NC0031046_COMPLIANCE_20030908

NPDBS DOCUMENT SCANNIN& COVER SHEET
NPDES Permit:
NC0031046
Document Type:
Permit Issuance
Wasteload Allocation
Authorization to Construct (AtQ
Permit Modification
Complete File - Historical
�CCompliance
Speculative Limits
Instream Assessment (67b)
Environmental Assessment (EA)
Permit
History
Document Date:
September 8, 2003
This document is priaited on reuse paper - igpnore ariy
ooateat on the reverse side

F�ad:.RC: Colonial Pipeline
Subject: Fwd: RE: Colonial Pipeline
Date: Mon, 08 Sep 2003 12:25:41 -0400
From: "Mary Thompson" <[e-mail]>
To: <dave.gooch-ich o ncmail.net>, <joe.corporon@ncmai].net>
CC: <[e-mail]>
Dave and Joe,
Please read the attached e-mail from Rick Gaskins, opposing counsel, and let me know if we can agree to
one of these procedures. It seems the 2nd procedure could be handled by a condition in the Settlement
Agreement until permit renewal time. I've cc'd Karen so she can see that he's agreed to the settlement on
the civil penalties, but there may be a delay due to this permitting condition question.
Look forward to hearing from you soon,
Mary Penny
Mary Penny Thompson
Assistant Attorney General
Environmental Division
N.C. Department of Justice
P. O. Box 629
Raleigh, NC 27602-0629
[phone] / main phone
[phone] / direct dial
[phone] / fax
[e-mail]
Subject: RE: Colonial Pipeline
Date: Mon, 8 Sep 2003 12:21:10 -0400
From: "Gaskins, Richard C." <[e-mail]>
To: "Mary Thompson" <[e-mail]>
Mary Penny -
Thanks for your response. The proposal that you have outlined is generally acceptable if we can obtain
some clarification about how the issue will be handled in the future. Because this issue is likely to arise
again in the future, we need to have some agreement about future sampling for phenol and we can't simply
postpone the issue until the next permit is issued. We propose that either:
.0,
1. The requirement to sample for phenol be removed from the permit because there is no evidence that
there is a reasonable potential for Colonial to have phenol in the discharge; or
2. We agree to a procedure for sampling for phenol that involves testing regularly for total phenolics and
doing the analysis for phenol only if there are total phenolics in excess of some agreed upon level.
Please let me know if this is acceptable and 1 will draft something up. If I don't hear back by the end of the
week, I may need to serve some discovery due to the upcoming OAH deadlines.
I ot2 9/8/03 1:57I'M

Fwd: RE Colonial Pipeline
- Rick
-----Original Message -----
From: Mary Thompson [maiIto: [e-mail]]
Sent: Thursday, September 04, 2003 2:15 PM
To: Gaskins, Richard C.
Subject: Colonial Pipeline
Dear Rick,
My client has confirmed that the current permit addresses the single compound of phenol, not
all phenolic compounds. With this clarification, DWQ is willing to rescind the NOV for LV
02-618 (the first civil penalty which was remitted entirely). That should resolve all issues on
that enforcement action.
On the second civil penalty, LV 03-225, DWQ cannot simply rescind the NOV and CPA b/c
there were violations of other parameters. Would your client pay the remainder of the civil
penalty after the phenol amount is removed? If so, I propose we handle the resolution of the
second civil penalty through a settlement agreement that indicates the NOV and CPA portions
related to phenol are withdrawn and the remainder of the penalty is paid as settlement without
admission of liability for those alleged violations.
The detection of creosolic phenol in your effluent will be handled in the next permit renewal
which you or your client can discuss directly with the NPDES Permitting Unit (Dave
Goodrich and Joe Corporon).
I hope this moves us closer to resolution of this case. If you wish to discuss this matter
further, please feel free to reply by e-mail or contact me by phone (I'm available this afternoon
and Friday afternoon).
Sincerely,
Mary Penny
Mary Penny Thompson
Assistant Attorney General
Environmental Division
N.C. Department of Justice
P. O. Box 629
Raleigh, NC 27602-0629
[phone] / main phone
[phone] / direct dial
[phone] / fax
[e-mail]
2 0l2 9/8/03 1:57 PM

Colonial Pipeline Phenol issue
Subject: Colonial Pipeline Phenol issue
Date: Wed, 03 Sep 2003 18:23:45 -0400
From: "Maly Thompson" <[e-mail]>
To: <karen.rust@ncmai[.net>
CC: <dave.goodrich@ncmail.
Karen,
net>, <joe.corporon@ncmai].net>
If you will recall, there are 2 civil penalties against Colonial Pipeline for reporting phenol violations. The
first penalty was remitted entirely, but Colonial Pipeline wanted the NOV rescinded as well. DWQ's
NPDES Permitting Unit has clarified with Standards that the permit limit addresses the single compound
of phenol instead of total phenolic compounds and that the creosolic phenols being detected will be
addressed in a renewal. My recollection was that DWQ would be willing to rescind the NOV for the
phenol violation if this turned out to be the case. Are you still willing to do that?
If so, we can probably resolve the first civil penalty. In truth, there would be nothing left to challenge!
The second civil penalty will be a bit more difficult because there were violations for other parameters than
phenol. If you agree, I will suggest to opposing counsel that we handle the second civil penalty through a
settlement agreement. If we can't resolve the entire second civil penalty, DWQ may have to rescind the
NOV and reissue it without the phenol violation, which would also mean rescinding the CPA and reissuing
it without the penalty for the phenol violation.
Let me know your thoughts as soon as you can. If you want to verify the phenol permit limit information,
please feel free to contact Dave Goodrich or Joe Corporon (both are cc'd on this e-mail).
Thanks,
Mary Penny
Mary Penny Thompson
Assistant Attorney General
Environmental Division
N.C. Department of Justice
P. O. Box 629
Raleigh, NC 27602-0629
[phone] / main phone
[phone] / direct dial
[phone] / fax
[e-mail]
I of 1 9/5/03 10:49 AM

Fwd: Colonial Pipeline
Subject: Fwd: Colonial Pipeline
Date: Sun, 17 Aug 2003 11:54:37 -0400
From: "Mary Thompson" <[e-mail]>
To: <dave.goodrich @ncmai ].net>, <[e-mail]>, <[e-mail]>
Dave, Joe, and Karen,
Rick Gaskins, atty for Colonial Pipeline, wants an update on our activities - can we resolve the phenol
issue w/o a meeting, do we need to meet, or should we continue with litigation? I've attached Rick's and
my e-mails as a refresher on the issue. The last 1 heard, the Standards person was going to look into how
"phenol" should be interpreted. Let me know if you have any new info. If not, let me know your
availability to meet with Rick Gaskins and his client.
Thanks,
Mary Penny
Mary Penny Thompson
Assistant Attorney General
Environmental Division
N.C. Department of Justice
P. 0. Box 629
Raleigh, NC 27602-0629
[phone] / main phone
[phone] / direct dial
[phone] / fax
[e-mail]
Subject: Colonial Pipeline Status Report
Date: Sat, 16 Aug 2003 11:34:10 -0400
From: "Gaskins, Richard C." <[e-mail]>
To: "Mary Penny Thompson (E-mail)" <[e-mail]>
Mary Penny -
It is my understanding from our prior conversations that you were going to talk to the DENR staff
about whether this case could be resolved without a meeting, or in the alternative, a date when
we could meet with them for an informal settlement conference. I think that the rules obligate
DENR to sit down and discuss this matter with us. We need to have a meeting to settlement
settlement or get on with discovery. Please give us some proposed dates when we can meet to
discuss this matter. Please provide me with some proposed dates for a meeting (after September
5) or let me know if DENR is unwilling to meet with us.
- Rick
-----Original Message -----
From: Mary Thompson[maiIto: [e-mail]]
Sent: Monday, July 21, 2003 4:37 PM
To: Gaskins, Richard C.
I of 2 8/ 19/03 6:48 AM

Pwd: Colonial Pipeline
, ' Subject: Colonial Pipeline Status Report
Dear Rick,
Please look over the attached Status Report and let me know if you have any edits, especially
whether you want me to send it in as a joint status report or if I should send it as Respondent's
status report only.
Thanks,
Mary Penny
2 of 2 8/19/03 6:48 AM

ENR-ENVIRONMENTAL MANAGEMENT TISA: 02B .0200
Sedimentation Control Commission or approved local
government programs as delegated by the Sedimentation
Control Commission shall be limited to no more than two
dwelling.units of single family detached development per acre
(or 20,000 square foot lot excluding roadway right-of-way) or
24 percent built -upon area for all other residential and non-
residential development; Stormwater runoff from the
development shall be transported by vegetated conveyances to
the maximum extent practicable;
(B) High Density Option: If new development density exceeds the
low density requirements specified in Sub -Item (3)(b)(ii)(A)
of this Rule engineered stormwater controls shall be used to
control runoff from the first inch of rainfall; new residential
and non-residential development shall not exceed 50 percent
built -upon area;
(C) No new permitted sites for land application of residuals or
petroleum contaminated soils shall be allowed;
(D) No new landfills shall be allowed;
(c) Odor producing substances contained in sewage, industrial wastes, or other
wastes: only such amounts, whether alone or in combination with other
substances or waste, as will not cause taste and odor difficulties in water
supplies which can not be corrected by treatment, impair the palatability of fish,
or have a deleterious effect upon any best usage established for waters of this
class; r
folic -compounds: not greater than 1.0 ugA (phenols) to protect water
supplies from taste and odor problems due to chlorinated phenols shall be
allowed. Specific phenolic compounds may be given a t erent trait if it is
demonstrated not to cause taste and odor problems and not to be detrimental to
other best usage;
(, (e) Total hardness shall not exceed 100 mg/I as calcium carbonate;
(f) Total dissolved solids shall not exceed 500 mg/l;
(g) Toxic and other deleterious substances:
(i) Water quality standards (maximum permissible concentrations) to
protect human health through water consumption and fish tissue
consumption for non -carcinogens in Class WS-IV waters shall. be
allowed as follows: '
(A) Barium: 1.0 mgA;
(B) Chloride: 250 mgtl;
(C) Manganese: 200 ug/l;
(D) Nickel: 25 ugtl;.
(E) Nitrate nitrogen: 10.0 mg/1;
(F) 2,4-D: 100 ug/l;
(G) 2,4,5-TP (Silvex): 10 ug/l;
(H) Sulfates: 250 mg1l;
(ii) Water quality standards (maximum permissible concentrations) to
protect human health through water consumption and fish tissue
consumption for carcinogens in Class WS-IV waters shall be allowed
as follows:
(A) Beryllium: 6.8 ng/l;
(B) Benzene: 1.19 ug/l;
(C) Carbon tetrachloride.. 0.254 ugA;
(D) Chlorinated benzenes: 488 ugn;
(E) Dioxin: 0.000013 ng1l;
(F) Hexachlorobutadiene: 0.445 ugA;
(G) Polynuclear aromatic hydrocarbons: 2.8 ngA;
(H) Tetrachloroethane(1,1,2,2):0.172ug1l;
NORTH CAROLINA ADMINLSTRA--TIVE CODE-- 09/01/00 - ---Page 39

06/03/2003 16:51 9197339612
PAGE 01/12
Post -it' Fax Note 7671
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papoa►
COJDapt.
Co.
Dhow a
P one 3
08 US. I
ax4 -I I U - �elLou
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Suppork��S Jotoc u-mkr\ts ;row\
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Y0" f�, VA- a K 1 T;A es A'I\on,s
�avt.i<s.

06/03/2003 16:51 9197339612 PAGE 02/12
Colonial Pipeline Company (��J
Creating Eraellence it, 7r=Vortarion Servhxa
Fattoy D. LBO" Telephore: 33a�2 MWV
EnvWnlnentalTechnicie �Dsl FuuosYnile: ,3392924i482
Monday, January 27. 2003
F E 8- 5 20.03
teen Sect
Ater Quality epion chief o Aryl
1617 MailService CcWw
Raleigh, NC 27699.1617
,l1�1S` �AQ�.. D �o►14ya.
16N 1 9 2003
SUMECT: Notice of Violation and Assessment o7tf Civil Penalty Oil
WA t Ltd QUALITY � � Jpi� )jy
for Violation of NC General Staudt 143-215.1(n)(6) w SECTION 1n {iQv
and NPDES permit NCO031046 ' wt 1�
Colonial pipeline Gleemsbaro Ta'a tal t � o—
Coe No. LV 02-6is
Guilford County` rl
V� i)�
Colonial Piptllne company respcctlully requests msciision of the penalty issued on December 31, 2002 for the I parrot
vloiedon referenced above. The alleged exceedence was the rest* of a reporting eror 21 ootfa11001 for oairhdy 2002.mmlitminng
even. A mrekbl exarammion of the labofatorY data indicates that there was not an Elneeft a of the permit hauls for plsettol (ot:any
other compound)- we erroneously calculated pounds per day for phenol by using the total pbewlies coacoursdon of 11.8 utglL as
opposed to the phenol concentration of <5.3 ug/L or 9W-detecL This resulted io our reporting a pounds Per day etiaCharge of 0:031
pouwda. Since our permit limit at each cutfall is 0.0006 pounds par day, this led to a posit violation, A corrected dleobtage
monitoring report (DMR) for ootfall 001 for July 2002 is auachad and an explanation follows.
We generally analyze total phenolics using EPA method EPA 420.1. This method is much more ocorwmical than method EPA 625
but, instead of just the add faction, it picks up all the other phenolic compmuls as well. Hoeaase our permit requires somi-aanudl
monitoring for EPA 625 analyses, and since these are generally performed in January sad July, we were Somewhat fortunate that we
had results for phenol daring this mmutor)ag period. Ad WonaRy, a further review of ourLPA 625 seW- mnal monitoring resolts .
for the past six years confirm that there has been no detection of phenol at any of our outfalls during this timeefiname while these bave
been detections of total PlaWOR s, we are curradly working with our ieboratones and oar N VES regulators to develop a psocm
that allows for accurate doteaion of phenol without Henning a foil EPA 625 au each o tW each month
JE eonclusioa,. since there was no actual exceedenoe of permit critens, there was no viandon of the standard G.S 143-215. ](a)(6) and
NPDES Permit No. NC0031046. This conclusion a based on the provisions provided below.
1. tbere was no harm to the untnal resources of the State, to the public healib. nor to private properly;
2. then was no effect on ground or surface water quantity or quality nor on air quality,
3. f t= was no damage and, therefore, no cost 10 rectify.
TUA you for reviewing the attached connected DMR and for considering our request for roeoiasion As you probably kvow, we have
also tIIed a formal petition for review contesting the proposed administrative penalty. This letter is iniande d as an informal afteutm
resolve this issue and it is not intended as.a substinde for the petition for review and Colonial is not agreeing to waive nay of its rights
to appeal the proposed penally. we would appreciate it ifyou could respond to our request for rescission of the penalty as soon as
411 Ga hi @ Dahy Read Graarhera, North Camara 2740D

06/03/2003 16:51 S197339612 PAGE 03/12
powbie because it will be necessity for both DEN1t and Colonial to prepare &adinge and tatbr* d=mM to the Office of
Ad ative Hearings m connection with the formal appeal of the penahy. We believe that it is ih the best interest ofbothColonial
and OEM 10 rmotve this issue gWddy and thereby to avoid tmneces U work relating to dw tbrwat appeal. If you have g .,.or
reggae adfitioael jeformadon, please contact me at 336-294-9737 or at the letterhead addreac.
Siaclrely, •
Fly"" .D'LeigA
Md-AdamleEnvitonmenWly Ttxlm3eien
ATfACMAENT
cc; D.V.Pcarmw/altachmcxd
C—P. simaw/mmdtment
D.D. Titan w/atlachmatt
411 Gatimors Dairy Rose OreeneboM North Cerolmt 274M

\\ 0G/03/2003 16:51 9197339612
PAGE 04/12
Per'tnit NC0031046
A I. IEFFLUENT LIMITATIONS AND MONITORING REQUIREMENTS
$cg(nrdng on the effective date of the permit and lasting until expiration, the Permittec'is authorized to
discharge from Outfall 001. Such discharges shall be limited and monitored by the PEmnittee as
specified bch)w:
EFFLUENT
CHARACTEWnCS,
LIMITS
MONITORING
RE i1IREMl3N'1`$.
Monthly
gaily
Meawrement
saioapla
sampl.
Average
Maximum'
uen
rt
Loea on
Flow t
Episodic
I.-
Effluent
Total Sumended.Solids
t}��z
45.0 m
30.0 me/L
MOVIthil
Monthly
b '
Grab
t
Effluent.
;
0.0006)bsJdav,
Monthly
Grab
E OR
.Phehol
B
Monthl I
Grab ..
Effluent -
Monthly
b
Effluent
.Toluene
E Bettzerta
Monthly
Grab
. Effluent
.1
X lens
Monthl
CkAb
Effluent
EPA 625
7/Year
©rati
Eiilueni
MIB
Monthly
Grab.
Effluent
Annually
Grab
}sf�laent
Acute Toxlci
1. Flow — During periods of no flow, the Permittee shall submit a monthly Discharge Monitoring
Report (DMR) indicating "No discharge." Flow shall be monitored with each discharge event
and may be monitored in one of four ways:
a. measure flow continuously;
b. Rational Method — calculate flow based on total rainfall per area
including built -on area draining to the outfall (This method shall not be
used at sites with large runoff -collection ponds);
c. estimate flow at 20-minute intervals during the entire discharge event; or .
d. report flow based on discharge pump logs.
2 Oil and Grease —Where possible, the grab sample for oil and grease should be skimmed from the
surfscc of a quiescent (calm water) zone.
3. MTBE — see Special Condition A. (7.) for other requirements relating to WMF-
4. Acute Toxicity (Fathead Minnow. 24-hour). Annual [see Special Condition A. (A.)].
Units: mglL = milligrams per liter
µg/L = micrograms per liter
MTBE = methyl tertiary butyl ether
Ibs/day - pounds per day
The Permittee shall not discharge floating solids or foam visible in other than trace amounts.
The Permittee shall not discharge tank solids. tank bottom water, or the tank rag layer.
The Perinittee shall not discharge tank (or pipe) contents following hydrostatic testing unless benzene
concentration is less than 1.19 jig/L. and toluene concentration is less than 11 Ag/L..

06/03/2003 16:51 9197339612 PAGE...05/12
of h rostatie test water if
3d benzene and/or toluene concentrations exceed their respective water
quality standard (2001 SOP, Parts LG. and LH).
Phenol — Monitoring and Limits Calculations. When combined with chlorine, phenol can cause
taste and odor (organoleptic) problems in drinking water, and can also result in the tainting of fish
tissues. Therefore, in accordance with SOP 2001, all dischargers to state water suppir (WS) waters
shall conduct fnouthly effluent monitoring for total phenol. Moreover, if analytical.results suggest
`reasonable potential' a phenol limit shall be included in the permit.` _
A phenol limit magnitude depends on dilution. Ideally dilution would be calculated at the Flip Point '
Dam water plant intake where chlorine is la7oduced, but it is impractical at this time to measure
dilation under lake conditions at the intake. Therefore, the Division calculated flow at the. assumed
headwaters of this water supply. Secondly, the Division used 1 µg/L (the aesthetic limit tar phenol) to
— ealeulate a wasteload allocation in pounds per day (ibsJday) at these beadwaters.' Finally, the•
wastdioad allocation was. distributed equally among phenol dischargers as a permit limit only as each
facrTlry's data -set showed reasonable potential to exceed the water quality stream standard .
Cntrwrtly nine (9) bulk storage facilities discharge to either the East Fork Deep River or long.
Branch. The oonfluertce of these two drainages was assumed to approximate die headwaters of High
Point Lake, the nearest downstream intake waterbody. For purposes of yield calculations. Long
Branch was assumed to have a similar runoff coefficient as the East Fork of the Dull River. The'
Division used published 30Q2 flows from an EPA stream gauge (02099000) located on the Rest Fork
Deep River near the confluence of the two drainages. The 30Q2 flow, not the 7Q10, was deemed'
appropriate because of -the aesthetic standard for phenol.
Flow Calculations:
Given: Flow (30Q2) East Fork Deep River — 3.8 cfs (USGS Gauging:Statia n)
Drainage Area Fast Fork beep River = 14.8 mi' (USGS)
Drainage Area Long Branch 3.94 mil (measured from t]SGS topo)
Total Drainage Area : 14.8 mi3 + 3.94 mi'
18.6 ml'
Yield East Atnk Plow (ors)
East Fork Drainage Area
= 3.8 cfs
14.8 mi
= o.257 cfwmit
Thcrefore:
Total Flow a Yield x Total Drainage Area
0.257 cfs(mi' x 18.6 mi'
4.7 do
Wast9lead Calculation:
4.7 46 x 0,001 mg/L x 8,34 = 0.025 IbsJday distributed among trine
1.55
dischargers
0.025 lbs./day
9 dischargers
i
FaCt Shoe. '
RmewN--NPp FiY "�CfK131(}l0
- Pugc 4 .

06/03/2003 16:51 9197339612
PAGE 06/12
0.003 lbsJday per diseberger
'Note: this allocation will be distributed equally among all oatfalls showing "reasonable potential' for
pgenol.
Outran 001 Maximum slow: 0.1728 MGD (forOutfall:001)
phenol Limit Example:
Limit = pllaWed wasteload tlba./davl x ���g�ted Fldw (MG1))
8.341bsJMG
3 .003 bs.AUz �--
8.34 0.1728
0.00208 M91L
= 2.08 µglL
SntnmarY of Reasogable Potential Analysts (RTA). The Division conducted the EPA-nfan&ied
repotted data for six outfsUr. The RPA compares the "allowable
RPA on Colonial Pipeline's ftdittOd" Concentration
corlcenirstion" (based on water quality standard or criteria) the "nnaxlmum p
based on data submitted (1996 jhroagh June 2001). RPA results for phenols and ber=c, toluene,
ters are summarized per outfali in Tables
ethyl'betuene, and xy1'ene (J3TEX), and oil & grease parame
4 through A
ND = not detected.
Fuct Shect
RCICIW .. NPDnS Nl7c%1110M.
PuF, 5

of
NEMVI
oft

16:51 9197339612
Analytical"
wmw.Peoeleea,00m
.Lab Sample Nos 922419692
Client SaNale TD: Kim Got
Project Sample
PAGE 08./12
OeeeAnehdlwl8erpise4, lee:
99W MCOy.AveaLie, 6V#p 190
Hunreaw* HC,23D76 ,
Dhow: 700.87SAm
Lab PMJeet flusher: 2236047 Iox. 04.875.wpf!
Client Proiett ID: &eenshoro WM :�•:
Matrix: Water Date Received: 07/90/02
RRralkers
Results Units Report Limit Arelraed 9v
en No. (yj,L B"
Wet Chemistry
Total Suapehded solids
Method:
EPA 160.2
Total Suspended solids
12,
mg/7
2.5
07/31/02 AST
(1C/9 SetDivolatiles
Exeractables in Water by 525
Prep/Method: EPA 625
tr / EPA 626
N- Ntsroaodlamthyl Gal ne
ND
ug/1
6.3
07/31/02 23:22 RPJ
62.75.9
bis(2-Chloroathyl) ether
ND
ug/1
07/31/02 23:22 RPJ
311,44.4 '
Phenol
ug/1
6.3
07/31/02 23:Pt RPJ
308-*4
2•Cfiloraphergl
ug/i
07/31/02 23:22 RPJ
ti5.67-0
1.3.Ofchlorobenzeke
MD
ug/l
5.3
07/31/02 23:22 RPJ
511.73.1
1,4.Oiehlorobenzene,
No
u9/1
6.3
07/31/02 23:22 RPJ
106.46.7
1,241chlorobenzenb
w
ug/1
5.3
07/31/02 23:22 RPJ
96.50.1
bis(2-Lk1eroisopropyl) ether
NO
ug/1
5.3
07/31/02 23:ZZ RPJ
39638.32.9
Nexachloroethanm
No
ug/l
6.3
07/31/09 23s22 RPJ
67.72.1.
11-Mtroso-df•n-propylamino
ND
ug/l
6.3
07/31/02 23122 RPJ
Ul-64.7
Nitrobentena
RD
ug/l
5.3
07/31/02 23:22 RPJ
98.95.3
14ophorone
RD
ug/l
6.3
07/31/02 23:22 RPJ
78.59-1
2-xitrOpMergl
NO
ug/l
5.3
07/31/02 23:22 RPJ
09-76.5. ..
2.4.0imethyl'phorol
ND
eg/1
5.3
07/311OZ 23.22 RPJ
105.0.9
bls(2-Chimroethoxy)methene
ND
uo/1
9.3
07/32/02 23r22 RPJ
131.93.1
2.4.111lichloropherol
No
ug/1
6.3
07/31/02 23:22 RPJ.
120.e3.2
i,2.4-Trlchlorobenlene
NO
u0/1
6.3
07/31/02 23:22 RAJ
12042-i .
Naptlthaleno
No
ug/l
5.3
07/31/02 2312 RPJ
91.20.3
Nax4ehlora•1,3-butadiene
No
ug/l
5.3 .'
07/31/02 23.22 RPJ
87.69.3
4-Chlaro•3-0ethylphenol
No
ug/t
6.3
07/31/02 23:29 RPJ
OS-50.7
NOxadhlorocycl.opentadiene
ND
ug/1
12.
07/31/02 23:22 RPJ
77.47.4
2,1:6•Trithloropheral
ND
ugn
SA
OVUM 23:22 RPJ
BO.65.2
2 Chloronaphehllene
ND
ug/l
6.3
07/31/02 23:22 RPJ
91.58.7
Acenephthylene
ilD
ugn
5.3
07/31/02 23.22 RPJ
M-96.0
Dtmsthylphtkutate '
N0
mg/l
5.3
07/31/02 23:22 RPJ
131.11.3
2.6.01nitrotaluene
ND
u0/l
6.3
07/31/02 M22 RPJ
606.20.2
Acenaphthan6
RD
ug/l
6.3
07/31/02 23:22 NPJ
83.32.0
2.4•Dinitrophenol
ND
ug/1
C6. -
O7/31/02 b.-22 RPJ
61,28.5
2.4-Dinitrototuene
ND
ug/1
5.3
07/31/02 23:22 Rili
121.14.2
4•gitrapherol
ND
ug/l
Xi .,
07/31/02 23:22 RPJ
100.024
Fluarene
No
ug/1
6l
.3
07/32/02 23:22 RPJ
86.73.7
4•Chlorophanylpheny) ether
N0
W/1
6.3
07/31/02 23r22 RPi
7006.7E-�
Atech7lphthalete
RD
ug/1'
6.3
07/31/02 23:22 RPJ
94•96.2
ew, Mama
0*2 1 ,
muomlDs
REPORT OF LABORATORY ANALYSIS
.�OhD nrv.cerhttatton.IDe '
Na Wostiwillir
NC Dri*ng W 12
NC Drink rig Water 97706
This report shall not be reproduced, except In full,
lA Wastewater 041w ..
VA Drinking Water . 213 .
SC 990116
without the written consent of Pace Analytical Services, Inc,
FL NELAP E87027
,y
i :

06/03/2003 16:51
9197339612
PAGE 09/12
PepeA02101cel Serldm lee,
/�
m
9600IOnceyAwnw, Sege Igo
�j Q f7e
QCe Ar al j4kal
Huntammilk 4 Mrs
rwr.paeehes.eom
Phone:704.873:9092'
Far 704.876.W91.
Lab Protect Number:
9235047
Client Project ID:
Grwtsbero (IPUES •-
Lab Sample go: 922419692
Project Semple kaber: 9235047'-001 Date (bllectedi 01R6/02'07:35.'
Elient Sample I0: NPDES OD1
Natrixr Water
.
Date Received: 07/30/02 i5:25 .
Parameters
Results Units a 1t Anam By
CAS ft. Ous,
4,4=Dinitro-2•methylphenol
ND
Ug/l
�26.
07/31/02 23:22 APJ
LU-62.1
N-21troirodiphanylamino
ND
Ug/l
5:3
07/31/02 23:22 RPJ
86.30.6
4-Bromophenylphenyl ether
ND
ug/I
5.3
07/31/02 23:22 RPJ
101.55=3
Rexachlorobenmene
NO
Ug/l
/5-3
07/31/02 23:22 RPJ
IU-7441 -
PerlCachlo►ophenol
NO
ug/l
f 26.)
07/31/02 23:22 WJ
87.86.9
Plomrithrene
NO
09/1
Y3
07/32/02 23:22 RPJ
85.01-a
Anthracene
ND
ug/l
5.3
07/31/02 23.22 RPJ
120.12-7
Di-m•butylphtNlato
NO
Ug/i
5.3
07/31/02 23:ZZ RPJ
84.74-2 --
FluorailtMene
NO
UW1
6.1
07/32/02 23:22 RPJ
06-4141•0 - -
Berodine
NO
ug/l
53.
07/31/02 23:22 RPJ
92.91-6
Pyrene
ND
UO/1
6.3
07/31/02 23:22 RPJ
1Zg-'00-�0
Butylberizylphtnalate
NO
Ug/1
6.3
07/31/02 23:22 RPJ
85-68.7
3,3'-Dichlorotxnsidine
ND
U9/1
1t.
07/31/02 23:22 RPJ
91.94.1.
Benm(s)anthracens
NO
U9/1
6.3
07/31/02 93:22 RPJ
66.55.3'
C"ohe
NO
UU/1
5.3
07/31/02 23:22 RPJ
219.41-e
bis(2•EthylhWI)phthal'ate
ND
ug/l
6.3 '
07/31/02 23:22 RPJ
117.11.7
PI•n-Ottylphthelate
NO
Ug/1
5.3
07/31/02 23:22 RPJ
117-04.4
Deozo(b)fluorenthene
No
u9/1
5.3
07/31/02 23:22 RPJ
205.99.2
Beneo(k)fluorintheno
ND
ug/l
6.3
07/31/02 23:22 RPJ
207-08.9
Beftw(0)pyrene
ND
UD/l
S.3
07/31/02 23.22 RPJ
60-34-0'
lndero(1,2,3-cd)pyrene
MD
U9/1
6.3
07/31/02 23:22 RPJ
193.39.6
DlbeftVa,h)enthracene
NO
Ug/l
5.3
07/31/02 23:22 AN
13.70.3
aerin(g.limperylene
MD
Ug/l
6.3
07/31/02 23:22 RPJ
191.24.2
111trobenzene-d5 (S)
63
X
67/31/02 23:22 RPJ
4165.60.0
2-Fluorobiphor(yl (S)
66
4
07/31/02 23:12 RPJ
322.60.6
Terphenyl-d14 (S)
71
X
07/31/02 2):22 RPJ
1718.61,0
Phenol•d5 (S)
30
X
07/31/02 23:22 RPJ
416S-62-2
2-Fluoropheno'l (S)
44
1
07/31/02 23:12 RPJ
367.12.4
2.,4,0•Tr1bromopherwt (S)
67
X
07/31/02 23:22 RPJ
.'
bate Extractad
97/31/02 '
QC 5elnivoletiles
Hexane Extractable Material
Method: EPA 1664
Oil end Grease
8.3
ag/l
5.0
08/06/02 JBR
30
GC volatiles
Pyrgeabla Aromatic
Method: EPA 602
Nethyl•tert•butyl ether
NO
ug/l
1.0
08/02/02 PR
1616.04-4
Benzene
ND
Ug/1
1.0
08/02/02 PPM
7143.2 1.12
NC Wastewater r °Non 1Da REPORT OF LABORATORY ANALYSIS
aCWastav2ter tz
NC Drinking Water 37706 This report shall not be reproduced, except in full,
SC '99000 without the written consent of Pace Anetydeal Services, Inc.
J ,py4
neEac
NOn a
r D� orarorycenMlcalton.lDs
LAWaslawater
04034
VA DrinkinD Water
2T3 .
FL NELAP
E67627

66/03/2003 16:51 9197339612
r,
�ceAnalidicar
Nnve:paeelabe.com
PAGE 10/12
PaceAnalylkal SpMcaa, bu.
BB00KaWAnVo. Stilte IN
Phgrre: ;raaes<�:eaai
Lob Project W nber: qnw5 Far' 704.87rr,.9f191:
Cl lent Project IDS Greeniftro, NPOES
Lab Steele flo: 922429692
Project Semple Wmber: 923SO47.001
0ete:Cbilectedi 07146,
Client Sappl'e ID: WOES 002
Matrix: Water
, .
0at9 111leceived:.0740;
Pdrametere
Results
units Roaort L'ieit
Anal yzed
By
tW Me. .. OUL
Toluene
ND
u9/l
1.0
06/02/02
PPM
lug 86.3 ri
Etbglbenzeae
Ip
ug/l
2.0
09/02/02
PPM
100,41 4
map -xylem
ND
ug/1
1.0
00/02/02
PPN
o-xylas
ND
Sign
1.0
08/02/02
PH
95.47.6
1-6bro-3-fluorabenzens (S)
100.
i
06/02/DY
PRN
620.w.g .
%to, aveeres
NC POd caeWasiewat0r 12 IDS
REPORT OF LABORATORY ANALYSIS
NC Drinking Water 37708 This report shall not be reproduced, except In full,
SC 99006 without the written consent of Pace Analytical Services, Inc.
nelac : •
t abOraEpgl CarNNeallod
LA Wastewater
14s
0A034
VA Drinking Water
213
FL NUP
E5$627

96/03/2003 16:51 9197339612
State of North Carolina
De' artmeht of Environment
algid Natural Resources
Division of Water Quality
N lchael F. Easley, Governor
Willalu G. Ross Jr., Secretary
Alan KI nek, P.E., Director
March 24, 2003
Attu: iaarou D. Leigh
411 Gallimore Dairy Road
Greensboro, NC 27409
.Dear Mr. Leigh:
PAGE 11/12
NORra1 CAMuNA DwAMwm4 cw . ..
ENMRORMEW-AM) NAniPAL'R6s¢LRCks ...
Subject: Remission Request of
Civil Penalty Assessment
Greensboro Terminal
Guilford County
Permit No: NC(1031046
LV 02-618
This letter is to acknowledge your request for remission of the civil penalty levied against the subject facility.
You will be ]totifted when a decision is made conceming the request. 1f you have any questions, please tall
Robert Farmer at [phone].
sincerely,
��}}
4Coleen. Sullins, Chief
Water Quality Section
Cc: WSRO WQ Supervisor w/attachment
Fnforeement fide #: LV 02-618 w/3 attachments
.Central Files
1617 Man Service Center, Raleigh, NC 27699.1617 Tolophone 919-733-601t3 Pa: 919-733-%12'
An Equal Opportunity AfQtmative Action Employer 50%v recycted/10% post -consumer paper '

06/03/2003 16:51 9197339612 PAGE 12/12
. �T •.••°f:, ,� Michael F. Easley, 0ovBOW
Gy.'r
Math n RosaJr..tiectticiry
DeparonentolEndronraaatandNaamlpaaounrYa t�.
/Iat'1yt.l0imek, P.E.„01aadzir 4 ..
niviaiefiat wAlioi tuaBty
C napq'
lvfr. Faxon D. Leigh
Colonial Pipeline Company
411 Gailimore Dairy Road
Greensboro, NC 27409
Subject: Remission Request of
Civil Penalty Assessment
NPDES Permit Number NC0031046
Colonial Pipeline Co. - Greensboro Terminal
Guilford County
Case Number LV 02-618
Dear Mr. Leigh:
I considered the information submitted in support Of your request fbr Ietilission in
accordance with G.S. 143-215.6A(1) and have decided to remit the entire civii penalty in the
amount of $1,067.32 and hereby close our case number LV 02-618.
Please be advised that a full reduction of the civil penalty asessmeat in ho way precludtis
the Division from taking future enforcement action against the subject facility should additional
violations occur.
If you bave any questions about this letter. please do not hesitate to contact Robert
Farmer at [phone], wension 531.
Thant you for your cooperation in this matter.
Sincerely,
Alan W. Rhmek, P.E.
cc: Winston-Salem Regional Office
Enforcement File
Central Files
Gustomer9arvice Division or Water Quality 1617 Mall 5arvirs Center Raleigh, NG 2'1699.1617
1 $00 823.7748 [phone] Fox [phone]

NC Division of Water Quality March/April, 2003
Laboratory Section
Basic Laboratory Techniques - Pipetting
Pipetting, or the measured transfer of liquids by suction, is a skill basic to laboratory chemistry and biology. The
reliable measurement of standards and samples is essential for the success of quantitative analysis. Particularly in
highly sensitive tests, a small mistake in pipetting can cause a large error in the final result. Special equipment and
techniques are required to pipet milliliter and microliter quantities of liquids typical of many laboratory procedures.
There are two basic types of pipetting equipment: glass pipettes and automatic pipettors.
Glass pipettes
There are three types of glass pipets commonly used in the laboratory, 1) the volumetric pipet, 2) the Mohr pipet
and 3) the serological pipet. The volumetric pipet has a single graduation that allows it to deliver one specific
volume to Class A or Class B tolerances. The Mohr and serological pipets are graduated pipets. The Mohr pipet is
graduated from a zero mark near the top of the pipet to a baseline near the tip of the pipet. Mohr pipets are intended
to indicate the delivered volume of liquid by the difference between the initial and final liquid position, with delivery of
the maximum calibrated volume leaving the tip of the pipet full of liquid. Mohr pipets come in calibrations with Class
A and Class B tolerances. A serological pipet is graduated from a zero mark near the top of the pipet to the very tip
of the pipet. It can be used to indicate the difference between the initial and final liquid levels similar to the Mohr
pipet, however to deliver the whole calibrated amount, the pipet is blown out with a pipet bulb such that no liquid
remains in the tip. The best serological pipets are available only with Class B tolerances. Pipets with wide tips for
measuring sludges and other viscous liquids are serological pipets. They will be marked with two wide bands or a
wide opaque ring near the top end of the pipet.
Volumetric glassware is calibrated according to either "to contain (TC)" or "to deliver (TD)" a specific volume. Since
some liquid sticks to the surface of the glassware, the indicated TD volume is slightly larger than the indicated TC
volume. Glassware is also calibrated to contain or to deliver a volume at a specific temperature, usually 20 degrees
Celsius, because the volume of the container is slightly temperature dependent. The solutions measured in the
glassware may also change volume with temperature; therefore, solutions must be measured at the temperature at
which the pipet was calibrated.

around the vessel to aid in orienting the eye to the exact plane of the mark.
When using glass pipets, be sure to remember to wet the pipet with solution prior to measuring an aliquot for
analysis. Fill the pipet with solution to a point past the calibration mark and rotate the pipet so that the inside walls
become coated with the solution. Allow the pipet to drain into a beaker. Fill the pipet with solution once again past the
calibration mark, wipe the tip and stem free of excess solution with a Kimwipe®, and drain until the bottom of the
meniscus is level with the calibration mark. Dispense in a vertical position with unrestricted outflow. Touch the tip of
the pipet to the inside of the filling vessel to remove any drops of solution sticking to it a couple of seconds after free -
flow stops. Again, for volumetric or Mohr pipets, do not blow out the liquid remaining in the tip of the pipet because it
is calibrated to include this liquid. Only serological pipets require that the last drops be "blown out" to obtain the total
capacity.
Using a Glass Pipet
Transfer an appropriate amount of the solution you wish to pipet into a small, clean, dry beaker. Never pipet directly
out of the stock bottle of solution or sample bottle. This creates a contamination risk.
Insert the tip of the pipet into the beaker of solution so that it is about
1/4" from the bottom. Be sure not to press the tip against the bottom
of the container.
If you are right handed, hold the pipet in your right hand, leaving your
index finger free to place over the top of the pipet. With your left
hand, squeeze the pipet bulb. Press it firmly over the top of the pipet,
but do not insert the pipet into the bulb. Release the pressure on the
bulb and allow the solution to flow into the pipet until it is above the
volume mark. Do not allow the solution to reach the bulb.
Quickly remove the bulb and place your index finger firmly over the
top of the pipet. Slowly roll your finger to one side and allow the liquid
to drain until the bottom of the meniscus is aligned with the volume
mark.
When the bottom of the meniscus is even with the volume mark, press your index finger firmly on the top of the pipet
so no liquid leaks out. Pull the pipet out of the solution and touch the tip once to the side of the container.
To transfer the solution, place the tip of the pipet against the wall of the receiving container at an angle of 10-20
degrees. Slowly allow the liquid to drain from the pipet. Keep the flow slow so that no droplets cling to the inside of
the pipet. When the solution stops flowing, touch the pipet once to the side of the receiving container to remove any
hanging drops. Do not blow out the remaining solution unless using a serological pipet.
Sources of error in measurements
The problems posed by different kinds of error must be met in different ways. It is important to recognize the
possibility of these different kinds of error before accepting the apparent results of a measurement.
• Random vs. systemic error: random error distributes actual measurements around the true value. All
measurements have some degree of random error. Systemic error biases error in some way. For
example, a pipettor with a leaky seal will consistently deliver volumes that are too small.
• Machine -dependent vs. user -dependent error: The pipettor (i.e., the machine) may be broken or
miscalibrated, or you (the user) may simply not know how to use the machine properly.
• Constant vs. conditional error: You and the machine might both work well together under ideal
circumstances, but measurements under other circumstances may still be untrustworthy. Consider the
possibility that a pipettor that dispenses water accurately may give incorrect volumes of high viscosity
solutions.
Typical glass pipetting errors and their consequences are described below:
Page - 2

Not rinsing. Cross contamination from residual detergents or rinse solvents or absorption of sample
onto the surface of the pipet can lead to low results. Pipets should be rinsed at least twice with sample
prior to use. This not only serves to rinse the pipet, but also gives the analyst an opportunity to observe
drainage of the rinses to determine whether or not the pipet will drain properly. In cases where there is
insufficient sample for pipet rinsing, the pipet should be hand cleaned and blown dry with a stream of
nitrogen. Never use compressed air because micronized grease from the air compressor can cause
contamination.
2. Pipet is dirty or does not drain correctly. Failure of a pipet to drain completely because of dirt or oils
will cause low results since the entire sample is not dispensed. Small pipets (e.g., 1.0 ml) will exhibit the
largest percent error as a result of incomplete drainage. If normal cleaning doesn't do the job then soak
the pipet in chromic acid cleaning solution, followed by normal washing, rinsing and drying. Another
effective regimen of cleaning, especially after using silicone -based compounds such as silanes and
silicates, is a 3-day soak in 10% ethanolic KOH, followed by a dip in 10% ethanolic sulturic acid, to
neutralize excess KOH, and finally a DI water rinse.
3. Parallax error. Viewing a pipet so that the mark appears as an ellipse rather than a single, straight line,
results in incorrect volume of liquid being dispensed because the analyst cannot determine if the liquid
meniscus is correctly aligned with the volume mark. The results can be either high or low, depending on
the chemist's angle of view.
4. Using a pipet with a chipped tip. This can cause a pipet to not drain correctly, resulting in analytical
error. Pipets with chipped tips should be discarded.
5. Blowing out the tip. Volumetric pipets are generally calibrated TD or "to deliver" and are designed to
drain by gravity, after which a small amount of liquid will remain in the tip. This is normal and with a
properly functioning pipet does not indicate incomplete draining. Blowing out this remaining liquid will
cause high results as more liquid than the rated volume of the pipet is being dispensed. Note: there are
special pipets that are designed to be blown or rinsed out, such as serological pipets. It is important to
check the pipette type before use.
6. Not wiping. Failure to wipe the outside of a pipet completely dry prior to dispensing its contents can
cause high results because liquid sample clinging to the outside of the pipet could drop off or be rinsed
off into the receiving vessel. Avoid touching the terminal tip of the hole to prevent inadvertent sample
absorption due to capillary action.
7. Insufficient drain time. Pipets are calibrated to deliver their contents in a set time, usually within
seconds. Not allowing a pipet to drain for at least its rated drainage time will cause low results since not
all of the sample will have been dispensed. Pipets used to have the rated drainage times printed on
them: however, this practice seems to have gone by the wayside. It in doubt, after the liquid has drained,
allow an additional 15 seconds for non -viscous samples or 45 seconds for viscous samples.
8. Drawing liquid too far up. This can damage pipet bulbs and contaminate samples. The main
consequence is wasted time, but results can be compromised if sample is contaminated by contact with
a pipet bulb.
Automatic Pipettors
Measuring and pipetting small volumes of liquid in the microliter range is generally performed using an automatic
pipettor (also referred to as micropipettors). The ability to carry out this task quickly and precisely is an absolute pre-
requisite for successful laboratory work.
Different brands of micropipettes vary in the volume range they will measure, the type of tips they fit, and the type of
device used to set the volume. Be sure that you understand how to operate the micropipettes you have and that you
obtain the right tips. A few features and rules are common to all micropipettes.
1. Never try to force the volume -setting device beyond its stated range. You can break
the pipette.
2. Never use a micropipette without a tip. Getting solutions on the plunger can ruin it.
Page - 3

3. Always pipette gently, releasing the plunger button slowly. Letting the button pop up
causes liquid to splash into the tip and can contaminate the plunger.
4. Never force the volume control dial, even it the volume indicator shows that improper
handling has damaged the pipette.
5. Handle the micropipette gently. Don't drop, throw, etc.
Using a Micropipettor
All micropipettes have a volume control dial. Determine whether yours shows tenths of microliters or whole
microliters in the smallest place, so that you can read the scale correctly. In general, low -range (10- to 20-pl) devices
show tenths, while high -range devices don't. This can be confusing, since different sizes of pipettes by the same
maker can have different scales on the volume dials.
First you must select an appropriate tip. The tip's
shape, material properties and fit have a
considerable influence on the accuracy of liquid
handling. Tips should be manufactured without any
contaminating chemicals and should demonstrate
good chemical resistance. They should be clean and
free from dust particles. They should be uniform in ►;it
size and geometry for leak -free attachment to the
nose cone. In addition, the surface of the tip (inside
and outside) should be smooth and regular to
prevent retention of the liquid and the opening free of
obstruction to prevent the formation of droplets. To
ensure accurate pipetting results, only tips specified
by the manufacturer should be used.
For optimal precision and accuracy and for volumes
of >10 µl, pre -rinse the pipet tip 2-3 times with the
solution to be pipetted. This will help compensate for
the system pressure adjustments, for differences in
temperature between the pipette tip and the liquid,
and for properties of the liquid. Liquids (especially
protein -containing solutions and organic solvents)
form a thin film on the pipette tip. To ensure that this
surface tension does not cause variation in the
volumes you aspirate, always pre -wet the disposable
tip with the sample before use. Aspirate some liquid
and then dispense it back into the original container.
Successive sample aliquots from this same tip will
exhibit good reproducibility. Without pre -rinsing, the
first volume may be too small due to retention of a
thin film on the inside wall of the tip. The "thickness"
and nature of this film, and therefore the potential
source of error, will vary depending on the nature of
the liquid being pipetted. For smaller volumes (i.e.,
<10 µl), pre -rinsing is not recommended as the
dispensed volume may be too great.
Most micropipettes have 2 stops as you depress the
plunger to expel liquid. The first stop is the correct
stop, the second stop puffs a little air to squeeze out -
any extra drops. When you draw liquid into the pipette tip, depress the plunger control only to the first stop (metering
stroke). If you go to the second stop, you will draw too much liquid into the tip. The most common pipetting error with
micropipettes is missing the first stop and thus drawing too much liquid into the tip.
The pipette should be held vertically during this step. The tip should only be immersed 2-5 mm in the sample;
otherwise, the pressure conditions in the tip are greater than when it was adjusted, causing too large a volume of
Page - 4

liquid to be drawn in (i.e., the volume of gas in the tip is compressed). A low immersion depth also reduces carry-over
on the external surface of the tip. The lower the pipetted volume, the lower the immersion depth should be.
Allow the pipetting button to retract gradually while observing the filling operation (the optimum speed for drawing in
liquid depends on the properties of the sample). To reduce the risk of aerosol formation, turbulence in the tip should
be avoided. IMPORTANT: When the pipetting button has retracted to its initial position (i.e., upper stop), take the
thumb away from it completely. The total absence of pressure increases the precision. Then slowly withdraw the tip
from the liquid, wiping off any drops clinging to the outside if necessary. If an air bubble is observed within the tip
during intake, dispense the sample to the original vessel, check the tip immersion depth, and pipette more slowly. If
an air bubble appears a second time, discard the tip and use a new one.
To dispense the set volume, hold the tip at a slight angle (10-45°) against the side of the container. Place the thumb
over the pipetting button and press it down uniformly as far as the first stop. Wait 1 second. Then press it down
swiftly to the second stop, on order to blow out the tip with the extended stroke.
Reverse pipetting
An alternative pipetting technique is called "reverse pipetting". This technique is often used to get better results on
viscous, highly volatile liquids or those with strong wetting properties. In reverse pipetting, the extended stroke is
used to draw in an additional volume of liquid.
In contrast to normal operation, the pipetting button is pressed down to the second stop. When doing so, the pipette
must be held vertically. When drawing in the liquid, a larger volume than the set value enters the tip. When
dispensing, the pipetting button is only pressed down as far as the first stop, and the tip is then quickly wiped off
against the side of the container. The liquid retained in the tip is then discarded.
Ideally, all pipetting operations should be carried out at the same room temperature as the calibration for maximum
accuracy and the temperature of the pipetted solution should be the same as the pipette tip (volume errors may
occur due to changes in air displacement and viscosity of the liquid. Do not pipette liquids with temperatures greater
than 70°C.
Volume errors may also occur with liquids that have a high vapor pressure or a density/viscosity which differs greatly
from water since water is generally used to calibrate and check the pipette for inaccuracy and imprecision. In such a
case, check your pipet instruction manual. It may be possible to recalibrate the pipette for liquids with densities that
vary greatly from that of water. Pipettes should always be used in a vertical position, otherwise the height of the liquid
column is lower than when the instrument was calibrated, causing too much liquid to be drawn in. Pipettors should
always be stored on an appropriate stand to prevent the risk of scratching the nose cone, which could jeopardize the
seal between the pipette and the tip. The reference methods should be reviewed for cleaning requirements specific
to each analysis.
Testing, calibration and adjustment
Malfunction of the pipettor can cause errors in numerous ways. Therefore, performance checking and service should
be done regularly for all pipettors. With each use, the operator should visually inspect the pipettor for any scratches,
damage to the nose cone or loose connections.
Performance checking can be done using a gravimetric or colorimetric method. The gravimetric method is more
commonly used by laboratories and involves weighing a series of sample aliquots of distilled water at room
temperature using an electronic microgram balance (generally with a readability of 0.1 mg). The key parameters
when evaluating the calibration are the statistically derived estimates for inaccuracy (i.e., the difference between the
set value and the arithmetic mean of the actual values) and imprecision (i.e., the coefficient of variation or relative
standard deviation). The manufacturer specifies tolerances for both parameters. As a rule, the tolerances only apply
to normal operation of the pipettor (i.e., not to reverse pipetting) with deionized water as the test liquid. The minimum
required balance sensitivity depends on the volume measured. The pipette, tip, water and balance must be at the
same temperature and should; therefore, be allowed to attain this temperature by being left immediately adjacent to
one another for a certain time. Room temperature should be between 20 and 250C and should not vary by more than
t0.50C while the test is being carried out. The room in which weighing is carried out should be windowless if
possible, in order to exclude direct sunlight or drafts. For temperature measurements, a thermometer with a
resolution of 0.1 ° C must be used. Using a sample container with evaporation protection facilitates quick and
accurate work.
Page - 5

Most manufacturers offer a combined calibration/adjustment service. Modern pipettes; however, are also designed
so that the user can adjust them. This procedure is generally described in detail in the product documentation. The
pipettor should always be recalibrated after adjustment to check the procedure.
Another important check is a leak test. This can be accomplished by drawing in the maximum nominal volume (using
distilled, degassed water) and placing the pipette on a vibration -free stand. After 1 minute, there should be no visible
droplet formation at the tip.
With experienced personnel following good laboratory practices in an ideal environment (i.e., constant ambient
temperature, constant pipettor, tips and measured liquid temperatures, constant humidity and pressure) most
pipetting errors can be avoided. Although we cannot always control the environment, as long as the operator is
aware of the possible factors affecting pipetting performance, unexpected results can be circumvented.
Preservation of Livestock Waste Samples for Nutrient
Analysis By Max Overman and Dana Satterwhite
Nutrient analysis involves determinations of total Kjeldahl nitrogen (TKN
as N), nitrate + nitrite nitrogen (NO3+NO2 as N), ammonia nitrogen (NH3
as N), and total phosphorous (TP). Occasionally, the laboratory receives
samples for Nutrient analysis collected in close proximity to livestock
operations, such as hog waste lagoons. Hog waste samples are
generally basic in nature (pH of 6-8) and contain carbonates and nitrates
(among other things). Proper chemical preservation of these samples is
important, but can pose a challenge and hazard to field personnel when
concentrated livestock waste is present in a sample.
Proper chemical preservation helps to retard the chemical and biological
changes in a sample. Changes occur rapidly once a waste sample has
been collected. Biological action involving the nitrogen and phosphorous
cycles are the most notable changes in these samples. Organic nitrogen
is released as ammonia nitrogen when bacteria decompose organic matter. Ammonia is lost as a gas or converted to
nitrites, which are rapidly oxidized to nitrates by bacteria. Nitrates can be reduced back to ammonia by bacterial
reduction. This cycle continues unless retarded by a bacterial inhibitor such as sulfuric acid and/or cooling.
Preservation protocol for samples collected for Nutrient analysis prescribes cooling the sample to 40C following the
addition of 25% sulfuric acid (H2SO4) to reduce the sample pH to <2. The addition of acid inhibits biological activity
and eliminates interference by causing salt formation with organic bases. For most samples collected near livestock
operations, the addition of 2 to 4 ml of 25% H2 SO4 to a 500 ml aliquot of sample is sufficient to lower the sample pH
to <2. The acid preservative can be added directly to the sample in a 500 ml bottle, followed by inversion of the
sealed bottle to mix the sample and acid. Use of pH strips is recommended for insuring that sample pH is <2 prior to
cooling the sample to 4°C. In general, samples for nutrient analysis that are received by the laboratory with pH >2
are not analyzed due to improper sample preservation.
When a sample collected near a livestock operation is highly concentrated with livestock waste material (e.g., effluent
directly from a hog lagoon), a larger volume of acid preservative may be required to reduce sample pH to <2.
However, mixing this type of sample with acid in a sealed plastic bottle can cause vigorous reactions. If carbonates
and/or bicarbonates are present, they will produce carbon dioxide (CO2) and effervesce (i.e., bubble) when the acid
reacts with them. Samples that are rich in carbonates can react vigorously causing loss of volatiles. The more
carbonates that are present, the more bubbles you will observe. When mixed with 25% H2 SO4 in a sealed bottle, the
vigorous reaction of a sample containing concentrated livestock waste can cause the sample to overflow from the
bottle when the bottle is opened. In addition, the sample bottle may bulge (or even burst) during mixing or transport.
For acid preservation of samples containing concentrated livestock waste, it is recommended that the sample initially
be collected in an open container (e.g., a 1000 ml beaker). Addition of acid to this type of sample in an open
container does not result in the violent reactions observed in a sealed bottle. Once a sufficient volume of sample has
been collected L500 mL) in the container, the 25% H2SO4 preservative may be added in 2 mL aliquots. Following
each addition of acid, mix the sample with a glass or plastic stir bar and check the sample pH using a pH strip.
Repeat the process until sample pH is <2. Then transfer the acid -preserved sample to a 500 ml sample bottle, seal
the bottle, and cool to 4°C. The volume of 25%, H2SO4 preservative necessary to adjust sample pH to <2 can be as
Page - 6

high as 10 ml for a 500 ml sample containing concentrated livestock waste. The total volume of acid (when greater
than 1 % of sample volume) should be recorded on the fieldsheet.
The addition of the acid preservative should preferably not dilute the sample. Anytime the sample volume is changed
by greater than 1 % (i.e., adding >5 ml of acid to a 500 ml sample bottle), the sample collector should document the
volume of preservative added so the final calculated sample results can be adjusted accordingly.
If a sample containing concentrated livestock waste is to be transported to the lab on the day of collection, then
eliminating the acid preservation (in the field) is an option. Document the reason on the fieldsheet, cool the sample(s)
to 40C immediately after collection, and immediately deliver the samples to the lab. The sample pH can then be
adjusted in the laboratory, under controlled conditions. The results for the sample will be qualified as an estimated
value.
The procedures outlined above are provided as general guidance for acid -preserving samples containing
concentrated livestock waste in a manner that will increase safety to field personnel and result in properly preserved
samples for nutrient analysis. Determining when a sample may require these alternate preservation procedures can
generally only be made in the field on a case -by -case basis. Additional precautions should always be taken when
working with concentrated livestock waste samples, such as the use of safety glasses or goggles, gloves and
working in a well -ventilated area. It there is any question on how to properly treat any sample, contact the laboratory
for guidance.
Phenol, Phenols, or Phenolics?
What is the difference between phenol, phenols and phenolics? These terms have often
caused confusion in environmental analyses. A phenol (or hydroxybenzene) is a single OH
organic compound. "Phenols" refers to the class of aromatic compounds having a
hydroxyl (-OH) group, as well as other substituent groups, on a six -carbon benzene ring
or, prior to the introduction of the list of priority pollutants in the late 1970's, to the
colorimetric analyses of phenols. "Phenolics" is the title used for the USEPA SW-846 Cr
Methods 9065 and 9066 for the colorimetric measurement of numerous known and
unknown substances with one or more hydroxyl groups attached to a benzene ring. The
organic compound, phenol, is the chemical used to calibrate the colorimetric test for the
classes of compounds known as phenols or phenolics.
EPA's list of priority pollutants includes a number of phenols measured in the acid fraction of the base/neutraVacid
(BNA) analysis (or the semivolatile organic compounds analysis) using EPA Methods 525, 625, 1625, and 8270.
These phenols include:
2,4-dimethylphenol
phenol
p-cresol (4-methylphenol)
2,6-dichlorophenol
2,3,4,6-tetrachtorophenol
2-chlorophenol
2-nitrophenol
2,4-dichlorophenol
4-chloro-3-methylphenol
2,3,6-trichlorophenol
2,4-dinitrophenol
4-nitrophenol
Note that phenol is included in the list of the priority pollutants.
2-methyl4,6-din itrophenol
pentachlorophenol
o-cresol (2-methylphenol)
2,4,6-trichlorophenol
2,4,6-trichlorophenol
Each of the priority pollutant phenols, including phenol itself and the pare substituted phenols, can be found,
identified, and quantified by several gas chromatographic/mass spectrometric EPA methods such as 525, 625, 1625,
and 8270. TIW colorimetric.analytical procedures entitled -phenols or.phenolicsmeasure many compounds and 7
proves - quantitative.ree uu t.for_phenols o�_phenolics as a class..However, no specific compound can be identified og
antifi qued-using the colorimetric-method.-Consequently, if a sample is analyzed by one of the colorimetric methods,
no -specific phenolic compound, including phenol itself can be stated to be present in the sample and is reported by
this laboratory as "total recoverable phenols".
Phenols may occur in domestic and industrial wastewaters, natural waters and potable water supplies. Chlorination
of these waters may produce odorous and objectionable -tasting chlorophenols. Decaying vegetation and, in
Page - 7

particular, wood produces numerous phenols because the benzene with the hydroxyl group is in a major portion of a
woody substance called lignin. Lignin is removed from paper pulp made from trees and degrades to form numerous
substances including phenols. These phenols include humic and fulvic acids, large molecules of organic matter that
are soluble in water, as well as aromatic substances with several hydroxyl groups on the benzene ring. These
phenolic compounds can and do form groundwater plumes emanating from swamps and wetlands, and the plumes
can contain a variety of phenols. Again, a positive result from colorimetric analysis can only tell you that the hydroxy
benzene structure is present. It cannot tell you what specific compounds are present.
Discrete Analyzers
"Discrete analyzers" are currently being marketed by several different manufacturers. The question of whether these
instruments are acceptable for NPDES reporting has been addressed by EPA Region 4. Below is a reprint of a letter
sent by EPA's Office of Water to one company describing EPA's (Office of Water, Engineering and Analysis Division)
policy on the use of the discrete analyzer.
Gregory Hirt
National Sales Manager
/achat Instruments • Hach Company
6645 W. Mill Road
Milwaukee, W153218
Dear Mr. Hirt:
Thu letter responds to your inquiry regarding the acceptability of discrete analyzer systems for
use with EPA approved methods. In general, EPA does not approve or endorse specific instrumentation
and allows equivalent instrumentation to be used in EPA approved methods. The main issue that we have
to resolve is whether the discrete analyzer system is equivalent to the instrumentation specifced in the
applicable EPA approved methods. The information available to EPA on the discrete analyzer system
indicates that the instrument automates several analytical steps and reduces sample sizes to 3 - 300
microliters.
Historically, EPA's Office of Water has allowed automation and reductions in sample volumes
provided that all sample to reagent ratios are maintained and the sample volume used is adequate to
achieve the required quantitation limit. Method developers, such as instrument manufacturers, typically
submit applications describing the specific steps to he automated and exact sample volumes to he used to
EPA for review and acceptance before marketing or using an analytical method for compliance
monitoring. This step avoids the potential that compliance monitoring data could be brought into question
if it is determined at a later date that the modifications made to the analytical method go beyond mere
automation or sample volume reduction. Specific concerns include the possibility that the proposed
automation makes substantive changes to the analytical procedure or operating parameters (e.g.,
temperature), and that extreme sample volume reductions would result in analysis of a non -representative
sample. To avoid these concerns and make it less likely that data quality would be questioned, we
recommend that method developers seek nationwide EPA review and acceptance for each compliance
monitoring method that they would like to use with the discrete analyzer system.
However, because we allow the use of equivalent instrumentation in EPA methods, laboratories
my use a discrete analyzer system for National Pollutant Discharge Elimination System (NPDES) and
National Primary Drinking Water Regulations (NPDWR) compliance monitoring provided that (1) they
understand the risk that auditors may question the data and its quality, (2) all procedures in the approved
methods are followed, (3) use and operation of the discrete analyzer system are incorporated into the
laboratory's standard operating procedures, and (4) all method specified sensitivity requirements and
quality acceptance/quality control criteria are met. Final responsibility for ensuring that all procedures
specified in the approved methods are followed and that all sample to reagent ratios are maintained rests
with the analyst and the party or parties responsible for reporting the results for compliance monitoring
purposes (e.g., permittees, contract laboratories).
If I can be of additional assistance on this and other matters, please contact Khouane
Ditthavong at (202) 566-I068.
Sincerely,
William A. TeUiard, Director
Analytical Methods
Engineering and Analysis Division
Page - 8

cc: Khouane Diuhavong, U.S. EPA, OW
Jim O'Dell, U.S. EPA, ORD
Wayne Turnbull, U.S. EPA, Region 4
Kevin Roberts, DynCorp
Additional information may be obtained by contacting Gary Bennett, Chief, Office of Quality Assurance and Data Integration -
USEPA - R4 SESD, 980 College Station Road, Athens, GA 30605, [phone].
Laboratory Safety - Disposal of Broken Glassware
Broken glassware poses a hazard to both laboratory and maintenance personnel. This article will describe proper
methods for safe glassware disposal.
Laboratory analysts should inspect all glassware before use. Broken, chipped, starred or badly scratched glassware
must not be used. If the glassware cannot be repaired, it must be discarded in a rigid, puncture -proof container
specifically designated for broken glass (e.g., a cardboard box with taped seams, plastic bucket, or metal can with a
sealing lid). Glassware must never be disposed of with normal
trash. Maintenance personnel may be injured when carrying
trash bags with broken glassware in them. Broken glassware
containers should be clearly marked "CAUTION - BROKEN
GLASS" to alert all personnel to the hazard. They should not be
filled to overflowing and quantities should be limited to
approximately 15 pounds to avoid creating a lifting hazard.
When the container is full, it should be,placed directly into the
dumpster.
Glassware with biological contamination (i.e., glassware that has
been in contact with infectious agents) such as slides, cover
slips, test tubes, beakers, and pipettes must be disinfected
before disposal. Glassware with chemical contamination Should
be emptied into a suitable container and rinsed thoroughly
before disposal.
Broken glassware should be cleaned up immediately. A laboratory should have a small brush and dustpan available
to clean up after small accidents. Forceps or duct tape can also be. used to pick up smaller pieces of broken glass.
Personnel should wear lab coats, safety goggles and chemical resistant gloves when handling contaminated
glassware. Extra caution should be used when handling broken glassware. If you get cut, remove visible glass
fragments, flush wound liberally with water and apply direct pressure. All injuries should be reported to a supervisor.
If medical attention is required, the incident is to be formally reported to your supervisor and to the Safety Officer (or
other designee as specified in the Chemical Hygiene Plan).
Resources
National Environmental Methods Index (NEMI).
The USEPA and the U.S. Geological Survey (Water Resources Division) now offer a free web -based clearinghouse
of environmental monitoring methods. The site indexes method summaries of laboratory and field protocols providing
a mechanism to compare and contrast the performance and relative cost of analytical, test, and sampling methods
for environmental monitoring. Visit www.nemi.00v.
National Volunteer Monitoring Newsletter Available.
The winter 2003 issue of the national newsletter for volunteer watershed monitoring is now available. This issue
focuses on university partnerships, and includes articles on Dickinson College's Alliance for Aquatic Resource
Monitoring (ALLARM), recent modifications to the Virginia Save Our Streams biomonitoring method, college -
community partnerships, the University of Florida's LAKEWATCH program, partnerships between cooperative
extension programs and volunteers, and linking citizens to scientists. A hard copy of this issue may be obtained by
Page - 9

sending an email request to Alice Mayio at [e-mail], or by downloading at
h[lp;//gww,ePagtiv/�y�g�y/mini wring/ygl�teer.
Calendar of Events
April 14-17, 2003 The 22na Annual National Conference on Managing Environmental Quality Systems will be
held at the Sheraton New Orleans in New Orleans, Louisiana. Conference activities provide
a forum to address issues involving environmental quality systems and information quality
issues across the EPA and its stakeholder organizations. The conference agenda offers
various Quality Systems training courses, technical sessions, and workshops. For more
information, visit http://production.alpha-gamma.cony/el)anationalcorVoverview.htm.
April 15, 2003 LabNet meeting at Meritech Laboratories, Inc. in Reidsville, NC. The program will be on
clean sampling for Mercury using EPA Method 1699.
April 29-30, 2003 The 26th Annual Conference on Analysis of Pollutants in the Environment, which is jointly
sponsored by the U.S. Environmental Protection Agency's Office of Science & Technology,
and Battelle, will be held on April 29 - 30, 2003, at the Holiday Inn Chicago Mart Plaza in
Chicago, Illinois. This conference has been recognized as a leading forum for dissemination
and discussion of technical analytical issues related to the most recent environmental
regulations. Participants will have the opportunity to discuss and debate the cutting -edge
issues of environmental and analytical chemistry, such as 1600-series Methods, Organics
analysis, and a Workshop on Whole Effluent Toxicity (WET) Testing to Support EPA's Final
Rule. On May 1, 2003, EPA will hold a public meeting on EPA's Assessment of Detection
and Quantitation Procedures Applied under the Clean Water Act. Visit the conference web
site at http://dvnseg.dyncorp.com/epa/owinorfolk2003.nsf.
May 22, 2003 Lab Technology Day at the NCSU McKimmon Center in Raleigh, NC.
Questions, comments or contributions to Benchnotes should be directed to Dana Satterwhite at [phone] ext. 243.
Page - 10

Hydrostatic Test Water Discharge
Subject: Hydrostatic Test Water Discharge
Date: Mon, 22 Apr 2002 08:46:34 -0400
From: "Leigh, Faron D" <[e-mail]>
To: "'Joe Corporon'" <[e-mail]>
Hi Joe!
This is a follow-up to our telephone conversation concerning hydrostatic
testing of tanks. As discussed, we have been sampling a "first flush" prior
to discharging. If parameters are within limits, we are discharging
directly to the main lake as opposed to discharging to the dikes. This is
the same process we have been using for as long as I can remember.
Discharging directly to the lake, as opposed to discharging into the dikes,
greatly reduces the potential for erosion and better protects the waters of
the State. My question is, how do I show this on my DMRs? Should I record
the flow as if it is going through the outfall that it would go through if
we were discharging to the dike area or should I submit an additional DMR?
Maybe I could submit an additional DMR showing the tank number, flow rates
and analytical data. What are your thoughts?
Thanks;
Faron
All
".0 4
1 of 1 4/26/02 6:42 AM

Sounds good, Joe. Have a nice vacation!
Faron
> -----Original Message-----
• From: Joe Corporon [SMTP:[e-mail]]
> Sent: Thursday, March 21, 2002 2:36 PM
> To: Leigh, Faron D
> Subject: Re: FW: NPDES Permit No. NC0031046 - Flow Rates
> Faron, Received xl files okay, but won't get to them right away. Many fires to
> put out. Leaving on vacation tomorrow. Check back in about three weeks.
> "Leigh, Faron D" wrote:
Sorry, Joe! I forgot to put the dot between Joe and Corporon in your e-mail address.
> > Faron
> > > -----Original Message-----
* > > From: Leigh, Faron D
> > > Sent: Thursday, March 21, 2002 1:46 PM
>>>To: [e-mail]'
> > > Subject: NPDES Permit No..NC0031046
Joe,
Since our recent telephone conversation, I have decided to go ahead and use the rational method to
calculate discharge rates for our NPDES effluent. The attached spreadsheets have calculations for all
five outfalls based on rainfall events and the impervious surface areas for each.
The rainfall events are in increments of five, one -hundredths of an inch and range from .05" to 2.00".
The impervious surface area was estimated from 1996 data the City of Greensboro used to determine
stormwater fees for their Stormwater Quality Management Program. It is my understanding that the
City of Greensboro performed aerial GIS surveys to measure impervious surface areas to calculate
unit fees for various facilities. They calculated that Colonial's Greensboro facility has approximately
1,706,000 square feet of impervious surface area. I have used their map to estimate how much of this
total area discharges to each outfall.
The runoff coefficient the City of Greensboro uses ranges from .20 to .80 depending on development.
I am proposing we use a runoff coefficient of .50 based on retention time in the dike areas, retention
ponds and/or basins, and the amount of "fill material" in place where our pipelines are buried and
equipment is installed.
When you get a chance, please take a look at these rates and let me know your thoughts. I realize that
totalizers installed at each outfall pipe would be the best method, but hopefully this will be acceptable
until I get approval for the meter installations.
Please give me a call if you have questions or need additional information. Thank you very much for
your assistance with our permit renewal and our flow rate measurement options.
Sincerely,
Faron