility
❑ Name change of the facility or owner
tf other please explain:
b. Permit issued to (company name):
c. Person legally responsible for permit
Ergon Asphalt & Emulsions, Inc. - Wilson
Paul Young
First MI Last
VP -Regulatory Affairs
Title
P.O. Box 1639
Permit Holder Mailing Address
Jackson MS 39215-1639
City State Zip
[phone] [e-mail]
Phone E-mail Address
Page 1 of 2 Revised 7'01.201.1

IV.
d. Facility name:
e. Facility's physical address:
f. Facility contact person:
Ergon Asphalt & Emulsions, Inc. - Wilson
2520 Wilco BLVD South
Address
Wilson NC 27893-
City State Zip
Brad Dixon
First MI Last
Terminal Manager
Title
[phone] bdixon ct,blackereekterminal.com
Phone E-mail Address
Will the permitted facility continue to conduct the same commercial/industrial activities conducted prior to
this ownership or name change?
® Yes
❑ No (please explain)
If applicable, the applicant shall submit a major permit modification request to D W R. A major modification shall be
defined as one that increases the volume, increases the pollutant load, results in a significant relocation of the
discharge point, or results in a change in the characteristics of the waste generated.
V. Required Items: THIS .APPLICATION WILL BE RETURNED UNPROCESSED IF ITEMS ARE
INCOMPLETE OR MISSING:
1. This completed application is required for both name change and/or ownership change requests.
2. Legal documentation of the transfer of ownership (such as relevant pages of a contract deed, or a bill of sale) is
required for an ownership change request. Articles of incorporation are not sufficient for an ownership change.
Applicable regulations: 40 CFR 122.41, 40 CFR 122.61 and 15A NCAC 02H .0114
....................................................................................................................
The certifications below must be completed and signed by both the permit holder prior to the change (Permittee), and the
new applicant in the case of an ownership change request. For a name change request, the signed Applicant's Certification
is sufficient.
PERMITTEE CERTIFICATION (Permit holder prior to ownership change):
1, attest that this application for a namelownership change has been reviewed and is accurate and complete to the
best of my knowledge. I understand that if all required parts of this application are not completed and that if all required
supporting information is not included, this application package will be returned as incomplete.
Signature Date
APPLICANT CERTIFICATION
1, Paul Youna, attest that this application for a name/ownership change has been reviewed and is accurate and complete to
the best of my knowledge. I understand that if all required parts of this application are not completed and that if all required
supporting information is not included, this application package will be returned as incomplete.
/�/ZOZy
Si ure � Date
PLEASE SEND THE COMPLETE APPLICATION PACKAGE TO:
Division of Water Resources
Water Quality Permitting Section
1617 Mail Service Center
Raleigh, North Carolina 27699-1617
NPDES PERMIT NAME/OWNERSHIP CHANGE REQUEST
Nee 2 of 2 lteriserl7 012014

Attachment 5
Sample Results

Lou ISIANA STATE UNIVERSITY
A N D A G R I C U L T U R A L A N D M E C if A N 1 C A L C O L L E G E
Schocl cf the roast art! �It�'uo;�rr�ent;'r7epart►rtarrt of Fn: irammentai Stvdres
Re,pome and f;'lsemkal Assessment Team
I28i liner ('oast & 1:nvii-onment 11kh—,
Baton Roinu r. LA 7003 V
D t?S/RCAT06-01
TO: Steve Lehmann. SSC
NOAA-HMRD
FROM: Buffi., Ashton
Response & Chemical Assessment `Ream
Louisiana State University. Dept of Environmental Studies
RE: BARGE MM53/54 OIL SPILL
10 February 2006
The Response and Chemical Assessment Team at Louisiana State University analyzed one (1)
paving grade asphalt sample collected from Barge MM54 (Barge MM53's sister barge) by
GC/MS; and performed a "water temperature" experiment to determine the properties of the
sunken asphalt at increasing temperatures. Stemple identifications and descriptions are given in
1`able 1. The GC/MS analvsis results are in Tables 2 and 3. and the results of the water
temperature experiment, including photographs, are given on pages 4 and 5.
Table 1. Sample Identifications and Descriptions.
LSIJ Ill##
Field lD#
Sample Description
Collection Date
2N6040-01
n/a
Asphalt from Barge tv M54
28 Jan 06
t'?''Al' has made the following conclusions:
• Due to the low concentrations of PA1-ls in the asphalt sample, we feel that there is a ve?y
lo►v probability of chemical leaching. The high temperature refining process and the
heated transport process for this paving grade asphalt greatly reduces the water soluble
PAHs, which is evident in the GC/MS data. The naphthalene compounds that are present
in the sample will naturally- degrade, and the other PAI-Is will be encapsulated within the
asphalt "pancake".
• There is little to no probability of sheening from the Bard, sunken asphalt, even at water
temperatures around 80' I'. The hot asphalt hitting the water results in a hardened asphalt
matrix that sinks. Once it hits the bottom surface, the hardened asphalt wily slowly
biodegrade throughout the rest oi'the winter and spring.
DES/RC AT06-01
Barge N. B15-31i4 Oil Spill

GUMS Results (Fast-ti(1i method):
Fable 2. Normal Alkane Concentrations in Barge NIN153154 :asphalt Sample
LSU ID#
2N6040-01
Site
Barge MM53/54
Sample Decri tion
Asphalt
ALKANES
Conc n !m
nC-10 Decane
2.0
nC-11 Undecane
2.5
nC-12 Dodecane
2.0
nC-13 Tridecane
2.4
nC-14 Tetradecane
2.4
nC-15 Pentadecane
3.1
nC-16 Hexadecane
3.8
nC-17 He tadecane
3.5
Pristane
1.1
nC-18 Octadecane
4.0
Ph tape
1.7
nC-19 Nonadecane
4.2
nC-20 Eicosane
4.7
nC-21 Heneicosane
6.0
nC-22 Docosane
6.8
nC-23 Tricosane
8.6
nC-24 Tetracosane
11
nC-25 Pentacosane
11
nC-26 Hexacosane
12
nC-27 He tacosane
15
nC-28 Octacosane
16
nC-29 Nonacosane
19
nC-30 Triacontane
24
nC-31 Hentriacontane
28
nC-32 Dotriacontane
35
nC-33 Tdtriacontane
39
nC-34 Tetratriacontane
26
nC-35 Pentatriacontane
28
TOTAL ALKANES
323
DFS/ ICAT06-p1
liar-c NIN153/54 Oil spill

Fable ;. PAII Concentrations in Barre NFNIS3154 Asphalt Sample (nd=nondetectibellm detection limits)
LSU ID#
2N6040-111
Barge WA-53154
Site
Sample Decri Lion
Asohalt
PAHs
Conc n tm )
Naphthalene
0.51
C•1 Na h
2.3
C-2 Naph
2.8
C-3 Na h
2.4
C-4 Na h
nd
Fluorene
nd
C-1 Fluor
nd
C-2 Fluor
nd
C-3 Fluor
nd
Dibenzothio hene
0.45
C-1 OBT
2.0
C-2 DBT
4.8
C-3 DBT
6.5
Phenanthrene
0.52
C-1 Phen
1.7
C-2 Phen
3.9
C-3 Phen
4.5
C-4 Phen
nd
Anthracene
nd
Fluoranthene
nd
P rene
nd
C-1 P r
0.75
C-2 P r
1.8
C-3 P r
2.6
C-4 P r
2.6
Na thobenzothio hene
1.1
C-1 NBT
10
C-2 NBT
17
C-3 NBT
21
Benzo a Anthracene
0.71
Chrysene
0.73
C-1 Chry
2.3
C-2 Chry
4.3
C-3 Chry
nd
C-4 Chry
nd
Benzo (b) Fluoranthene
nd
Benzo k) Fluoranthene
nd
Benzo e P rene
nd
Benzo (a) P rene
nd
Per lene
nd
Indeno (1.2.3 - cd) P rene
nd
Oibenzo (a.h) anthracene
nd
Benzo tc.h.il perylene
I nd
TOTAL PAHs
1 97
DE'ti/lt(A I'06-01
l3aru,c -NI NIU154 Oil Spill

Water Fxnerimenl Procedure and Results:
I he asphalt sample was heated to approximate 110"F and x%as added to a beaker ofdeionited
water at a temperature nl 60"F. The water was then healed to the linal temperature ill' I2Y'F.
Observations were made and pittures were taken at the tollo%%ing temperatures:
Water temperature o f' 60"F
o Asphalt Iloats at first (Figure I ), bill then sinks to the bottom alter swirling thRECEIVED/DENR/DWR
beaker (Figure 2).
o No visible sheen or oil on the water surface at this water temperature after OCT 10 2014
swirling the beaker with the asphalt on the bottom.
Water Quellty
Permitting Section
Figure I.
Figure 2.
• Water temperature of 70°F - 90°F
o Asphalt still at bottom of beaker and is stuck to the glass.
o No visible sheen or oil on the water surface at this water temperature after
swirling the beaker.
o Asphalt has a glassy appearance.
• Water temperature of I00°F — I I OT
o Asphalt still at bottom ol'beaker and is still stuck to the glass.
o No visible sheen or oil on the water surface at this water temperature after
swirling the beaker.
o Asphalt appears to be melting, as shown in Figure 3.
1)1; S/RGCI06-01
Barge NINI5364 Oil Spill

Figure 3.
• Water temperature of 120°F - 125T
o Asphalt still at bottom of the beaker, stuck to the glass. When the asphalt glob
was moved with a spatula, some of the asphalt Floated to the water surface.
o Small oil droplets are visible on the surface of the water; however, not really able
to photograph them.
o Appearance of the asphalt at 1250F is displayed in Figure 4.
Figure 4.
DE;S/ItCA 1'04-01 5
Rai ge )I?153/544 Oil Spill

ASPHALT INSTITUTE
Executive Offices and Research Center
Research Park Drive
P.Q. Box 14052
Lexington, KY 40512-4052
USA
Telephone [phone]
FAX No. 859-288-4999
LEACHABILITY OF ASPHALT AND CONCRETE PAVEMENTS
Anthony J. Kriech (Heritage Research Group, 7901 W. Morris St., Indianapolis, Indiana 46231,
U.S,A.; e-mail [e-mail])
CONTENTS
INTRODUCTION
SITE LOCATIONS
SAMPLE PREPARATION
METHODS
SAMPLE ANALYSES
COMMENTS
CONCLUSIONS
REFERENCES
0. INTRODUCTION
The IAPA (Illinois Asphalt Pavement Association) contracted with Heritage Research Group to
study the leachability of both Portland Cement Concrete (PCC) and Hot Mix Asphalt
Pavements (HMA). Granular materials, including soil from the edge of each pavement type,
were also tested to determine leachability. The design of this experiment was through the joint
cooperation of the Illinois Environmental Protection Agency, Illinois Department of
Transportation and IAPA. The purpose of the study was to determine the suitability of using
concrete, asphalt, or soils from the surrounding roadway for use as clean fill. The concern is
that the incidental spills onto the road from cars and trucks could contaminate the pavement
and surrounding road side, and make these road materials unsuitable for use in clean fill
situations below the water table. Specifically, unsubstituted Polynuclear Aromatic
Hydrocarbons (PAH's) and heavy metals were studied. These were chosen because volatile
and semi -volatile compounds, which may be spilled on the road, evaporate quickly. Previous
studies by Heritage Research Group'2 have not found these compounds present. Only the
metals and high molecular weight organic compounds tend to remain.
1.0 SITE LOCATIONS
The Illinois Department of Transportation located a section of pavement on Route #4 south of
Springfield. The unique feature of the pavement section was that it contained Portland Cement
Concrete, which was built in 1976 and a Hot Mix Asphalt pavement, which abuts this section
and was also built at the same time. Because these sections are contiguous, the traffic on
each are identical. Three sites were randomly selected in each pavement type, as to
longitudinal location. Coring occurred on December 17, 1991 by IDOT District personnel. Once
a site was selected, three four inch specimens were taken across the pavement. The first is
between the wheel paths, the second was in the outer wheel path, and the third was taken
outside the outer wheel path. A sample of soil and granular material was also taken from the
shoulder of the road. The sample identification and locations are listed in Fi ure A. The "W'

proceeding the numbers indicates white (PCC) pavements and "B" indicates black (HMA)
pavements.
Heritage Research also received some laboratory prepared samples from IDOT laboratories.
&.r 1ple W-0 is a Portland Cement Concrete laboratory cylinder and is considered typical of
Portland Cement Concrete by I DOT. Sample B-0 is a Hot Mix Asphalt sample prepared by
(DOT and the compositional mix design is also considered typical by IDOT. These samples
were used as controls and are free of any potential contamination: which the road samples
may have received since they were placed in 1976.
2.0 SAMPLE PREPARATION
To prepare the sample for Toxic Characteristics Leachability Procedure (TCLP) in accordance
with EPA guidelines, the samples were crushed to pass the 9.5 mm. sieve size. An impact
crusher was used to reduce the samples to below this size.
Representative materials from each sample location were combined with other samples sites
to test various hypothesis about pavement contamination. The first was that contamination
may be greater between the wheel path, because this is where crankcase drippings tend to
fall. To test this theory, all samples from between the wheel path were combined for each
pavement type to make one sample. A second hypothesis was that the samples taken from the
wheel path would be cleaner, because the tires are constantly wearing this pavement away.
This idea was tested by combining all samples in the wheel path for each pavement. Samples
outside the wheel path were also combined to make a sample to determine if there was a
similar trend in the data. The soil samples from the shoulder were also combined to determine
if the soil was higher or lower than the pavement in leachability. Finally, one transverse sample
was taken from one location of each pavement type and compared to longitudinal samples to
test for site specific contamination. All of these combined samples were compared to the
laboratory samples of each pavement type, which had been prepared in the laboratory as a
control. Table A lists the combination of sites used to make each sample for TCLP testing.
3.0 METHODS
After the combined samples were prepared by Heritage Research, they were submitted to
EMS Heritage Laboratories for TCLP testing. EMS Heritage is an EPA certified laboratory. The
test methods used are listed below.
Contents
Test`
TCLP Procedure
PAH`s I
MethodlProcedure - -----_
SW-846-1311
SW 846-8310
Metals _
-
Barium_
SW-846-7080
Cadmium
Chromium
SW-846-7130
SE-846-7190
Lead !
SW-846-7420
Silver Arsenic
PKV-846-7760
Selenium
SW-846-7740
Mercury ;
SW-846-7470

4.0 SAMPLE ANALYSES
A summary of the test results from the TCLP are listed in Table B for the Portland Cement
Concrete Pavement and soil located next to this pavement type. Table C lists the leachability
of Hot Mix Asphalt samples and soil corresponding to this pavement.
Please note that PAH's are measured in ?g/L, which is parts per billion. The metal leachability
is in mg/L or parts per million. The detection limit of the barium analyses varied with the
sample. Because of high calcium in the leachate of some samples, the detection levels varied
from 0.2 to 2.0. Matrix effects do impact on the detection level achievable in these samples.
5.0 COMMENTS
5.1 Both the PCC and HMA laboratory prepared samples from IDOT had measurable amounts
of metals leaching, but no measurable PAH's. The PCC sample indicated a small amount of
leachable chrome. The HMA had measurable barium in the leachate.
5.2 Samples taken in the PCC section, whether taken longitudinally or transversely, showed
trace amounts of naphthalene and phenanthrene in two samples. Both samples contained
material from site W-3, so it could be the same contaminant. Four samples contained a small
amount of Naphthalene. These values were, in all cases, less than one part per billion. One
sample from the wheel path had measurable barium on the leachate.
5.3 The soil samples taken from the PCC shoulder produced no leachable PAH's. However, a
measurable (3.5 ppm.) level of barium was found.
Contents
5.4 The HMA pavement appeared quite similar to the PCC pavement in leachate results. Only
naphthalene and phenanthrene were found in the pavement leachate. In all cases, the level
was under one part per billion. Metal leachate was confined to barium, which was present in
both the laboratory and field samples. This would indicate that barium is not coming from
contamination, but rather is most likely coming from the aggregate in the mixture. These
values would probably be lower if the sample was not crushed, which exposes the uncoated
aggregate surfaces and increasing the exposed surface area greatly.
5.5 The soil from the HMA shoulder also contained a measurable level (0.76 parts per billion)
of naphthalene. Since the laboratory samples did not have measurable levels, it is possible
that this came from surface contamination. Used crankcase oils and tire composition contains
measurable quantities of both naphthalene and phenanthrene, and could be potential sources
for these very low, but measurable values.
5.6 The hypothesis that contamination would be greater between the wheel paths than at other
location was not supported by these results. Overall, the level of leachable PAH materials was
too low to determine trends in the data.
6.0 CONCLUSIONS
This study found that both PCC and HMA pavements each have very low levels of leachable
metals and PAH materials. The relative low levels of leachable materials from both pavement
types are quite similar. Soils from the shoulder of the road are quite similar in characteristics to
the PCC and HMA pavements.

7.0 REFERENCES
1. Kriech, Anthony J. Evaluation of Hot Mix Asphalt for Leachability. HRG #3959AOM3.
October 15, 1990.
2. Kriech, Anthony J. Evaluation of RAP for Use as a Clean Fill. HRG #4122EM02. January 30.
1991.
TABLE A
Sample Identification
Sample #
Sample Identification :Description
1 `W-0
PCC Uncontaminated, Laboratory Specimen
2
W-1, 2, 3
PCC Transverse Across the Pavement
3___......
W--1,_5,._9
:PCC
Between Wheel Path, Longitudinal _Sample
--
4
W 2, 6, 10
PCC In Wheel Path, Longitudinal Sample
5! _
W 3, 7, 11 °
PCC Outside Wheel Path, Longitudinal Sample _
6 `W
4, 8, 12
PCC Soil from Shoulder, Longitudinal Sample _
7
IHMA Uncontaminated, Laboratory Specimen ;
8
B-1, 2, 3 1
B-1, 5, 9
HMA Transverse Across the Pavement '
9 ;
HMA Between Wheel Path, Longitudinal Sample
10 1
B-2, 6, 10
HMA In Wheel Path, Longitudinal Sample
1 1B_3,
_ _
7, 11^
HMA Outside Wheel Path, Longitudinal Sample
12
B-4 8, 12
IHMA Soil from Shoulder, Longitudinal Sample _
Contents

TABLE B
Illinois TCLP Test Results for Portland Cement Concrete Cores
[Sample Number
(Control)
2
3 4
5 ;fi
(Soil) --
Site Number
PAH's, N/L
W-0
W-1,2,3
W-1,3,9
W-2,6,10
W _
3,7,11
_ Heritage
W Det.
4,8.12 Limit
[Naphthaiene
BDL
0.44
0.21
0.23
0.26
BDL
0:16
Acena hth lene
BDL
BDL
BDL ;
_ BDL ^:
_BDL
BDL! J
BDL
BDL —r0.25
F�cenaphthene `
BDL_
BDL f
BDL
0.16
__—
Fluorene
..__-_-------.____.............._.__.__ _..___ _ �
Phenanthrene
Anthracene I
Ffuoranthene
_ -J _BDL
BDL i BDL €
_ _.
BDL 0.44
BDL BDL ,
BDL BDL
BDL
_ _..
BDL
_ BDL
BDL
BDL i
__ _. _. ___..
BDL '•,
BDL
BDL
BDL
..j
0.26
BDL
'
BDL _
,
BDL
BDL
_ 0.019
0.16
0.021 -
BDL
BDL
0.021
Pyrene
_. __-- - _-.. _. _ _.— _,
BDL BDL
^BDL
BDL
BDL
BDL f
0`075
��tjzo(A)Anthracene
BDL BDL
BDL
BDL
BDL
BDL -+
BDL
BDL
- -!
0.013
0.041
---
Chrysene
BDL BDL
BDL
BDL
Benzo(B)Fluoranthene
BDL BDL
_ _ _ ._
BDL BDL
BDL
........
BDL ;I
BDL
..........�
BDL
__
0.029
-- --- -..
Benzo K Fluoranthene
BDL
BDL
BDL--
BDL
0.013
Benzo(A)Pyrene
Dibenzo A,H Anthracenel
( )
Benzo(G, H, 1) Pery Iene
_ BDL ?
BDL
BDL
BDL
BDL
BDL
BDL
BDL I
BDL
BDL
BDL 't
BDL
0.023
BDL
BDL
L
_
0.085
-
BDL
BDL
B—DL--�-�
BDL I
0.14
indeno(1,2,3-cd)Pyrene
BDL
BDL
BDL
BDLII
BDL
BDL
0.028
Metals,_mg_/L_
Barium_
BDL
BDL ':
_BDL
1.2*
BDL
3.5
_ 2.000
Cadmium
Chromium
JI-ead _ _ _ _
BDL _�-_
0.072
BDL
BDL
BDL -J
_ BE
BDL
BDL -
BDL
BDL
BDL
BDL _
BDL
0.020
0.050�
_BDL
i BDL
BDL
B_DL
_ BDL
0200�
Silver _ _ _
Arsenic_
_BDL
BDL
BDL s
BDL
BDL
BDL
_BDL BDL s
BDLi� BDL
BD_L
BDL_I
_0.040
0.005�
Selenium
^ BDL
BDL
j BDL
BDL BDL
BDL -BDL
_ _1
BDL
__ BDL
0.010
]mercuryBDL
BDL
BDL
• This sample had a detection limit for barium of 0.2.
Contents

TABLE C
Illinois TCLP Test Results for Portland Cement Concrete Cores
Sam le Number ;F7 (C�o--n-trot
8
9 -F-10
11
Fi Soil
i Site Number
i._-_...__...__._._......----.._..
B-0
B-1,2,3
-
B 1,3,9
_ _ ..
B-2,6,10 :
..
B-3,7,11
�
B-4,8-12
.. ___--.._
Heritage'
Det.
_...._.emit-
_...--._..._......._:..
.:
.............. .
Naphthalene ._
BDL.-...
._
26
._.__.0.31 _.._..
0.28......... .
Acenaphthylene
BDL
...026...- ..:....0
BDL
BDL
BDL
-BDL
BDL _
_ 0.25 _
Acenaphthene
_._._°...BDL
,
-.BDL
BDL....._
._...BDL ,
_ BDL__.i--_0.16._.
Fluorene
__--BDL
BDL.....-_.._._
-
BDL . _..
.__._BDL-- I
BDL
- ..BDL....:
BDL }
- -0.019
Phenanthrene
BDL
-BDL
BDL _ J.
BDL_ ��—�0.3-0
;
BDL
_ _BDL IF
0
Anthracene
BDL
BDL -- `
BDL
- -BDL -
BDLW�
--BDL___
BDL
_BDL:
BDL __
0.021
FluorantheneDL------
BDL _�
0021-
Pyrene
Benzo(A)
i
nthracene
Chrysene IE
BDL
BDL
BDL
BDL
BDL i
j
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL '
BDL
BDL
0.075
0.013
0.041 t
Fluoranthene
BDL
BDL
BDL {
BDL
BDL it
BDL
0.029
Benzo(K)
t
Fluoranthene
BDL
BDL
BDL i
BDL
BDL
BDL
0.013
Benzo(A)Pyrene
- BDL _
BDL i�
BDL
BDL
BDL-ir
DL i
-0.023
Dibenzo(A,H) j
Anthracene_
BDL
BDL
BDL
BDL
[:iD:L:.*..,BDL
0.085
Benzo(G,H,I)Peryle
BDL `•:
BDL
BDL
BDL
BDL
BDL_
Indeno(1,2,3-cd)
Pyren_e
BDL
'
BDL
_
4�
BDL
_
BDL I BDL
-
BDL
0.028
Metals, mgA-
-' -
Barium
2.9
3.7 BDL
3.1 2.6
3.5
2.000
.Cadmium
BDL
BDL , BDL
BDL
0.020
IChromium
BDL
BDL BDL i
BDL BDL ���
�_
BDL
0.050
Lead
BDL �w-
_-BDL; _BDL_
-
_ -BDL iBDL
_
. _BDL _
�0.200 _
Silver
!�
BDL BDL
BDL
BDL BDL
BDL
0.040
Arsenic
E
BDL_....
BDL E�...
005
..._........
Selenium ---
Mercury_
.
BDL
BDL
_.._
BDL
BDL
-BDL
BDL
BDL
BDL F BDL
BDL BDL
.BDL....
_BD_ L f
BDL
..0 ..
0.010
0.005
Contents

ASPHALT INSTITUTE
Executive Offices and Research Center
Research Park Drive
P.O. Box 14052
Lexington, KY 40512-4052
USA
Telephone [phone]
FAX No. 859-288-4999
Oregon And Washington Fish Hatcheries Lined With Asphalt
by Ed D. Schlect, District Engineer, Asphalt Institute
More than 30 fish hatchery ponds are operated by Oregon and Washington and many of them
are lined with hot -mix asphalt (HMA). The states' fish and wildlife officials say the ponds are
durable and produce good -quality fish.
HMA is one of the most commonly used liners for hatchery ponds, according to Ray Sheldon,
hatchery operations coordinator for the Oregon Department of Fish and Wildlife. 'We've had
good results rearing quality fish" in the ponds, says Sheldon.
One of Oregon's ponds, the Clackamas fish hatchery at McCiver State Park, releases more
than 1.5 million chinook each spring into the Clackamas River. The hatchery houses the fish
about 18 months before releasing them into the river.
In Washington, the State Department of Fisheries and the Department of Wildlife operate more
than 25 hatcheries. At least two Indian tribes in the state also maintain hatchery ponds lined
with HMA.
A typical Washington state fish hatchery pond is 5 to 7 feet deep and covers a one-half acre
surface area. The liner is 2 or 3 inches of HMA on 8 inches of granular base. Liners consist of
3/8-inch nominal maximum -size aggregate with 6.5 percent asphalt cement. The higher
volume of asphalt cement ensures a low -void, impermeable mix.
When the ponds are empty, pressure relief valves in the pond bottom relieve hydrostatic
pressure under the liner. Some ponds are designed with pressure relief valves throughout the
pond floor while others use valves only in the drain channel. All joints between the HMA liner
and the headwalls and outlet gates are sealed with rubberized asphalt liners.
Many of the HMA ponds are sealed with an asphalt emulsion because a bacteria detrimental to
r:>' r an find a habitat in the surface voids of the HMA. Current specifications require either
a proprietary asphalt emulsion sealer, a CSS-1 or a CS-1 h.
Both Washington and Oregon state agencies are pleased with the effectiveness of the HMA
liners and plan to use them for additional fish hatcheries in the future.
This article appeared in the Winter 1990-91, Volume 4, No. 3, ASPHALT magazine.

;tI1tI•hhi\{}? fit. 1!tI WI
0011 J$ It}ll+
DE TERNIINATION OF POLYCYCLIC
AROMATIC COMPOUNDS IN ASPHAI:I- AND
IN CORRESPONDING LEACHATE WATER
A. J. Kriech
J. T. Kurek
L. V. Osborn
H. L. Wissel
B. J. Sweeney
heritage Research Group, Indianapolis, Indiana, USA
The environmental impact of polveYclic aromatic
compounds (PACs) in asphalt (bitumen) materials is related
to their availability for environmental transport and
biouptake, rather than their total concentrations. This study
examines six Stratetg c Highway Research P►ogrant (SARI')
paving asphalts and four commercial roofing asphalts.
Three cleanup procedures fir the neat asphalt samples are
evaluated. This study reports on anal),ses fur 29 PACs,
including the EPA 16 prioritypollutant P.411.s and
additional Persistent Bioaccumulative Toxins. These require
reporting by the U.S. EPA under the Emergency Planning
and Community Right -to -Knott, Act (EPCRA) section 313.
Tire analytical prvtocol,for analysis of the higher molecular
weight PACs by GC/MS it reported, with inclusion of
GCIUS/MS verification of sone of the detectahle
compounds. Additionally, each asphalt uws taken through a
toxicity characteristic leaching proceclure firllowi» g U.S.
EPA method SW846-1311. Results oj'the paving and rzrofing
asphalts and their con-v�sponding leachate waters are
presented in this study.
Kevwords EPCRA section 313, GC/MS. leachate, PACs, paving asphalt,
rofin asphalt
USA.
The atrthors thank Caralyn K. Clark for her diligent efforts to finalize and re%ie«v this article.
Address correspondence to A. J. Kriech, i leritage Research Group, Indianapolis. IN 46231.
517

i I 1 A. kricch rl al.
.Asphalt cement is (lie nondistillable fraction obtained in the distil-
lation of crude oil. It is a c01111))eX mixture of high-n)olecular-weight
aliphatic and aromatic hydrocarbons and organosulfur compounds with
smaller amounts of nitrogen and oxygen COMI)011nds. While there are
many similar components in different asphalt samples, the exact compo-
sition and properties are a function of both the source of the crude oil and
its processing (1). Asphalt is used widely for highways, parking lots, air-
port runways, and has also been used in many hydraulic applications for
waterproofing reservoirs used for drinking water, fish hatcheries, boat
ramps, and canals (2). A significant number of roofing systems also use
asphalt in their formulation including asphalt -shingled roofs and flat or
sloped built-up roofs (BUR).
Some standard differences between asphalt paving and roofing in-
clude application temperatures, hardness of the asphalt, and the presence
of aggregates. BUR roofing asphalt is typically harder than paving as-
phalt cement. Penetration values for BUR roofing asphalt range from 12
to 35; paving asphalt typically has 50 orhigher. Roofing application tem-
peratures can be as high as 337"C, but are typically in the range of 232`
to 274"C. Application temperatures for paving are generally less than
160°C. Hot mix asphalt composition generally consists of 95% mineral
aggregate (rock) and 5% asphalt cement for paving applications.
Because of their widespread use in environmental applications,
asphalt paving and roofing materials are subject to storm water runoff
from rainfall events. This study examines the presence of PACs in the
neat asphalt cement as well as the leachate from asphalt.
This study reports on analyses for 29 PACs, including the U.S. EPA
16 priority pollutant PAHs and additional Persistent BioaccumuIative
Toxins (PBT). These require reporting by the U.S. EPA under the Emer-
gency Planning and Community Right -to -Know Act (EPCRA) section
313 (3) if certain conditions are met. Benzo[g,h, i]perylene is a separately
listed PAC which requires reporting at a much lower threshold. The act
also requires reporting if these PACs are released to the environment
through air, water, or the land. As such, a thorough understanding of
their partitioning in the environment is required.
Previously reported studies show very low content of PAHs in the
leachate fraction of asphalt (4). Even in reclaimed asphalt pavement
from old roads, which could contain PAHs from crankcase drippings
and tire abrasion, studies have found that recycled asphalt pavement
(RAP) is nonleachable for the EPA's 16 standard PAI-Is (5). Other in-
vestigations (6-8) concerning leachability of road materials indicate
that the PAFf concentrations were near or below detectable limits. This
study reports the 16 standard PACs, but fOCLISeS on the analysis of an

OCILTMilWfirur P4Cc in : t.VVILrlt ? 19
extended list of PAC's (13 additional compounds not listed before and
required by E:PCRA), for both the raw asphalt material and its coire-
sponding leachate. The significance of these compounds and their envi-
ronmental fate are related to their properties, some of which commonly
require metabolic activation to produce reactive intermediates before
they can express their toxicity, mutagenicity, and carcinogenicity (9).
A few compounds on the list are not considered carcinogenic (phenan-
threne) or the status is unknown (chrysene has mixed reviews). Others,
such as benzo[u]pyrene, have been extensively studied and are classified
as known carcinogens.
Since these studies were performed on virgin asphalt materials, it
does not address spills from traffic and equipment that can lead to leach-
ing of these compounds from other sources which could be released
from pavement during storm water runoff. The presence of some of
these compounds like 3-methylcholanthrene and 1-nitropyrene would
not be expected in neat asphalt, but are on the EPCRA list for other RECEIVEDIDENRIDWR
materials.
EXPERIMENT
Specimens
Six paving asphalts were obtained tiom the Strategic fligbway Re-
search Program (SHRP) library. SHRP was a $150 million research study
of asphalt sponsored by individual State Departments of Transpot•tation
across the United States. The SHRP library stored samples of asphalt ce-
ments from petroleum refineries throughout the United States. These six
paving asphalts are produced from single -source crudes rather than mix-
tures and represent a significant portion of the composition variability
in asphalt cement produced commercially in the United States.
Four roofing asphalts were obtained from different regions of the
United States from commercial sources of roofing asphalt for built-up
roofs.
Precipitation of Asphaltenes for Extraction of PACs from Asphalt
Asphaltenes are a component of asphalt, defined by ASTM as solu-
ble in carbon disulfide but insoluble in paraffin naphthas. This compo-
nent is comprised of polynuclear hydrocarbons of molecular weight up
to 20,000..joined by alkyl chains (10). It is precipitated and removed
to minimize extraction and analytical complications. Asphalt samples
OCT 10 2014
Water Quality
Permitting Seeccttion

20 A..1. Kric'c-11 c t a/.
(--0.4 g) were weighed into a 50 nil- beaker. then dissolved in 10 ml_
of methylene chloride. This was quantitatively transferred to a 100-mL
volumetric flask and brou(,ht to the mark with hexane. lifter mixing,
samples were allowed to settle overnight prior to aliquot removal for
centrifugation and subsequent cleanup. 'this procedure is similar to the
one outlined in ASTM D 4124-97 (10).
CN/Si Cleanup Procedure (Extraction Method A)
This cleanup procedure was initially used since the combination of a
cyanopropyl and silica gel chromatographic separation scheme has been
shown to be successful for the EPA list of 16 PAHs in asphalt fumes
(11). Twenty milliliters of the above hexane solution were concentrated
to 2 mL, then passed through a cyanopropyl cartridge and eluted with
hexane to 25 mL. This fraction was concentrated to 2 mL, then taken
through a silica gel cleanup using'' g of silica baked at 270'C for 2 hr.
Twenty milliliters of hexane was used to elute the aliphatic portion of
the samples (this fraction discarded), and 20 mL of methylene chloride
was used to elute the PAC fraction.
Acetonitrile/Methylene Chloride Liquid/Liquid Extraction
(Extraction Method B)
This extraction procedure was designed to replace Extraction
Method A, since dibenz[u j jacridine did not survive the silica gel cleanup
and to attempt to minimize the aliphatic background prevalent even after
Method A's cleanup. After centrifugation, 20 mL of the hexane/methy-
lene chloride solution (90/ I 0) was transferred into a 40-m L via]. Ten
milliliters of 20% methylene chloride in acetonitrile (ACN) was added,
then the vial was manually shaken for 2 min. After centrifuging, the
bottom layer was transferred to a new 40-mL vial. Using 5 mL of the
20% methylene chloride in ACN solvent, this step was repeated twice.
The combined extracts were concentrated to slightly under 1 mL using
a nitrogen evaporation system at 54'-59°C. For all asphalt samples, two
phases formed after settling overnight. The exact composition of the
bottom phase was not investigated, although it is believed to contain
high -molecular -weight non -"GC able" material. The top ACN phase
was removed and brought to a final volume of 1.0 nil- in ACN. For
simplicity, this method will subsequently be referred to as the ACN
Method B.

DMSO Method (Extraction Method C)
This method is a modification of a method previously developed
(IP346/80) (12) for extraction of Polycyclic Aromatics in Petroleum
Fractions by Dimethylsulfoxide (DMSO). T%N.-enty milliliters of the orig-
inal hexane solution after asphalt precipitation was concentrated to 5 mL
and extracted in triplicate with 2.5 mL of DMSO. Ten milliliters ofwa-
ter was added to the DMSO extracts, which was then back extracted
twice with isooctane, 5 mL first, and then 2 mL. The combined isooc-
tane layers were extracted in triplicate into 2.5 mL of DMSO as before.
The DMSO was diluted with water and back extracted three times into
isooctane. This isooctane extract was concentrated to 1.0 mL, then an
aliquot combined with internal standards (chrysene-d12 and perylene-
d>>) for GC/MS analysis. Surrogates could be added prior to extraction
but were not added in this study.
Leachate Procedure
Samples of 10 asphalts were frozen to facilitate breaking the asphalt
into small enough pieces to pass through a 9.5-mm sieve. Samples were
leached according to SW846 1311. Toxicity Characteristic Leaching
Procedure (13), which is designed to emulate what goes on in the envi-
ronment. This TCLP test is a batch leaching prescribed by the EPA to
determine whether a solid waste is hazardous by toxicity characteristic.
One hundred grams of the sieved asphalt material were tumbled for 18 h
in 21 of p1l 4.93 buffered solution (acetic acidisodium hydroxide mix).
Extraction of Leachate Water for PAC Analysis
Method SW-846 3510C (14) (Separatory Funnel Liquid -Liquid Ex-
traction) was used for the extraction of the Leachate waters. This method
involves three triplicate extractions of the water with methylene chlo-
ride under neutral, basic, and acidic conditions. The base/neutral and
acid extracts were combined prior to concentration to 1.0 mL in methy-
lene chloride.
Analytical Method for EPA's 16 PAHs
EPA SW846-8270 B (15) was used for the analysis of the leachate
water extracts and the total asphalt extracts for 8 of the 29 PAC's reported
(those not on the EPCRA list, but on the EPA's list of 16).

Program Modifications for GC'/.N— iS Analysis of 22 EPCRA
Section 313 Compounds
Using a Varian Saturn 4 GCINJIS/MS, the column (a 25 m x 0.25 mm
ID BPX5 0.25 micron film SGE Cat # 0541 13) was held at 150 C for
3 min and then increased to 300 ' C at 10'/min and held for 15 min, then
increased to 320 -C at 2'`/min kept for 2 min. With a CT 8200 autosam-
pier, the solvent plug 0.2 M L with upper and lower air gap and sample
volume of 2.0 pl- was programmed with air-dry after wash at an in-
jection rate of 5.0 IA/sec and hot -needle time of 0.04 min. The mass
range was 100 to 410 m/z and the scan time 0.600 sec, segment length
30 min, filament delay 2.70 min, mass defect 40 mp/100 14, and back-
ground mass 98 miz. Most importantly, the injector was at 320°C (de-
activated 1078 glass insert with glass wool -Varian Cat no. 392611953),
transfer line at 325°C, and the trap temperature at 285' C. An internal
standard quantification procedure was used. A total of seven calibration
standards (dilutions of a custom mix prepared by AccuStandard, USA)
were analyzed to provide a concentration range of 0.1 to 10 pg//tL.
Figure I shows a chromatogram of the 22 compounds on the EPCRA
l::aw.tt..urtu+ :•lot
r.Ca:
0 ^tttntiun: 3EI.HH PIC* 1419
nns3cs IW-105
Plat td+' 1,ififl t.;, ZGt,N
W%nyr:' 1 -n .:fdilt
S"HJ.. - '471729
i
13.14115.10
1
910
A
i1 �17
2122
13
?
192o 2324
12
}
1
27 28 29
i
ilkUl
1iS3P 2,k�N
?.-ti+i�
t 1 .9y
1 � _ �y ' y •':fit
g? . cq
:\ = C'hrt•sene d-12
H = Perylene d-12
FIGURE 1. A chrotnato�,rani of it 10 pgipL calibration standard of the 22
EPCRA compounds. The orcler of elution is outlined in Table 5 for
compounds 7 to 29.

Oetc•rnnituti ,n ()j P.1 .V in . Js/)holt 521
section 313 list. The linear ranee for most of these compounds was
between 0.1 and 10 pg/11 L. _Rvo compounds, I -nitropyrene and 7.12-
din»thylbe0zz[ct]antliraccile. prodUced nonlinear curves. The instrument
limit of detection is approximately 0.10 pg/pl. for these 29 analytes.
Values between 0.05 and 1.0 pgip 1.. are semiquantitative and reported
as estimated.
GC/MS/MS Analytical Method for Verification
of Selected Compounds
Using the same system as above, a MS/MS program was developed
for selected compounds with mass 228, 252, and 276. The same GC
program described above was used. The mass data collection was broken
into separate segments by inserting a unique ion preparation method for
each molecular ion class. The ion preparation methods are generated
by the Saturn software and a unique waveform is applied to the ion trap
afterelectron ionization. This waveform ejects all nontarget ions from the
trap allowing increased sensitivity. Collisionally induced dissociation by
applying a secondary voltage is then used to obtain the fragmentation
pattern of the trapped ions.
RESULCS AND DISCUSSION
Separation and analytical procedures far asphalt materials pose ex-
traction and analytical challenges when attempting to find trace quanti-
ties of PACs in a primarily aliphatic high -molecular -weight media. It is
one of the most complex, difficult materials to chemically analyze, even
after cleanup steps and separation techniques are employed (Figure 2).
Analytically, the heating zones of the instrumentation were elevated to
accommodate the higher -molecular -weight compounds on the EPCRA
313 list. To retain the ion trap at 285` C, glass wool was placed over the
trap exterior, taking care to place all cables above the glass wool so the
protective coatings would not melt.
Initially, a CN/Si cleanup procedure (Method A) was employed and
recoveries of these 29 compounds were Similar to the other two extraction
methods discussed. Two disadvantages, however, caused the abandon-
nient of this approach. First, the dibenz[a,j]acridine did not recover frorn
the silica gel cleanup. Second, the injection port liner required frequent
chanOng to retain calibration of the instrument. In an attempt to obtain
a "cleaner" extract for injection, the ACN (Method B) was developed
and analyze recovery for the Laboratory Control Standard (LCS) and

a A. 1 Kilc•ch et al.
.n .. _..5: +.:� � i�,! .•:ti-/:7t�1-1!\i4.'. !i+:..d:; _iit.. t: .r. . _ 't': -t�: tf;• !.. •-
- il.t•.• II�`�I..i 1�.
z. �'`•LZ:1 :C:- 1 '►��:1• rtc#Y* ir-i 14.ilij ji1"' -1111
t' t::1 �.•Irl 1/�Gt4i .:. i,:iir"1 T:.+i:tra' 1 :.r. ;.u:i, ;t:_. S It+te;.•,
:Nn:•
i
i
i
f
r:: � f �� .;tiff � �• � l��i, r'� _
.41M
• �.`.
FIGURE 2. A chromatogram of paving sample 2. The complexity of asphalt
analysis is evident. This injection is of the DMSO extract, which is even
cleaner than the corresponding ACN extract.
Duplicate Control Standard (DLCS) are listed in Table 1. These control
standards are spiked with a solution of standard reference compounds.
This was performed in duplicate to obtain replicability data. Sample ma-
trix and duplicate matrix spikes are also provided in Table 2 and show the
difficulties of recovering the mass 302 compounds. This method elimi-
nated the need to run two separate fractions, since the benz[aj]acridine
survived this extraction procedure. The injection port liner, however,
still required frequent changing to retain calibration. Third, the DMSO
Method C was evaluated and tuned out to yield the best extraction ap-
proach for this matrix and these analytes. The advantages of the DMSO
extraction over the first two methods attempted are twofold, but related.
First, the injection port liner did not require as frequent a change as
when the CN/Si (Method A) or ACN (Method B) were used. Second,
the aliphatic background of the asphalt matrix was greatly reduced and
apparent in the chromatogram, allowing better detection of the com-
pounds in the samples. Recoveries comparing the DMSO (Method C)
and ACN (Method B) PAC fortified sample results are similar and shown
in Tables I and 2. The mean of the relative percent difference is 23.3
for the DMSO preparation and 9.9 for the ACN preparation for the lab-
oratory control standards and 10.4 (DMSO) versus 15.8 (ACN) for the
asphalt sample spikes.

1
'f':ABLE I. Comparison ut'"-b Reco%eries from LabaratOl-V C'untrul Stctndards
Taken throuch Txvo Diftcrent Extraction Procedures
t Method C) I Niethktd I31
REC REC % REC REC
EPC'RA section 313 compounds l-CS DI -CS RPD LC'S Dl_C S RPD
Fluoranthene 59.7 68.5 13.7 76.3 06.8 13.3
Benzo[a]anthracene 76.4 87.1 13.1 75.1 71.9 4.4
Chrysene 78.6 93.4 17.2 73.9 71.7 3.0
5-Mcthylchrysenc 83.0 92.7 11.0 74.1 69.6 6.3
1-Nitropyrene 90.8 124.5 31.3 85.7 75.3 12.9
Benzo[h]rluoranthene91.8 101.1 2 1. 1 79.1 78.3 1.0
7,12-Dimethylbenzlalanthracene" 204.0 297.9 37.4 32.6 44.3 30.4
Benzo[a]pyrene 89.2 93.1 4.3 78.3 76.7 2.1
3-Niethyleholanthrcnc 63.2 39.1 25.1 71.0 63.8 10.7
Dibenz[a.h]acridine 87.9 94.3 7.0 82.1 82.1 0.0
Dibenz[a j]acridine 82.6 94.3 2.0 83.1 87. 3 4.9
Indeno[ 1,2,3-calpyrene 80.0 94.9 17.0 79.6 77.3 2.9
Dibcnz[a.h]anthracenc 85.9 92.6 7.5 82.2 79.1 3.8
7H-Dibenzule,glcarbazole 19.3 2.4 156 131.1 89.0 38.3
Benzo[g,h.i]perylene 83.6 91.5 9.0 77-4 80.7 4.2
Dibenzo[a,I pyrene 99.8 86.6 3.6 66.9 61.1 9.1
Dibenzo[a,elfluoranthene 86.3 83.2 3.7 80.3 79.0 2.9
Dibcnzo[u.e]pyrcne 83.8 73.9 12.6 93.2 76.6 8.3
Benzo[l;s.11pentaphene 80.2 48.0 49.1 90.8 73.0 21.7
Dibenzo[a,h]pyrenc 65.4 51.1 24.5 86.0 71.9 17.9
Average 83.6 90.5 23.3 79.4 73.7 9.9
Average excluding compounds in bold 77.2 79.6 22.6 81.9 75.3 8.9
Abbreviation: RPD, relative percent difference.
"The h. j. and k isomers are not resolved and reported as a mix of Benzo[h]fluoranthcne.
"Chromatographic coelution problems with 3 isomers of 252 mass affect precision and accuracy.
Three of the mass 252 compounds are not resolved and the 7,12-
dimethylbenz[a]anthracene elutes among them, which sometimes causes
quantization problems. A different chromatographic column should help
to alleviate these complications.
Sample results for the raw asphalt (DMSO extraction) are listed in
Table 3. Roofing asphalts show the sum of all 29 PACs to be between
4.0 and 23 mg/kg (ppm), with a range of 2.4 to 19 mgr'kg for the
EPCRA listed compounds. This includes benzo[g,,h,i]perylene which
must be reported separately. Neat paving asphalts show the sum 01-
all 29 compounds to be between 1.9 and 66 mg/kg and a range of'

TABLE 2. Comparison of Recoveries from Matrix Spikes and Matrix Spike Duplicates Using DMSO and ACN Extracti011s
Roofing C Roofing 13
% REC ?,,, REC % REC % REC Average "t-I REC ';(, REC RI:C I', REC Average
DNiSO
MS
D!%'ISO
%,ISD
DN1SO
MS
DMSO
MSD
DMSO
recovery
ACN
MS
ACN
MSD
ACN
?v1S
ACN
!vISD
ACN
reemcry
Fluoranthcne
71.7
65.8
76.9
76.7
72.8
68.8
70.9
62.7
64.9
66.8
Belmlcrjantlu-acene
79.8
81.4
91.4
87.9
85.1
74.7
82.3
74.9
76.",
77.2
C-'hrysenc
81.8
79.6
92.8
93.8
87.0
73.4
78.4
73.6
69.0
7:.6
5-Methylchryscne
78.5
83.3
87.1
94.4
95.8
73.7
96.7
74.0
7 ".1
76.9
1-Nitr•onyrene
71.3
99.9
45.3
42.8
64.8
30.0
39.2
79.5
65.4
53.5
Benzolhllluoranthcnc"
80.7
S3.1
89.9
91.3
80.3
69.1
77.9
70.4
b7.9
71.
7,12-DinicthylbenzialanIbracene''
201.2
225.6
192.7
205.9
206
19.3
18.3
17.1
2(l.1
18.7
Benzo(ulpyrene
85.8
82.0
90.6
82.7
85.3
62.8
80.4
56.3
5 7.4
64.2
3-Mel hylcholmillirenc
32.0
52.3
82.3
76.2
60.7
44.7
46.8
47,0
49.5
47.0
Dibenzla,hjacridine
82.2
82.9
68.4
60.4
73.5
40.1
55.1
50.6
46.5
48.1
D'sben z(a,/'jacriditic
71.5
69.7
53.7
45.8
60.2
44.8
51.2
51.3
45.3
4.9,2
lndeno(1,2,3-ctjpyrcnc
76.7
76.4
37.7
57.8
62.2
43.5
50.6
44.1
37.6
44.0
DibenzIu,hjanIIiracctie
84.3
78.1
75.2
68.5
76.5
54.1
52.3
53.9
48.3
53.?

71-f-Dibenzole,gIcarbazole`-
3.S
3.0
11.5
9.0
6.7
57.8
58.7
97.8
78.2
73.1
Bcnzo[,U,h.j]perylcnc
79.4
71.1
50.3
67.5
67.1
34.2
42.5
35.9
32.5
36
l�ibcnzct(n.j]pyrenc
G2.4
?C.9
6G.0
59.(i
61.2
25.1
29.2
27.2
?3.;
2o.2
Dibenzo(u.e]fluoranthene
42.9
42.1
47.1
41.5
43.4
18.2
21.7
25.7
18.5
21.i1
Dibenzo[melpyrenc
36.2
33.9
45.1
40.4
38.9
17.1
22.3
21.9
1 i.5
19.2
13ct170[1:.c./]pesltapltcne
25.4
24.6
26.8
24.0
25.2
15.3
26.9
14.1
10.5
16.7
Dihcnzo[rr.h]pyrene
21.6
23.8
25.9
28.2
24.9
12.6
18.3
15.7
10.9
14.4
Average
68.7
47.4
Average excluding compounds in bold
61.4
48.9
Abbreviations: NIS, matt -ix spike; MSD, nuilrix pike duplicate.
"The h..j, and k isomers arc not resoived and arc reported as a tnix of Bcnzo(h]fiuuranthcnc.
"Chromatographic coclution hrohicnss with 3 isomers ol'252 mas% afTed precision and accuracy.
Low recoveries fix this compound are more apparent in the DMSO cxtruction compared to the AC N extractiun.

i2ti 1..I. Kric-c h (,I ell
(ABLE 3. Raw Asphalt Results (mg;I:g}- Four Etoufin��,:lici Six
Paving PAC's
Not tin LPC'RA .,cction 313 list
A
Roc 1liOIL,
!3 i • 1)
- �
Ri ine
3 1
0
Naphthalene
< 1
< 1 <-1 < 1
.-I I
t1.6A - !
I < t
list.
Acenaphthylenc
<!
: I < I - I
_ 1 I
; I i
: I - I
Acenaphthalene
< I
<: I : l < I
: l :1
< 1 ; 1
< 1 <r I
Fluorene
1.2
0.56 < 1 < 1
1.1 -.:1
-. 1 1.8
< 1 0.79
Est.
E.S1.
Phenanthrene
1.9
1.1 0.74 1.0
9.9 1.7
1.2 30
< 1 9.3
Anthracene
r I
< 1 < I < 1
1.1 ; I
< 1 1.5
-: 1 < I
Pyrenc
0.86
< I < I •< 1
3.1 0.64
< 1 9.1
< 1 1.9
Est.
Est.
EPCRA section 313 list
rluoranthen<
< I
< I
< 1
r 1
0.75
<:1
< I
< l
< I
< I
Est.
Benz[a]anthracenc
0.76
1
< I
<.1
1.3
< I
•: l
2.0
-. t
0.96
Est.
Est.
C'hrysene
9.5
2.2
1.8
2.4
6.5
3.2
< 1
12
2.9
4.3
5-Methylchrysene
3.5
0.72
0.82
0.94
2.8
1.1
< 1
9.2
<-1
0.75
Est.
Est.
Est.
Est.
-Nitropyrene
< 1
< I
< I
< I
.: I
< I
< I
: I
< I
< I
Benzo[b]flauranthene
1.0
< 1
0.62
< 1
1.5
< t
< 1
0.74
•< I
<. I
Est.
Est.
Benzo[ j)fluoranthene
< I
< I
< 1
< I
< I
< I
< I
< 1
<: I
< I
Benzo(k)fluoranthene
< 1
< I
< I
< 1
< 1
< I
< I
< l
< I
-, I
7.12-Dimethylbenz[ul.tnthracene
< I
< I
I
< 1
-. ;
•: I
< 1
-: I
-: I
< I
Bcnzo[u)pyrcne
< I
< I
<. I
< 1
3.7
< I
< I
< 1
:. I
0.34
Est.
3-Methylcholanthrene
<: l
< I
< 1
< 1
7.8
< I
< !
,:1
< 1
< !
Dibenz(u.h)acridine
< l
< I
< 1
< 1
< 1
: !
< I
I
<. I
<. I
Dibenz[a j]ucridine
< I
< 1
< 1
< I
< 1
< I
< I
< I
-- I
< I
Indeno[ l ,2,3-rd1pyrene
< I
< 1
< 1
< !
< I
< 1
< I
< 1
< I
< I
Dibenz[a,h)anthracene
0.59
< I
< 1
< 1
< 1
< I
< I
: l
< I
< I
Est.
711-Dibenzu[c g)carbazole
< I
<. I
< I
< I
<- I
: i
< 1
: I
< I
:- I
BenzoLg.hj]perylene
1.4
0.65
< 1
0.89
2.4
< 1
< 1
< 1
1.0
< 1
Est.
Est.
Dibenzo[a,npyrene
< I
< l
< l
< I
< 1
< I
< I
< I
.-1
< I
Dibenzo(a,e]Huorunthene
< I
< I
< 1
< I
< 1
< i
< I
: I
< I
< I
Dibenzo(u.elpyrene
< l
< 1
< I
< I
- 1
< 1
< I
: I
I
< I
Bcnzo[r.mjl-wmaphene
< I
< I
<. I
< I
; I
: I
- I
- I
; I
< I
Dibenzo[o.lt]pyrene
< I
- I
<. I
< I
-: I
< I
< I
=: I
< I
< 1
Total of 29 PAC's .
23
4.1
4.0
5.2
43
6.6
1.9
(,6
.j.9
19
detectables only
Total of FPC•RA list only
19
2.4
3.3
4.2
2K
4 Z
NI)
24
39
6.5
Abbreviation: Est., estir rates. detectablc but bcl,)%v calibration.

nondetectable to 28 Ing/kg for the FPC RA list. Since the samples had
been taken through two different extractions, these results were com-
pared and show (food agreement. The primary detectable compounds of
benz[a]anthracene, chrysene, and 5-methylchrysene are listed in Table 4
showing these comparisons. The 3-tnethy1cholanthrene «vas detectable
in only one sample, but its mass spectrum was a good match. The M- I
ion at 267 was 34% for the standard and 37"Xi f'or the sample. Also,
the 253 ion was 53% and 49% respectively. Quantitation of this com-
pound may be skewed high, as there were shoulders on both sides of
the peak. The presence of 3-methy[cholanthrene is not understood, since
3-methylcholanthrene is a synthetic compound and therefore not likely
to be in the neat asphalt.
Structures for these 29 PACs are readily available in the literature
(16). Their presence in the neat asphalt and leachability appear to be
varied with different types of asphalt. Three of the 252 mass com-
pounds are not baseline resolved and are integrated as one peak re-
ported as benzo[h]fluoranthene (j and !, isomers included). The 7,12-
dimethylbenz[a]anthracene (mass 256) elutes at a similar retention time
and chromatographic problems are evidenced in the recovery data. The
7H-dibenzo[c,g]carbazole was also problematic. Recovery of the mass
302 compounds dropped off with all three: methods of extraction and
seemed to vary depending on which sample was spiked. The sample
extracts ranged in color from light yellow to pink and varied in intensity
as well as PAC concentration.
Little data on these PACs in asphalt are found in the literature to
compare with the data in this study. Malaiyandi et al. showed results for
only a subset of this list detennined by HPLC (17). Even though HPLC
with fluorescence detection is a sensitive analytical technique, HPLC
suffers from two problems. One is that matrix problems with complex
mixtures such as asphalt may lead to high reported values. Second,
it is difficult to verify the identity without a spectroscopic technique.
Analysis of the leachate samples by HPLC would be suitable, since the
chromatograms are relatively clean. For asphalt, however, the complex
background inhibits the identification and quantification, which could
easily be in error using HPLC. .
Leachate results are presented in Table 5 for the 10 asphalt samples
tested. Results for all 29 compounds are below the regulatory limit, with
only two results above the detection limits of 0.1 ppb. A few samples
contain results reported as estimated data (detectable but below the cal-
ibration). One sample (Paving 3) had a result of 0.18 �tg/L (ppb) of
naphthalene. Another sample (Paving 1) had 0.1 pg/L of phenanthrene,
which is right at the detection limit. All four roofing samples and three

P
TABLE 4. Sample Results (mgAg) Comparing Both the DMSO and ACN Extraction Procedures
C'umpound DMSO ACN DMSO ACN DMSO ACN DNISO ACM DMSO AUN
PO 64-22
Roofing A Rooling 13
Roaring C:
Rooting D
Bun/jaj.uitluacenc
0.96 < 1
0.76 0.88 ---
C:hrysene
3.6 2.6
9.5 7.9 2.2 2.2
1.8 1.6
2.4 1.7
5-7.v1cthy1c1uryscnc
1.2 1.0
3.5 2.5 0.72 < 1
0.82 1.3
0.94 ,• I
Paving I
Paving 2 Pavino 4
Paving 5
Paving 6
Bcnz(a janthcaCelle
1.3 2.9
- -
_
0.96 < I
C hivscnc
0.5 7.0
3.2 3 12 16
2.9 3.5
4.3 3.2
5-Mcilivlchrysene
2.8 5.5
1.1 1.7 9.2 11
-•-
0.75 1.9

11
1���lNr;l►%milioil uJ /'.1 CS lt► _ J yllf;h
TABLE 5. Quantification lots, Retention Times. and Leachatc itesult: f01-
Docctable Samples
Relative PAC riot an
order of 1:PCRAsection Quant. Retention
elution 1131 list ion lime (min)
Paving Pavia;;, Paving
1 ? 4
(mg4iter)
I
Naphthalene
128
0.67
<0.1
0.18
<0.1
?
Acenaphthylene
152
12.11
<0.1
<0.1
<0.1
3
Acenaphthalene
154
12.69
<0.1
<0.1
<0.1
4
Fluorene
165
14.15
<0.1
<0.1
<0.1
Phenanthrene
178
16.66
0.1
<0.1
0.06
Est.
6
Anthracene
178
16.76
<0.1
<0.1
<0.1
9
Pyrene
202
20.20
<0.I
<0.1
<0.1
EPCRA section 313 list"
7
Fluoranthene
202
11.02
<0.1
<0.1
<0.1
9
Benz[u]anthracene
778
14.39
<0.1
<0.1
<0.1
10
Chrysene
228
14.50
<0.1
<0.I
<0.1
II
5-tilethylehrysene
242
15.54
<0.1
<0.I
<0.1
12
I-Nitropyrene
247
15.65
<0.1
<0.I
<0.1
I3
Benvo[h]fluoranthene
252
16.81
<0.1
<:0.1
<0.1
14
Benzo[ j]fluoranthetic
252
16.81
<0. I
<0.1
<0.1
I
Benzo[k]fluoranthenc
252
16.81
<0.I
<0.I
<0.I
16
7.12-131tnethylbenz[c;]-
256
16.89
<0.1
<0.I
<0.1
anthracene
17
Bcnzo[ajpyrene
252
17.47
<0.1
<0.I
<0.I
18
3-Methylcnolanthrene
268
18.26
<0. I
<0.1
<0.1
19
Dibcnz[u.h]acridine
279
19.39
<0.1
<0.1
<0.1
20
Dibcnz[u.j]acridinc
279
19.48
<0.1
<0.1
<0.1
21
Indeno[1.2,3-cxdlpyrene
276
19.87
<0.1
<0.1
<0.1
22
Dibenz[a,h]anthraccnc
278
19.92
<0.1
<0.1
<0.1
23
7H-Dibcn7o[c,glcarba7ole
267
20.39
<0.1
<0.1
<0.1
24
Benzo[ .h.rlperylene
276
20.45
<0.1
<0.1
<0.1
25
Dibenzo[u.l]pyrcnc
302
23.53
<0.1
<0.1
<0.1
26
Dibcnzo[a,e]fiuoranthene
302
24.57
<0.I
<0.I
<0.1
27
Dibenzo[a.elpyrene
302
24.64
<0.i
<0.1
<0.1
28
Bettzo[,:s,i]pentaphene
302
24.96
<0.1
<0.1
<0.1
29
Dibenzo[a.hlpyrene
302
25.20
<0.1
<0.1
<0. I
\'n;c,. All four roofing asphalts were nondetectable (ND) for all 29 compounds. 'rhree or six
pay Zug asphalt samples were also ND.
" \ separate analytical limeram was designed for thla list.

5 32 : 1-1 kt'1 t'd h c/ (it'.
TABLE 6. Learhate Recovery Data ltlr FPC'RA Section
313 C'ompoutids
EPCRA section 3 13 compounds
LCS
DLCS
"4, RPD
Huoranthene
95.4
86.7
9.5
Ben7(0]anthracene
96.9
101.7
4.8
Chzysene
96.6
94.3
2.4
5-Methylchtysene
101.5
103.1
13
1-vitropyrcne
101.8
141.3
32.5
Benzo[b]fluoranthcnc - other isontiers
98.8
95.8
0.3
7,12-Dimethylbenz[u]anthracene
83.5
88.4
5.7
Benzo[u]pyrene
101.6
103.2
1.6
3-Mcthyleholanthrene
100.1
110.0
9.4
Dibenz(a.h]acridine
94.1
98.9
5.0
Dibcnz[a j]acridine
93.9
102.2
83
Indeno[ 1.2,3-calpyrene
95.0
99.1
4.2
Dibenz[a,h]anthracenc
93.1
100.7
7.9
7H-Dibenzo[c•,gjcarba7o1e
111.2
121.E
8.9
Benzo1g.0]petylen:
93.1
93.9
0.7
Dibcnzo[a.1]pyrene
86.9
102.8
16.8
Dibenzo(ax]fiuoranthene
90.1
107.8
17.9
Dibento(o.elpyrene
88.2
102.9
15.4
Benzo[rs.t]pentaphene
88.1
103.7
16.2
Dibenzola.h]pyrene
84.4
108.5
25.0
Average
94.7
103.3
9.7
The LCS was spiked at 2.0 u.L,,'L and the DLCS spiked at 4.0
of six paving samples showed no trace of any of these PACs. None of the
EPCRA 22 PACs were found in the leachate of any asphalt. Recoveries
within a leachate matrix laboratory control standard (LCS) are shown in
'Fable 6.
Excellent recoveries and repeatability for most compounds are demon-
strated, with the relative percent difference (%RPD) being under 20%,
for all compounds except I-nitropyrene, which showed 141.3% recov-
ery for the Duplicate Laboratory Control Standard (DLCS) and a 32.5%
RPD. Eight of the traditional 16 PAH compounds not within the EPCRA
section 313 list were also tested for recoveries and repeatability with all
results between 101.211'0 and 124.6% recovery and RPDs all below 501(,.
Results for the leachate samples are consistent with previous data
(5-8), although data for the bulk of the EPCRA section 313 list has not
been previously studied in asphalt or their leachates.
Finally, the ttse of GC/MS/MS to validate the presence of these low
levels was pursued. The GUMS mass spectra were sometimes not

19
TABLE 7. GC/MS/MS Results on Selected Masses (m,rikg)
Mass
Compound
Roofing A
GC/M5 h1S GOIMS
Paving 1
GC'/MS-Y1S GUMS
Paving 4
Oc"MS/MS GCNIIS
?28
Benz[a)anthsaccne
0.94
0.76
3.9
1.3
2.8
2.0
228
ChrYscnc
4.9
9.5
8.5
6.5
12.0
12.0
252
Benzo[b]tiuroallthene
0.92
1.0
1.9
1.5
+
0.74
252
Berszo[k]fiuorantilcnc
-
< 1.0
1.5
< 1.0
+
< 1.0
232
Benzo[a)pyreslc
<0.5
< 1.0
3.4
3.7
+
< 1.0
276
Indeno[ 1,2,3-ccl] pyre nc
0.40
< 1.0
2.5
< 1.0
_
< 1.0
278
Dibenz[u,hjatlthracene
0.75
0.59
-
< 1.0
-
< 1.0
276
Benzo(g.lU)pctvlcnc
1.9
1.4
3.2
2.4
0.38
1.0
4-, Detectable but not quantifiublc; -. Nondclecttd.

C-
;4 A. I Knt' h (�t u/.
definitive when concentrations were too low relative to the background.
The GCi`MS.:MS teclmicltte improx ed the sensitivity by a factor of about
10 for the masses investigated, providing more definitive confin-nation
for the presence or absence of some of these PACs. Using this technique,
Roofing Sample A and Paving Samples I and were further investigated.
Results show good agreement with the MS data both qualitatively and
quantitatively and are shown in Table 7.
CONCLUSIONS
Recovery of 29 environmentally relevant polvcyclic aromatic com-
pounds from leachate waters is excellent using traditional liquid/liquid
extraction (Method SW 846-3510C), with trace levels of naphthalene
and phenanthrene in 3 of 10 samples. None of the compounds on the
EPCRA section 313 list showed evidence of leachability from the as-
phalts tested. None of the roofing asphalts tested leached any of the
29 compounds. The two paving asphalts that do contain detectable levels
of naphthalene and phenanthrene are well below drinking water limits.
Determination of these compounds in the raw asphalt is, as expected,
much more challenging. All three extraction procedures yielded simi-
lar recoveries, however the DMSO extraction (Method Q provides the
least interferences in the analysis of these 29 PAC compounds. The an-
alytical method described here for the nontraditional list of these PACs
works well to provide quantitative recoveries of these higher -molecular -
weight compounds. GC/MS/MS analyses provided verification of some
compounds that were too low to obtain a confirmatory mass spectrum.
FUTURE RESEARCH
Although none of the EPCRA section 313 compounds appear to be
leached from asphalt, literature findings show release of some of these
PACs at extremely low levels during the application of hot mix asphalt
(18). Collection of data for these same compounds within asphalt fumes
from field applications is a key component to their environmental release
requiring additional study.
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