EPA-600/3-84-0^8
March 1984
DRILLING MUD ASSESSMENT
CHEMICAL ANALYSIS REFERENCE VOLUME
by
Science Applications, Inc.
Environmental Chemistry Division
La Jolla, CA 92038
RIN-57 60-83-N
Project Officer
Thomas W. Duke
Environmental Research Laboratory
Gulf Breeze, Florida 32561
ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
GULF BREEZE, FLORIDA 32562

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DISCLAIMER
This report has been reviewed by the U.S. Environmental Protection Agency,
and approved for publication. Approval does not signify that the contents
necessarily reflect the views and policies of the U.S. Environmental Protection
Agency, nor does mention of trade names or commercial products constitute
endorsements or recommendation for use.

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FOREWORD
The protection of our estuarine and coastal areas from damage caused by
pollutants requires that regulations restricting the introduction of these
compounds into the marine environment be formulated on a sound scientific
basis. Accurate information describing concentration-response relationships
for organisms and ecosystems under varying conditions is required. The
Environmental Research Laboratory, Gulf Breeze, contributes to satisfying this
information requirement through research programs aimed at determining:
the effects of pollutants on individual species and communities of
organisms.
the effects on ecosystems processes and components.
the significance of chemical carcinogens in estuarine and marine
envi ronments.
This report presents a chemical characterization of 11 industry-supplied
drilling fluids collected from operating rigs in the Gulf of Mexico and one
commercial drilling fluid additive. Concentrations of aromatics, aliphatics,
selected heavy metals in the liquid, suspended particulate and whole mud phases
of the drilling fluids are reported. These data will add to our knowledge of
the chemical composition of drilling fluids and can be used by regulators and
others as part of a risk assessment process.
Environmental Research Laboratory
Gulf Breeze, Florida
in

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ABSTRACT
This report presents concentrations of specific metals and hydrocarbons
in eleven drilling fluids (muds) taken from operating gas and oil rigs in the
Gulf of Mexico. Each drilling fluid was analyzed chemically for heavy metal
and hydrocarbon content in three distinct phases: (1) the bulk or whole mud,
(2) a suspended phase derived from the bulk mud sample, and (3) a "dissolved"
or liquid phase, Aliquots of bulk muds were removed for barium analyses by
instrumental neutron activation and for analysis for iron, aluminum, lead,
zinc, cadmium, copper, strontium, and calcium by atomic absorption analysis.
Analysis of the suspended particulate and liquid phases was similar. The
aromatic and aliphatic content of the three phases were determined by
extraction and then fractionation by column chromatography.
The analysis for each of the 11 drilling fluids is presented in four
parts:
A.	Drilling fluid concentrations,
B.	Whole drilling fluid organic concentrations,
C.	Particulate phase organic concentrations,
0.	"Dissolved" phase organic concentrations.

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CONTENTS
Foreword	iii
Abstract		iv
Tables	vi
1.	Introduction 		1
2.	Methodologies 		4
3.	MIBLKA51		28
4.	AN31-1-6		48
5.	MILGEL®		68
6.	SV76-2-5		88
7.	PI-1-3 	108
8.	P2-1-3 	128
9.	P3-1-3 	148
10.	P4-1-3 	168
11.	P5-1-3 	188
12.	P6-1-2 	207
13.	P7-1-2 	227
14.	P8-1-1 	247
References		27
v

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TABLES
Number	Page
1	List of Samples Characterized for
Chemical Content 	 2
2	Whole Drill Fluid pH Values 	 6
3	Dissolved Bioassay Phase Syphon Volumes 	 8
4	Instrument Operating Conditions and Detection
Liinits for Metals Analyzed by Graphite
Furnace Atomic Absorption Spectrophometry 	 10
5	Instrument Operating Conditions and Detection
Limits for Metals Analyzed by Flame Atomatic
Absorption Spectrophometry 	 11
6	Trace Metal Sample Accuracy and Precision 	 14
7	Comparative Whole Mud Hydrocarbon Concentration
and Water Content Data	 24
8	Comparative Hydrocarbon Concentration in Whole
Suspended and Dissolved Drilling Mud Phases 	 25
FIGURES
Number	Page
1	Analytical Scheme for Metals in Drill Muds	13
2	Analytical Scheme for Organics in Drill Muds	18
3	Petroleum Hydrocarbon Concentrations and
Water Contents from this Study vs No, 2
Fuel Oil Concentrations and Water Contents
from NEA	23
v i

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I. INTRODUCTION
This compendium serves to document chemical characterization
data obtained on eleven industry-supplied drill fluid mixtures
(Table 1) and one commercial drill mud additive (Milgel®). Drill
mud materials were obtained from PESA (Petroleum Equipment
Suppliers Association) by the U.S. Environmental Protection
Agency (Gulf Breeze Laboratory), and analyzed as part of a multi-
disciplinary assessment and cataloguing of acute aquatic toxicity
and chemical make-up. Companion reports contain toxicity and
bioaccumulation data.
All the materials analyzed are used in off-shore well
drilling and, as a result, are candidates for ocean discharge as
a means"of "waste disposal. Drill muds in general are mineral-
based, typically enriched in barium (in the form of barite,
BaS04), chromium and zinc, to name a few elements, and are
fortified with a variety of other, usually synthetic, materials
to obtain desired consistencies for drill-line lubrication and
well-hole pressure control. The mineral base is typically a
mixture of barite (barium sulfate) and various clays, and other
additives are predominantly organic-based, but can contain
relatively high concentrations of heavy metals. Presumably,
drill muds which will eventually be disposed of at sea as a
direct discharge are to be free of any potentially harmful
additives, such as petroleum-derived compounds and other
suspected toxicants.
1

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TABLE 1* List of Samples Characterized for Chemical Content
Sample
MIBLKA51 Al-7
An 31-1-6
Milgel®
SV 76-2-5
Pl-1-3
P2-1-3
P3-1-3
P4-1-3
P5-1-3
P6-1-2
P7-1-2
P8-1-1
Laboratory.Identifier
83-323
83-324
83-325
83-326
83-2000
83-2001
83-2002
83-2003
83-2004
83-3312
83-3313
83-8537
2

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As direct discharges, these materials are controlled under
federal and state discharge permit requirements, which stipulate
routine acute toxicity testing. Historically, a problem has
existed in equating observed toxicities with chemical
composition, largely because comparative sets of data have not
existed.
In preparing this data reference report, the selected drill
fluid materials were analyzed in the bulk ("whole mud") state,
and as both dissolved and particulate bioassay phases. The two
"bioassay" phases were prepared in a manner identical to the
dissolved and particulate phases stipulated in EPA-prescribed
acute toxicity pre ^colsd). Included in this reference volume
are analytical procedure descriptions, followed by data on
chemical concentrations and identifications.
It is readily apparent from the organic analysis results
that a number of samples contain substantial amounts of
petroleum-derived hydrocarbons. Although it is not possible to
identify the source(s) of hydrocarbons found in the fluids
analyzed, the qualitative evidence does not point toward crude
oil contamination picked up from the drilled formations.
Instead, in the cases of noticeable hydrocarbon presence, these
components appear to be "refined" petroleum fractions.
3

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II. METHODOLOGIES
A. Sample Preparation
Each drill fluid material was chemically analyzed for heavy
metal and hydrocarbon contents in three distinct phases: 1) the
bulk mud as supplied by PESA and shipped to the laboratory? 2) a
suspended particulate phase derived from the bulk mud using the
EPA Reigon II bioassay test procedures^) ; and 3) a dissolved
phase generated from the same protocols. One purpose of this
approach was to examine the whole fluid mixture after it had been
used, or "spent", in a drilling operation? this form represents
the potential bulk waste discharge, data which are important in
dispersion modelin and other impact assessment tools which can
predict chemical influence. The second purpose was to create the
same phases used in aquatic bioassay testing in order that
correlations can be made between chemical content and degree of
toxicity.
Whole Drill Fluid
Whole drill fluid samples were received frozen and, after
thawing, were thoroughly homogenized. An approximate 30-g wet
aliquot was removed from each bulk sample, weighed wet to the
nearest mg, lyophilized (freeze-dried), and re-weighed to the
nearest mg. This allowed determination of water content and also
4

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prepared a sample aliquot for heavy
except mercury). A separate wet
hydrocarbon measurement.
Particulate Bioassav Phase
After measuring the pH of each drilling fluid sample (Table
2), 400-ml aliquots were added to 2000-ml graduated cylinders
containing 200 ml of filtered seawater (pH 7.7), The volume was
adjusted to 2000 ml with filtered seawaterr the pH re-measured,
and adjustments made with reagent grade in HNO3 or 5% NH4OH to
original pH levels*
At this point/ each sample was stirred vigorously in its
cylinder for 30 minutes with a glass rod. After being allowed to
settle for 1 hour, 1000 ml were syphoned from the tops using
Teflon tubing. Or this "syphonate", a 50-ml aliquot was taken
and stored in an acid-cleaned linear polyethylene bottle for
subsequent heavy metal analyses, while the balance was placed
into a continuous liquid/liquid extraction vessel for hydrocarbon
analysis preparation.
Dissolved Bioassav Phase
Duplicate samples of each bulk drill fluid were made up in
2000-ml graduated cylinders with seawater as described above.
5
metal analysis (all metals
aliquot was removed for

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TABLE 2. Whole Drill Fluid pH Values
Sample No.

2H
8.8
MIBLKA51 Al-7
83-323
An 31-1-6
83-324
9.3
Milgel®
83-325
7.5
SV 76-2-5
83-326
9.3
Pl-1-3
83-2000
9.4
P2-1-3
83-2001
9.8
P3-1-3
83-2002
9.3
P4-1-3
83-2003
7.4
P5-1-3
83-2004
8.9
P6-1-2
83-3312
7.9
P7-1-2
83-3313
9.2
P8-1-1
83-8537
9,1

Method Blank
7.7
6

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After 30 minutes of vigorous stirring, each sample was allowed to
settle for 72 hours, after which the topr relatively clear layer
was syphoned off with Teflon tubing. This upper layer of "clear"
seawater varied in thickness depending on the settling
characteristics of each drill fluid. Table 3 indicates the
thickness of the syphoned layer for each sample. Each
"syphonate" was centrifuged at 300 rpm for 10 minutes and
decanted; each centrifugate was then filtered sequentially
through 8.0 m, 0.8 m and 0.4 m membrane filters. Of the final
filtrate volume for each sample, 50 ml were set aside in acid-
cleaned linear polyethylene bottles for heavy metals analyses and
the balance went to liquid/liquid extraction vessels.
B. Elemental Anal/sis Procedures
Whole Drill Fluid
After freeze-drying and powdering, an accurately weighed (to
the nearest 0.1 mg) aliquot of -0.25 g was removed for barium
analysis by instrumental neutron activation, and an approximate
0.1-g aliquot (also to the nearest 0.1 mg) was removed for acid-
digestion and atomic absorption analysis for iron, aluminum,
chromium, lead, zinc, cadmium, copper, strontium and calcium.
For barium analyses, instrumental neutron activation
1 2
included six-hour irradiation in a TRIGA reactor at 10
7

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TABLE 3. Dissolved Bioassay Phase Syphon Volumes
Sample No.

MIBLKA51 Al-7
83-323
An 31-1-6
83-324
Milgel®
83-325
SV 76-2-5
83-326
Pl-1-3
83-2000
P2-1-3
83-2001
P3-1-3
83-2002
P4-1-3
83-2003
P5-1-3
83-2004
P6-1-2
83-3312
P7-1-2
83-3313
P8-1-1
83-8537
Volume. Syphoned, (mil
1000 ml
840 ml
1000 ml
940 ml
740 ml
600 ml
600 ml
1000 ml
1200 ml
1200 ml
340 ml
700 ml
8

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neutrons/cm^-sec, followed by a 12-day "cooling" period to allow
interfering isotopes to decay, and a 30-minute to two-hour count
of the Ba-131 line. Gamma counting was performed with a two-inch
Nal Ge(Li) detector and a multi-channel analyzer. Detection
limit of this procedure was 1-5 ug/g (dry sample weight).
In the case of the other metals, each accurately weighed
aliquot (-0.1 g to the nearest 0.1 mg) was totally dissolved in a
pressurized Teflon bomb, using a low-volume combination of
nitric, hydroflouric and hydrochloric acids. The digestion was
carried out in a 60°C water bath for approximately six hours,
rendering each sample totally dissolved with the exception of
observable, small amounts of barite (barium sulfate); this barite
residue was cons :ered to have no effect on the successful
analysis of the other metals.
The resulting aigestate was brought to volume with 1U nitric
acid and analyzed by a combination of flame and flameless atomic
absorption for the nine other elements. Tables 4 and 5 present
the instrumental operating conditions for each element; in
general, these follow the criteria given in EPA!s Methods for
Water and Wastewater^' and in Standard Methods^), with
modifications to accommodate the complex drilling mud sample
matrix.
9

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TABLE 4. Instrunent Operating Conditions and Detection Limits for Metals Analyzed by Graphite Furnace Atomic
Absorption Spectrophotometry
l leflu-rit
UdvfIrnglh
(nm)
I iimp
Current
("¦A>
SI u
width
(nw)
In jec t ion
Voluue
(..U
Gd s

f in nat e
' i.rnlil hhiv
Hm imuii
Detection
i i*it (ppij)
Absolute
Detection
I ifliit
(programs)
Sens it wily
(ppb/0.0044 Abs)
Sensitivity
(picograas/O 0044 Abs)
Additional Coavents
A1
;«J9 3
i'u
0. /
20
Ai (3 sec.
flow, SO)
normal
Dry : 110". 77 sec.
Char: 1300 C. 22 sec.
Alanine: 2700"C, 7 sec.
2
3
m
60
correction
ltd
SS
2S
0.2
SO
Hp (3 sec.
tfow» e*>)
normal
Ory: 110°C. 30 sec.
Char . I800T, iO sec
Atcrotze: 2fi00°C, 8 sec.
10
600
20
1000
Ho Op correction
10
422
10
0.7
20
Ar (3 sec.
flow, ?0)
normal
Dry: 110 C. 2? sec.
Char: II00°C, 22 sec.
AtanUe: 2700'C. 7 sec.
0.5
10
1
20
No 0^ correction
Environmental
Contamination
i.ti
278 8
4
0.7
10
Ar (3 sec.
flow. 20)
normal
Ory. 110°C. 77 sec
Char: 3S0WC, 22 sec.
Atan1;e ?ID0°C. 7 sec.
0.1
1
0. 3
3
Dp correction
( r
IS/ 9
B
0.7
20
Ar {3 set.
flow. 30)
norma 1
Ory : 1 IO C. 22 sec.
Char; HOOt. 22 sec
AtomUe: 2700°C, / sec.
Oi
10
0. ?
14
0^ correction
r.i
V4. 7
10
o ;
20
Ai ( j sci .
flow. 40)
nor nial
Dry: HO C, 22 sec.
Char: 90U"C, 27 sec.
Atom we- 2700"C, 7 sec.
Ob
10
1
20
0^ forrec t ion
re
24H. J
/b
0?
20
Ai ( J sec .
flow. 20)
normal
Dry: HO C. 22 sec.
Char: tl(KPC, 7? sec.
Atom we: 2700WC, 7 sec.
o.s
IS
10
30
Op correction
Ph
283. 3
10
0./
20
Ai ( J «,t't .
flow. 20)
norma 1
Ory : HO C. 72 sec
Char: 7SO"C. 22 sec.
Atomize: 7 sec
OS
10
I
20
Dp correction
jr
460. /
20
0.2
20
Ar ( i s«-i ,
flow, 20)
norm* 1
Ory IIU'C, 77 sec.
Char: 000 "C. 22 sec.
Atomize 2 MOT, 22 sec.
1
20
IS
30
Ho Op correction
/n
213.9
IS
0.7
10
Ai ( j sec .
f1ow, )
nonna 1
Ory: 110" C. 77 sei
Char: 500 C. 72 sec.
Aluni/iv ?V)rt°C, / sec.
O.I
1
0. i
3
D;> correction
fnviromental
Coniaatnat ioii

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TABLE 5. Instrument Operating Conditions and Detection Limits for Metals Analyzed by Flame Atomic Absorption Spectrophotometry
Element
Wavelength
(nm)
Lamp
Current
(mA)
Slit
Width
(nm)
Gas
Oxidant/Fuel
Flame Type
Minimum
Detection
Limit(ppm)
Sensitivity
(ppm/0.0044 Abs)
Additional Comments
A1
309.3
20
0.7
n2o/c2h2
Reducing
0.5
2.0
D2 correction
Bd
55
25
0.2
n2o/c2h2
Reducing
0.5
1.5
No 02 correction
Ca
422.7
10
0.7
A1r/C2H2
Oxidizing
0.01
0.1
No D2 correction
Environmental
contamination
LaCl^ matrix used
Cd
228.8
4
0.7
Air/C2H2
Oxidizing
0.01
0.03
correction
Cr
357.9
8
0.7
Air/C2H2
Reducing
0.03
0.1
correction
Cu
324.7
10
0.7
Air/C2H2
Oxidizing
0.04
0.1
D2 correction
Fe
248.3
25
0.7
Air/C2H2
Oxidizing
0.02
0.15
D2 correction
Pb
283.3
10
0.7
Air/C2H2
Oxidizing
0.2
0.6
D2 correction
Sr
460.7
20
0.2
n2o/c2h2
Reducing
0.02
0.1
No 02 correction
LaCl^ matrix used
Zn
213.9
15
0.7
Air/C2H2
Oxidi zing
0.015
0.02
D? correction
Environmental
contamination

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Figure 1 summarizes the analytical scheme used for metals
determination* All elemental concentrations are reported in as
mass of component per unit dry weight of whole drilling fluid.
Water content data are available to convert these data to mass of
metal per unit volume of wet mud. Table 6 presents accuracy and
precision data for metals analyzed for.
Particulate Bioassay Phase
The 50-ml aliquots removed from the one-hour syphonates
described above were subjected to a 6U HNO3 leach described in
EPA's Methods for Water and Wastewater. After heating and
being allowed to cool and settle, each acid leachate was decanted
off into a 25-ml c.aduated cylinder and brought to volume with
1.0 U HNO3. Analyses followed using flame and flameless atomic
absorption as described for whole drill fluids. In this case,
barium was also analyzed for by atomic absorption
spectrophotometry as opposed to neutron activation analysis.
Dissolved Bioassay Phase
The dissolved bioassay phases, prepared by 72-hour settling
in seawater, centrifugation and filtering, were analyzed for
heavy metal contents in the same manner as described above for
the particulate bioassay phase. Again, atomic absorption was
utilized for barium rather than neutron activation.
12

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FIGURE 1. Analytical Scheme for Metals in Drill Muds
grin SamoI# (1 l Ttflan J*r)
orqnles
ii—iwia wiw
uflon stirrer.
SoHt
1
wait
S4i ^fir« 2
uct 4liquet for
1 1
«*1?A vtt 10Q. 5 9
grim $1»
aliquot '30 9 iHouot

d#t«r»i nation
I I


'ma 4ry |
mur cmtmt
4*t*rwi nation
••1*1 try
9QMCT
^•2S f dry
«iiau0t
vtt
*•1*1! iccurtttly
into 1/4
palyrui
* .1 9 4pf 4l 1quot
low terro. ash
l
t*f!on dictation
at «TC *1tft *10,, *C!
and H*
;w (9»i
ervftsftr -J ?i*Mta
4fta arrtiq to vo'tua*
m -i -WO,
*at*r sat* Hgtrtlan
it ^90*C for 3 loun
1:1 *4,:HtS3i> 4iW
OMk. Initial
reduction fry MMt0H.
HC*.
Col4 vtoor AAS]
4ft*r -^auction «f
¦<** •• «itrt SflO,
mttnawrt inalysos oy
^IM/'^4Ml«SS us -
*0, A1 , >. C4, Zfl,
At
13

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TABLE 6. Trace Metal Sample Accuracy and Precision (Concentrations in yg/g dry weight unless otherwise Indicated)
Element3
River Sediment
(SRM-1645)
River Sediment
(SRM-1645)
Estuarine Sediment
(SRM-1646)
Estuarine Sediment
(SRM-1646)
Determined C.V.*
N.B.S.
Determined
N. li.
Determined
SRM-1645
SRM-1646
At
—
¦ —
(X) 6.25 i 0.2
(%) 6.03 i 0.1

2
Ca
—
	
(%) 0.83 i 0.03
(%) 0.86 t 0.02

2
Cd
10.2 • 1.5
10.8 t 0.5
0.36 ± 0.07
0.29 * 0.03
5
10
Cr
(%) 2.% ' 0.28
(%) 3.02 t 0.05
76 i 3
60 x 2
2
3
Cu
109 19
107 i I
18 t 3
17 ± 1
1
6
Fe
(%) 11.3 » 1.2
(%) 10.7 • 0.2
(%) 3.35 t 0.1
(X) 3.47 t 0.05
2
1
Pb
714 < 28
728 < 33
28.2 t 1.8
28.6 ±2.5
5
6
Zn
1720 i 169
1588 • 18
138 t 6
121 i 4
1
3
aMean values obtained from n=5 analyses

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C. Organic Analysis Procedures
Whole Drill Muds
Each sample was weighed wet and an aliquot withdrawn for
dry weight (percent water) determination. Each sample was then
extracted, dried with a methanol/shaker table agitation
procedure, and the dewatered samples further extracted with
methanol/methylene chloride. The methanol used for the initial
water removal step was back-extracted with hexane and the
combined organic extracts, then further back-extracted with
saturated sodium chloride solution to remove residual water from
the organic phases. The saturated sodium chloride was then back-
extracted with methylene chloride (3 times) to ensure removal of
all the organic components of interest.
Each combined hexane and methylene chloride fraction was
then passed through a sodium sulfate drying column to remove the
last traces of water, and then solvent exchanged to hexane in
preparation for fractionation by column chromatography. Fraction
1 (Fl), the hexane eluant, would include aliphatic hydrocarbons
and PCB's, if these were present in the samples tested. The
hexane:benzene eluant would contain aromatic hydrocarbons varying
from toluene to polynuclear aromatics, if these were present in
the samples tested. The third fraction, the methylene
15

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chloride:methanol eluant, would contain polar acids and more polar
pesticides, if these were present in the samples tested.
Each of the fractions obtained with the extraction procedure
was analyzed by capillary column gas chromatography, utilizing
two detection techniques. Flame ionization detection was used to
screen for aliphatic and aromatic hydrocarbons and the more polar
phenol, carboxylic acid and ester components. These analyses
allowed determination of petroleum contaminants in the drilling
mud samples. These same extracts were subjected to electron
capture capillary gas chromatography, providing a screen of
chlorinated hydrocarbons such as PCBs and biocides including a
variety of chlorinated pesticides and herbicides as well as
phosphorous and nitrogen and/or sulfur containing compounds.
Fractions of particular interest were then subjected to
additional analyses by gas chromatography/mass spectrometry,
providing individual compound verification.
All gas chromatographic data were recorded and reduced to
digital format by computerized data reduction programs, and all
concentrations of resolved component peaks have been reported on
a microgram (or nanogram) per liter of bulk drilling mud samples.
Water content measurements were made so that conversions of
concentration data to dry weight base can be made; these data are
included in the elemental analysis results for each whole mud.
16

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Figure 2 summarizes the analytical scheme used for organic
measurement.
Particulate Bioassay Phase
The sample phases obtained after one hour settling in
seawater were subjected to continuous liquid/liquid extraction
for 24 hours using methylene chloride. Deionized water was added
to each sample volume (which was approximately 500 ml in each
case) prior to beginning extraction to provide sufficient volume
for the extractors to operate. Also, reagent grade sulfuric acid
was added to each sample to bring its pH to less than 2 prior to
extraction.
After 24 hours, each sample extract in methylene chloride
was concentrated to 1.0 ml using a Kuderna-Danish apparatus.
Each concentrate then underwent two solvent exchanges with 3 to 5
ml of hexane, and fractionated over activated silica gel in a 1-
cm x 19-cm column. Three fractions were obtained:
F1 - after 30 ml of hexane
F2 - after 45 ml of benzene/hexane (1:1)
F3 - after 60 ml of methanol/methylene chloride (1:1)
Each fraction was concentrated a final time to volumes ranging
from 0.25 ml to 1.0 ml by Kuderna Danish techniques.

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FIGURE 2, Analytical Scheme for Organics in Drill Muds
StflDla
u
b £
i5
41 iQuot 'or Ory
'4a1qn (X Uatar)
3atarwinit1oM
3rtm 51 z%
Analyfli
«iOM
Orrlnq/E* traction
35:69
0
-------
After final concentration, a three fraction analytical
scheme using GC and GC/MS instrumentation was performed as
described above for the whole drill fluid fraction.
Dissolved Bioassay Phase
The dissolved bioassay phaser obtained for each sample after
72 hour settling in seawater, centrifuging and filtering, was
extracted and concentrated just as described above for the
particulate bioassay phase. However, after solvent exchange to
hexane and final volume concentration to 100-300 ul, no further
fractionation was performed prior to GC and GC/MS analyses.
D. Data Presentation
Concentration
For each whole drilling fluid sample, heavy metal
concentrations are expressed as mass of metal per unit mass of
dry sediment (usually ug/g dry weight; weight percent for Al, Ba,
Ca, Fe). Table nAn for each sample contains these data and
includes a water content value (expressed as weight percent).
Whole drilling fluid heavy metal concentrations may be changed
from dry weight basis (i.e., ug/g dry mud or weight percent) to
wet weight values (i.e., ug/g wet fluid) by the following
conversion:
19

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ug metal/g balk drill fluid
. uq metal . g. dry mud	
g dry mud g bulk drill fluid
g. dry mud
" gVfgid * tl-
-------
All hydrocarbon concentrations are expressed in mass of
component/volume of bulk drill fluid (or volume of final bioassay
phase). As just described for heavy metal contents, conversions
can be made between mass/volume, mass/dry mass and mass/wet mass
concentrations using the measured water contents and an assumed
dry mud density of 2.5 g/ml (g/cm^).
Comparison With No. 2 Fuel Qil Analysis
In a companion report prepared by New England Aquarium
(NEA)(4)/ whole drilling fluids were also analyzed for
hydrocarbon contentf but a slightly different analytical approach
was used. Although several differences exist in the sample
extraction protoco.s, they probably account for only relatively
subtle differences in qualitative and quantitative results. Host
important is that the analytical hydrocarbon content data in this
report were derived from identification and quantitation of all
individual components recognizable by a combination of GC-FID and
GC/MS; the approach taken in the NEA study*4) was to identify and
quantitate only select components common to a No. 2 fuel oil
standard. A set of dominant chromatographic peaks found in the
No. 2 fuel oil standard were selected from each sample's profile,
quantitated and summed.
In general, results from the two analytical approaches
correlate well with each other producing a coherent trend in
21

-------
"hydrocarbon-type" contents among the production muds
characterized. Figure 3 plots the independently derived
concentrations of petroleum hydrocarbons (PHCs), as well as the
water contents of each sample. Although the muds used by both
laboratories were from common sources, the measured water
contents of each sample set were of the same trend but different
in value; since NEA's data are reported in mg/g wet weight and
SAI's in mg/mlf variations in water content are important. With
the exception of mud P3/ the two sets of data are comparable over
a broad range of hydrocarbon content levels.
Conversion of the two sets of data to common concentration
units (mg/ml or mg /g wet), as explained in the preceding
discussion, remove . most of the numerical variance between them.
However, there is a significant, although very consistent,
variation in water contents between the two sets of samples (see
Figure 3 and Tab.e 7) which is a factor in attempting to
normalize the data.
Table 8 compares, for each drill mud characterized,
petroleum hydrocarbon concentrations for whole, suspended and
dissolved phases (prepared as described for bioassay testing).
In general, the three phases trend in accordance to the levels
measured in the whole mud phase; notable exceptions are a
relatively high dissolved concentration for SV 76-2-5 and a
relatively low dissolved phase level for P-l. Presumably, these

-------
FIGURE 3. Fetroleim Hydrocarbon Concentrations (mg/ml whole mud)
and Water Contents (%) from this Study vs No. 2 Fuel Oil
Concentrations (rng/g wt. weight) and Water Contents from
NEA(4'. Data are for whole muds.
100/10
90/9
00/8
70/7
60/6
50/5
40/4
30/3
20/2
10/1
Whole Mud Analyses
X = FHC concentrations
• = % H2O (by weight)
X
X
•/
/
/
~
/
/
/
/
2 pi
P3
/
/
/
-X XX
© /
/
I	I	1	1	I	1	1	1	I	1	1	1	I	1	1	i_1	1	1	a	'	1	1	1	I	1	1	1	I	1	1—u
EHC(ir.q/ml) 1	2	3	4	5	6	7
H20 (%) 10	20	30	SAI 50	60	70
23

-------
TABLE 7. Comparative Whole Hud Hydrocarbon Concentration
and Water Content Data
1
1 Sample ID
I
I
I SAI(mg/ml)
1
I 1
1 sai %e2o I
NEA(mg/g wet)
1 !
i NSA %H20 I
1
1 AN31
I
I 0.90
j
I 1
1 66.7 I
1 j
1.18
1 I
I 49.9 I
I MIBLKA51
1 0.06
I
! 75.8 I
i ]
0.19
1 |
1 69.5 I
| |
I SV 76-2-5
i
1 1.93
i t
i 58.1 |
3.59
I |
1 27.3 |
j |
1 F~1
|
I
I 8.50
j
I |
I 59.9 I
I I
1 58.8 1
1 |
9.43
I 1
1 33.8 1
I P-2
I
1 P~3
i
I 1.33
j
2.14
| |
i 30.0 |
J I
[ 7.91
1
1 0.89
j
1 57.8 I
1 |
3.98
1 1
1 26.8 |
I I
I P-4
l
1 60.2 I
I !
0.67
1 1
I 33.5 1
I P-5
1
1 1.32
1 57.5 I
t i
1.41
| !
1 26.3 1
| 1
I P-6
1
I
I 0.J3
1 1
1 78.1 I
i i
0.10
1 1
1 71.5 1
1 1
I P-7
I
I 0.14
j
I 1
1 69.9 1
1 j
0.50
1 1
1 57.0 1
1 p-e
] 0.7 2-
I 58.1 I
0.56
| |
1 27.3 1
24

-------
TABLE 8. Comparative Hydrocarbon Concentrations in Whole,
Suspended and Dissolved Drilling Mud Biases* SAI data
are based on total resolved and unresolved aliphatic and
aromatic hydrocarbons; NEA data are based on chromatographic
comparison with No. 2 fuel oil standards.
1 1
1 Sample ml
SAI Whole Mud
fmg/1}
SAI Suspended
SAI Dissolved
(mg/H
NEA Suspended |
1
1 1
IMIBLKA51 |
j |
60
0.12
1.17
1
0.09 I
1
IA101-1-6 I
I j
900
0.42
1.38
0.61 I
1
ISV 76-2-51
1 1
1930
4.43
7.55
2.10 I
1
1 1
IP-1 1
1 |
8500
19.7
0.96
2.55 1
1
1 1
IP-2 |
1 1
1330
1.12
0.01
0.24 I
1
1 1
1P—3 1
1 1
7910
18.7
7.58
1.23 1
j
1 1
1P—4 1
| 1
890
0.90
0.01
0.10 1
1
1 1
IP-5 1
1 |
1320
5.11
1.33
0.13 1
1
1 1
IP-6 1
1 1
30
0.08
0.04
ND I
1
1 1
IP-7 1
1 1
140
0.09
0.18
0.07 I
I
1 1
|P-8 1
730
3.08
2.58
0.36 1
25

-------
variations are related to the exact nature of the dominant
hydrocarbon components and their varying solubilities are
particle/dissolved partitioning characteristics. NEA(4)
suspended phase hydrocarbon concentrations are also included in
Table 8; the significantly lower values result from using
selected aromatics in No. 2 fuel oil to quantitate these samples
rather than quantitating from total resolved and unresolved
components.
26

-------
References
^'u.S. EPA Region II Drilling Mud Bioassay Teat Procedures
(2)ePA Methods for Chemical Analysis of Water and Wastes Method
200-4.1.1 through 4.1.3 (In: EPA-600/4-79-Q20)(March 1979).
<3'standard Methods for Examination of Water and Wastewater, 15th
Edition, Methods 300D, 303AP 303C and 304 (American Public
Health Association: Washington D.C.)(1980).
(^A Survey of the Toxicity and Chemical Composition of Used
Drilling Muds. Final Report, Cooperative Agreement No.
CR806776, New England Aquarium, August 1, 1983.
27

-------
III. MUD IDENTIFICATION: MIBLKA51
LAB NUMBER	83-323
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	dissolved Bioassay Phase Organic Concentrations
23

-------
Ill A. DRILLING MUD ELEMENTAL CONCENTRATIONS
MIBLKA51 Al-7 (Sample I.D.: 83-323)
1
Element
—	
Whole Muda
Particulate Phase
Bioassay ^reDaration"
Di ssolved 3hase
3ioassay Preoaration3
A1
5.19(8)
473.
0.026
3a
9.85(S)
13.9
0.409
Cd
0.387
0.007
0.001
Ca
4.39(*)


Cr
337.
5.76
0.338
Cu
23.4
0.349
0.000
Fe
4.31(S)
546.
0.295
Pb
135.
1.41
0.011
Sr
510.
	
	
Zn
161.
2.76
0.001
h2o
75.sen


Concentrations expressed as ug/g dry weight unless otherwise indicated.
^Concentrations expressed as ug/g wet weight unless otherwise indicated.
29

-------
11 IB- WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic Fraction

Aromatic Fraction
Sample *
Resolved (mg/1)*
UCM (mg/1)

Resolved (mg/1)
UCM (mg/1)
MIBLKA51 Al-7
34.5
0

9.33
12.3
AN31-1-6
185.
419.

98.5
194.
1 gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
P-l
2,700.
4,200.

636.
96*.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
646.

207.
183.
P-6
10,1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.5
P-8
204.
270.

86.9
164.
*A11 concentrations expressed per unit volume of wet sample.
30

-------
Ill B. (cont.) WHOLt DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/1)*
Sample H
N-Cg
N-Cio
N-Cji
1100
N-Ci2
1540
nc13
N~C 14
N"C15
N"C16
N-C17
Pristane
925
N-Cis
1780
Phytane
NC19
MIBLKA51 Al-7

3640
1810
2030
2420
2420
2250
593
1330
AN 31-1-6
182
2600
3300
6440
8310
9790
13,600
14,000
10,800
7110
8780
4250
7880
Mil ye 1
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151,000
201,00Q
197,000
94.000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
I—»
P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
. 6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
Ill B. (
cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS
Sample #
n-c20
n-c2i
n-c22
n-c23
n-c24
n-c25
n-c26
n-c27
n-c28
n-c29
N-C30
K-Cji
1IBLKA51 A1-7
940
780
478
289
144
111
_
_
_
_
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
"
-
-
-
Nilgel
55
55
55
-
-
56
-
-
-
-
-
"
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
CO
*> P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
* -
-
-
-
-
P-6
393
353
327
322
268
283
234
A* 15
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
—
_


*A11 concentrations expressed per unit volume of wet sample.

-------
Ill B. (cont). MIBLKA51 Al-7 WHOLE DRILLING FLUID FRACTION CONCENTRATIONS
Compound Name
KOVAT No.
Concentration (ug/l)3'
Methyl ethyl benzene
960
42.2
Trimethylbenzene
991
37.6
Naphthalene
1179
13.9
2-Methylnaphthalene
1289
177.
1-Methyl naphthalene
1306
68.3
1,1' -Biphenyl
1375
20.4
•Dimethylnaphthalene
1400
241.
•Dimethyl naphthalene
1415
134.
•Dimethyl naphthalene
Methyl-1,1'-biphenyl
1434
56.1
1483
104.
Methyl ethyl naphthalene
1500
136.
•Trimethylnaphthalene
1522
74.8
•Trimethylnaphthalene
1527
135.
•Trimethylnaphthalene
1544
28.5
•Trimethylnaphthalene
1578
27.4
•Trimethylnaphthalene
1560
194.
•Methyl -(methylethyl)-Naphthalene
1647
53.1
•Methyl-(methyl ethyl)-Naphthalene
1668
92.5
Phenanthrene
1775
162.
Methyldi benzothi ophene
1849
35.8
•Methylphenanthrene
1890
113.
•Methylphenanthrene
1915
72.7
•Methylphenanthrene
1904
13.5
•Oimethylphenanthrene
2011
32.9
•Dimethylphenanthrene
2030
96.1
•Dimethylphenanthrene
2037
i
t
j
24.9
i
1
1
^Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. <0VAT index can be utilized for
comparison and evaluation of isomers among samples.
a
Concentration expressed per unit volume of wet sample.
33

-------
B

FIGURE HI B. CAPILLARY COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND
AROMATIC (B) FRACTIONS OF WHOLE DRILLING FLUID MIBLKA51 Al.

-------
IIIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mi 1 gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-l
6.43
7.78
14.2
P-2
0.694
0
0.594
P-3
4.35
11.45
15.8
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0
J
0.039
P-7
0.063
0
0.063
P-8
0.690
0.68
i
1.37
35

-------
inc. (WILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample H
MIBLKA51 A1-7
N-Cg
NC10
NC,,
0.29
nc12
NC13
NCi4
NC)5
NCJ6
NCi?

0.12
0.46
0.88
0.73
0.34
0.20
0.25
AN31-1-6
.....
2.3/
7.0
10.7
15.4
18.3
21.7
23.41
23.39
Mi 1 go 1
0.09
0.25
0.43
0.51
0.69
0.84
0.84
0.91
0.90
SV76-2 5
	
7.58
27.2
52.6
86.7
110
129
119
113
P-l
12.0
72.6
198
274
362
391
448
489
481
P-2
2.7
7.6
14
22
33
42
50
54
51
P-3

15
65
124
194
239
289
279
280
P-«
cr»
0.96
3.8
8.3
11
19
26
36
46
51
P-5

7.0
15
30
62
93
113
132
127
P-6
0.20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.57
P-7
... —
0.37
0.68
0.97
1.6
2.3
3.2
4.2
4.4
P-8
2.7
8.4
20
28
37
43
46
47
41

-------
Sample H
HIC. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Pristane NC13 Phytane NCjg ^20 "**21 ^22
MIBLKA51 Al-7

0.11
- i —

0.15


0.14
0.50
AN31-1-6
14.8
17.9
9.
0
15.1
9.
6
6.8
4.6
Mi lye)
0.45
0.70
0.
29
0.58
0.
39
0.28
0.21
SV/b-2-b
54.8
85.6
30.
1
66.6
43
4
33.0
20.6
F-l
142
368
119

302
203

143
78
P-2
30
41
lb

33
24

17
11
P-3
135
229
92

196
171

119
84
£ P-4
17
36
11

24
13

7.5
4.3
P-5
43
101
39

79
54

37
22
P-6
0.32
0.52
0.
17
0.61
0.
50
0.56
0.76
P-7
2.0
3.3
1.
2
2.5
1.
6
1.1
0.83
P-8
23
32
10

25
18

13
8.2

-------
inc.
DRILLING FIUID SUSPfcNDED SOLIDS -
Sample t
M1BLKA5I Al-7
AN31-1-6
Mi I gel
SV76-2-5
P-l
P-2
P-3
U>
CD p.4
P-5
P-6
P-7
P-8
NC
23
NC-
24
1.2
3.5
11.9
36
6.8
54
3.3
12
1 30
0.86
5.3
2.0
3.6
7.6
17
5.3
44
3.5
6.3
1.9
1.1
4.1
NC25
2.9
3.9
0.32
5.2
7
4.4
28
3.9
2.4
4.2
»
?
ALIPHATIC FRACTION CONCENTRATIONS (pg/1)
NC26 NC-27 NC28 NC29 NC3(j
4.3
4.3
4.2
26
4.3
1.9
6.0
5.1
4.8
5.8
4.2
3.0
3.0
3.8
2.8
3.2
3.2
3.4
2.6
2.5
3.1
2.7
2.1

-------
F1 (Aliphatic) Fraction
U>
kO
: b ;
R 5 i
I
I
L»
*
1
UM
ill
FIGURE III C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID MIBLKA51 Al-7.

-------
IIIC SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC -RACTIC^
Sample *
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBL:
-------
IIIC. MIBLKA51 Al-7 SUSPENOED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
2-Methylnapthalene
1290
0.46
1-Methylnapthalene
1306
0.25
~Dimethylnapthalene
1400
0.60
~Dimethylnapthalene
1415
0.56
~Dimethylnapthalene
1435
0.16
Methyl-1, 1'-biphenyl
1485
0.22
Menthylethylnaphalene
1502
0.23
~Trimethylnaphthalene
1524
0.22
~Trimethylnaphthalene
1528
0.34
~Trimethylnaphthalene
1544
0.19
*Trimethyl naphtha1ene
1561
0.57
~Methyl-(methyl ethyl)-Naphtha 1ene
1668
0.10
Phenanthrene
1775
0.45
~Methylphenanthene
1891
0.14
41

-------
F2 (Aronatic) Fraction
c
sc's
s i j •
SIR B f	i i 3
—i—K— # ^
CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID MIBLKA51 Al-7.

-------
IIIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
Resolved(ug/T)
Unresolved (ug/1}
Total (yg/1)
MIBLKA51 Al-7
25.0
0
25.3
AN 31-1-6
497
0
497
Mi 1 gel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-S
165
0
165
P-6
13.6
0
13.6
P-7
00
N
0
478
P-8
836
0
336
43

-------
I
fit t
-	I
¦t*
4*
I
2 S
« J


F3 (Polar) Fraction
FIGURE 1IIC.
CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID MIBLKA5I Al-7.

-------
HID. DISSOLVED BIOASSAY PHASE - TOTAL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Samole #
Total Resolved Components
(mg/1)
Total Unresolved Components
(mq/l)
MIBLKA51 Al-7
. 358
.813
AN 31-1-5
.136
1.24
Mi 1 gel
.0783
0
SV76-2-5
.920
6.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
= -5
.166
1.16
?-6
.043
0
P-7
.175
0
P-8
.161
2.42
Concentrations expressed per unit volume of wet sample.
Dissolved Bioassay Phase sample were not fractionated into
alipnatic (PI), aromatic (FZ) or polar (F3) fractions due
to the chromotographic simplicity of the samples.
£ 5

-------
HID (cont). MIBLKA51 Al-7 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
iompound Name
KOVAT No.
Concentration {-.q/
Cy-Alcohol
Cg-A1coho1
Ethylhexanol
C9-Ketone
Benzoic Acid
C^-Ketone
Molecular Ion m/e = 170
Molecular Ion m/e = 199
Cig-Alcohol
C^g-Carboxylic Acid
Cxg-Carboxylic Ac i d
C2(j-Carboxylic Acid
911
1023
1041
1065
1223
1495
1552
1676
2081
2168
2302
2445
1.4
26.0
1.6
1.0
5.8
.2
3.5
5.2
.8
.8
.2
6.5
'Concentrations expressed per unit volume of wet sample.
46

-------
f	fL ^ • J	«
~ ^5 j j f f - k
lm *	« *
CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "DISSOLVED PHASE" BIOASSAV
OF SPENT DRILLING FLUID MIBLKA51 A1.
PREPARATION

-------
MUD IDENTIFICATION: AN 31-1-6
LAB NIMBER	83-324
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Btoassay Phase Organic Concentrations
D.	Dissolved Bloassay Phase Organic Concentrations

-------
IV A. DRILLINS. MUD ELEMENTAL CONCENTRATIONS
AN 31-1-6 (Sample I.D.: 83-324)
Element
Whole Muda
Particulate Phase
Bioassay Preparation13
Dissolved Phase
Bioassay Preparatio
A1
3.74U)
i
1
1206.
0.079
6a
21.8(%)
15.0
0.469
Cd
2.38
0.076
0.005
Ca
1.57(55)

	
Cr
774.
828.
1.15
Cu
33.6
2.56
0.098
Fe
2.68(%)
1565.
1.09
Pb
142.
1.20
0.040
Sr
538.
	
	
Zn
247.
14.5
0.526
H20
66.7 (%)


Concentrations expressed as yg/g dry weight unless otherwise indicated.
^Concentrations expressed as ug/g wet weight unless otherwise indicated.
49

-------
IV B. WHOLE MUD - RESOLVED ANO UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic Fraction

Aromatic Fraction
Sample #
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
UCM (mg/1)
MIBL.KA51 Al-7
34.5
0

9.33
¦2.3
AN31-1-6
185.
419.

98.5
194.
Mil gel
.004
0

.004
0
SV76-2-5 *
464.
966.

166.
330.
P-I
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
4A5.
P-4
132.
548.

106.
103^
P-5
284.
646.

207.
183.
?-6
10.1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
P-3
204.
270.

36.9
164.
*A11 concentrations expressed per unit volume of wet sample.
50

-------
IV B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/U*
Sample §
N-Cg
N-C10
N-Cn
N-Ci?
N"cl 3
N~C 14
N"C15
«C16
N-C17
Pristane
N-Cjb
Phytane
N-C,9
HIIH.KA51 Al-7

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-1-6
182
2600
3300
6440
8310
9790
13,600
14,000
10,800
7110
8780
4250
7880
Mil ye1
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101.000
112,000
141,000
151,000
201,000
197,000
94,000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
cn
- P-3

5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
IV B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/1)*
Sample H
N C2Q
n-c21
n-c22
n-c23
h-c24
n-c25
NC26
i
r>
ro
n-c28
n-c29
N-C^
N"C31
MIBLKA51 A1- 7
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-
-
Mi 1 gel
55
55
55
-
-
56
-
-
-
-
-
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
S P"2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
-
P-6
393
353
32/
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
-
-
-
-
*A11 concentrations expressed per unit volume of wet sample.

-------
IV 3 (cont.) AN31-1-6 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
Methyl ethyl benzene
~Trimethylbenzene
*Trimethy1benzene
~Methyl propyl ben zene
*01 me t hy 1 et hy 1 ben ze ne
~Methyl propyl benzene
~Dimethylethyl benzene
Methyl-(methyl ethyl)-benzene
Dimethyl propyl benzene
~Tetramethylbenzene
Methylpropenylbenzene
~Tetramethylbenzene
Naphthalene
2-Methylnaphthalene
1-Methylnaphthalene
1 .l'-Biphenyl
•Dimethyl naphthalene
~Dimethyl naphthalene
~Dimethylnaphthalene
~Oimethylnaphthalene
Methyl-1,1'-biphenyl
Me^hyl^thy-lnaphthalene
*Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimehtylnaphthalene
~Methyl -(methylethy1)-Naphthalane
~Methyl-(methyl ethyl)-Naphtha; sne
Phenanthrene
Methyldi benzothiophene
~Methylphenanthrene
~Methylphenanthrene
~Dimethylphenanthrene
~Oimethylphenanthrene
~Dimethylphenanthrene
KOVAT No
Concentration (ug/l)a
77.8
164.
136.
157.
111.
' 75.2
251.
177.
306 *
207.
383.
92.8
391.
2720.
3600.
3845.
3082.
4130.
478.
202.
1790.
1570.
1320.
2560.
739.
727.
1100 .
923.
1110.
872.
761.
794.
1160 .
464.
1010 .
351 .
~Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
^Concentrations expressed per unit volume of wet sample.
53

-------
FIGURE IV B, CAPILLARY COLUMN GAS CHRQMATOGRAMS OF THE ALIPHATIC (A) AND
AROMATIC (B) FRACTIONS OF WHOLE DRILLING FLUID AN31-1-6.

-------
IV C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample 4
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
i 0.325
Mi 1 gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-l
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
o
0.462
P-5
1.55
2.19-
3.74
P-6
0.039
0
0.039
P-7
0.063
0
0.063
P-8
0.690
0.68
1
1.37
55

-------
IV C. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (py/I)
Sample H
n-c9
NCjo
NC,i
NC,2
NCn
nc14

NC|6
NC,?
MIBLKA51 Ai-/

0)2
0.29
0.46
0.88
0.73
0.34
0.20
0.25
AN31-1-6

2.37
7.0
10.7
15.4
18.3
21.7
23.41
23.39
Mi igel
0.09
0.25
0.43
0.51
0.69
0.84
0.84
0.91
0.90
SV76-2-5

7.58
27.2
52.6
£J6. 7
110
129
119
113
P-l
12.0
/2.6
198
274
362
391
448
489
481
P-2
2.7
7.6
14
22
33
42
50
54
51
P-3

15
65
124
194
239
289
279
280
P-4
0.96
3.8
8.3
11
19
26
36
46
51
°>-5

7.0
15
30
62
93
113
132
127
P-6
0.20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.57
P-7

0.37
0.68
0.97
1.6
2.3
3.2
4.2
4.4
P-8
2.7
8.4
20
28
37
43
46
47
41

-------
IV C. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample #
Pristane
NC|8
Phytane
nc19
nc20
nc2,
nc22
MIBIKAS1 A1 - 7

0.11

0.15

0.14
0.50
AN31-1-6
14.8
17.9
9.0
15.1
9.6
6.8
4.6
Milye1
0.45
0.70
0.29
0.58
0.39
0.28
0.21
SV/6-2-S
54.8
85.6
30.1
66.6
43.4
33.0
20.6
P-l
142
368
119
302
203
143
78
P-2
30
41
15
33
24
17
11
P-3
135
229
92
196
171
119
84
1
a.
57
17
36
11
24
13
7.5
4.3
P-5
43
101
39
79
54
37
22
P-6
0.32
0.52
0.17
0.61
0.50
0.56
0.76
P-7
2.0
3.3
1.2
2.5
1.6
1.1
0.83
P-8
23
32
10
25
18
13
8.2

-------
IV c.
DR11IING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (pg/1)
Sample H
nc23
N( 24 '
NC25
NC26
nc27
CO
CNJ
nc29
NC30
NCjl
NC32

MIBLKA5I A1 -7
1.2
2.0
2.9








AN31-1-6
3.5
3.6
3.9
4.3
6.0


	

	

Milgol

	
0.32
__ ...
	
	

	
—
	.

SV76 2-5
11.9
7.6
5.2
4.3
5.1
3.0
3.2
2.5

.	

P-l
36
17
7

„




	

P-2
6.8
5.3
4.4
4.2
4.8
3.0
3.2
3.1
		.


P-3
54
44
28
26


T _
		
	...
	

P-4
en
00 P-5
3.3
12
3.5
6.3
3.9
4.3
5.8
3.8
3.4
2.7
... .


P-6
1.3D
1.9
2.4
1.9
4.2
2.8
2.6
2.1
1.9


P- 7
0.86
1.1




__




P-8
5.3
4.1
4.2

	
	
—
	
	



-------
cn

F1 (Aliphatic) Fraction
* t
i i
i i
: t
r c

FIGURE IV C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID AN 31-1-6.

-------
IV C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBL.KA51 Al-7
.072
0
.073
AN 31-1-6
.088
0
.089
Mi 1 gel
.15
0
.147
SV76-2-5
.48
. ^33
.912
?-l
2.5
3.060
5.53
9-2
.29
.134
.426
P-3
1.36
1.50
2.86
P-A
.28
0.17
.442
P-5
cc
< W V
1.83
1.37
P-6
.038
o
.038
P-7
.030
0
.030
P-3
1.1C
0.61
1.71
63

-------
IVC. an 31-1-6 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATION
Compound Name
KOVAT #
Concentration (ug/1)
~Trimethylbenzene
991
0.38
*Trimethylbenzene
1020
0.38
~Dimethylethylbenzene
1083
. 0.39
Methyl-(methyl ethyl)-benzene
1103
0.14
Dimethyl propyl benzene
1112
0.37
~Tetramethylbenzene
1116
0.32
Methylpropropeny1 benzene
1145
0.34
Naphthalene
1178
1.1
2-Methylnaphthalene
1290
5.0
1-methylnaphthalene
1306
2.6
~Dimethyl naphthalene
1419
0.63
~Dimethyl naphthalene
1400
2.5
~Dimethyl naphthalene
1435
0.63
Methyl-1,1"-biphenyl
1485
0.55
Methyl ethyl naphthalene
1501
0.39
~Trimethylnaphthalene
1528
0.50
~Trimethylnaphthalene
1546
0.16
61

-------
F2 (Aromatic) Fraction
CT\
ro
FIGURE IV C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID AN 31-1-6.

-------
IV c. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
Resolved(ug/1)
Unresolved(ug/1)
Total (Mg/1)
MIBLKA51 Al-7
25.0
0
25.0
AN 31-1-6
497
0
497
Mllgel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
0
165
P-6
13.6
0
13.6
P-7
478
0
478
P-8
836
0
336
63

-------
F3 (Polar) Fraction

CAPILLAR* COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID AN 31-1-6.

-------
IV D. DISSOLVED BIOASSAY PHASE - TUTAL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Components
(roq/1)
MIBLKA51 Al-7
.358
.813
AN31-1-6
.136
1.24
MUgel
.0783
0
SV76-2-5
.920
5.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
P-5
.166
1.16
P-6
.043
0
P-7
.175
0
P-8
.161
2.42
*Concentrations expressed per unit volume of wet sample.
Dissolved Bioassay Phase sample were not fractionated into
alipnatic {FI), aromatic (F2) or polar (F3) fractions aue
to the chromotographic simplicity of the samples.
65

-------
IV D. (cont.) AN31-1-6 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Name
KOVAT No
Concentration
C7-A1coho1
Cg-Alcohol
Benzoic Acid
Methoxybenzaldehyde
C^-Ketone
Molecular Ion m/e = 170
Methoxybenzoic Acid
Molecular Ion m/e = 199
Hexadecanoic Acid
C^g-Carboxylic Acid
C2Q-Carboxylic Acid
910
1023
1214
1418
1500
1552
1591
1681
1984
2164
2454
2.1
11.4
.9
2.5
1.0
.5
4.1
20.8
2.3
.6
3.5
aConcentrations expressed per unit volume of wet sample.
66

-------
I
""" " D'	°F THE "D,ssol#ED »>»««» mm*,m
w

-------
V. MUD IDENTIFICATION: MILGEl® (Additive)
LAB NUMBER	83-325
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bioassay Phase Organic Concentrations
D.	Dissolved Bioassay Phase Organic Concentrations
£8

-------
V A. DRILLING MUD ELEMENTAL CONCENTRATIONS
MILGEL® ADDITIVE (Sample I.D.: 83-325)
Element
Whole Muda
Particulate Phase
Bioassay Preparation®
Dissolved Phase
Bioassay Preparation
AT
8.86(%)
2741.
0.020
Ba
0.064(%)
30.9
2.60
Cd
0.494
0.095
0.007
Ca
0.470(%)

	
Cr
8.02
0.689
0.287
Cu
8.18
1.17
0.002
Fe
3.75(55)
1992.
0.081
Pb
27.1
1.54
0.003
Sr
60.5
	
	
Zn
66.5
11.2
0.054
h2o
—
i

Concentrations expressed as yg/g dry weight unless otherwise indicated
'Concentrations expressed as ug/g wet weight unless otherwise indicated
69

-------
V B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic Fraction

Aromatic Fraction
Sample #
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
UCM (mg/1)
MIBLKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mil gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
P-l
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
646.

207.
183.
P-6
10. i
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
2-3
204.
270.

86.9
164.
*A11 concentrations expressed per unit volume of wet sample.
70

-------
v B- Uont.) WHOLE DRILLING FLUID - ALIPHAIIC FRACTION CONCENTRATIONS (ug/1)*
Sample tf
N-Cq
N-C10
N-Cn
N-C^
N"Cl3
n-c14
N_C15
N"C16
N C]7
Prlstane
N-Cia
Phytane
N-C,9
MIBLKA51 Al-7
.
3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-1-6
18?
2600
3300
6440
8310
9/90
13,t; "•
14,000
10,800
7110
8780
4250
7880
Mi 1 gel
55
b40U
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22.900
7960
19,200
P-l
3450
28,400
101,000
112,000
141.000
151,000
201,000
197,000
94,000
42,900
148.000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10.100
P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
2 P 4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
V B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (pg/1)*
Sample H
n-c20
N~C2l
n-c22
n-c23
n-c24
1
CNJ
n-c26
n-c27
n-c28
N-c29
N-C30
N*C31
MIBLKA51 A1-/
910
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-

Mi lye 1
55
55
55
-
-
56
-
-
-
-
-
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719

^ p_3
ro ¦ J
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
"
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
"
P-6
393
353
327
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
~
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
-
-
-
_
*A11 concentrations expressed per unit volume of wet sample.

-------
V B(cont). MILGEL* ADDITIVE WHOLE SAMPLE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
Methyl ethyl benzene
Trimethylbenzene
Naphthalene
2-Methylnaphthalene
1-Methylnaphthalene
~Dimethylnaphthalene
~Dimethyl naphthalene
KOVAT No
Concentration (ug/1)
66.5
52.1
14.0
29.8
16.1
18.1
17.8
~Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
aConcentua.ijons expressed per unit volume of wet sample.
73

-------
I

I i
d i- JI|m- I
JUUi-i

I 1
•» /*- V
I	km i* m
• ' 'W'' 4Ul
FIGURE V B. CAPILLARY COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND
AROMATIC (B) FRACTIONS OF BULK MILGEL®.

-------
V C. SUSPENDED PHASE. - RESOLVED ANO UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
Resolved(ug/1)
Unresolved(ug/1)
Total (ug/1)
MIBLKA51 Al-7
25.0
0
25.0
AN 31-1-6
497
0
497
Mllgel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
0
165
P-6
13.6
0
13-6
P-7
478
0
478
P-8
836
0
836

-------
F3 (Polar) Fraction
FIGURE V C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID MILGEL®.

-------
V C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTI
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mi 1 gel
C. 016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-l
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0
0.039
P-7
0.063
0
1
0.063
P-8
C. 690
C. 68
1.37
77

-------
V
C.
DRILLING FLUIO
SUSPENDED
SOLIDS - ALIPHATIC TRACTION CONCENTRATIONS (y
-------
V C. DRILLING FLUID SUSPENDED SOLIDS
Sample $
MIBLKA51 Al-7
AN31-1-6
Milgel
Pristane NCjq	Phytane NCjg
O.ll			0.15
14.B 17.9	9.0	15.1
0.15 0.70	0.29	0.58
SV76-2-5
P-l
P-2
P-3
P-4
P-5
P-6
P-7
P-8
54.8
142
30
135
17
43
0.32
2.0
23
85.6
368
41
229
36
101
0.52
3.3
32
30.1
119
15
92
11
39
0.17
1.2
10
66.6
302
33
196
24
79
0.61
2.5
25
ALIPHATIC FRACTION CONCENTRATIONS (ug/1)
nc20	nc21	nc22
_	0.14	0.50
9.6	6.8	4.6
0.39	0.28	(L21	
43.4	33.0	20.6
203	143	78
24	17	11
171	119	84
13	7.5	4.3
54	37	22
0.50	0.56	0.76
1.6	1.1	0.83
18	13	8.2

-------
DRILLING FLUID SUSPENDED SOLIDS
Sample $
Nc23
NC
24
NC25
M1DLKA51 A1-7
AN31-1-6
MI Igel
SV76-2-5
P-l
P-2
P-3
P-4
P-5
P-6
P-7
P-8
1.2
3.5
11.9
36
6.8
54
3.3
12
1.30
0.86
5.3
2.0
3.6
7.6
17
5.3
44
3.5
6.3
1.9
1.1
4.1
2.9
3.9
0.32
5.2
7
4.4
28
3.9
2.4
4.2
ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
NC26 NC27 NC28 NC?9 NC3(j
4.3	6.0	_		
i
4.3	! 5.1	3.0	3.2	2.5
4.2	4.8	3.0	3.2 3.1
26 					
4.3	5.8	3.8	3.4	2.7
1.9	4.2	2.8	2.6	2.1

-------

fl (Aliphatic) Fraction
« 8 1 2 !! * s I t
i *« « " ! ? * « » t *
Ifiiilljit''
r
-i— >
CO
FIGURE V C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID MILGEL®.

-------
I
VC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
I
Sample *
Resolved Cmg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
.088
0
.089
Mi lgel
.-•5
0
.147
SV76-2-5
.48
.£¦33
.912
P-l
2.5
3.060
5.53
P-2
.29
. 134
.426
F-3
1.36
1.50
2.86
P-4
.28
0.17
.442
P-5

1.83
1.37
?-6
. C2S
0
.038
P-7
. C30
C
.030
P-8
1. ;C
0.61
1.71

i

32

-------
»
V C. MILGEL® ADDITIVE SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
Naphthalene
1178
0.30
2-Methylnaphthalene
1290
0.40
1-Methyl naphthalene
1307
0.21
~Dimethynaphthalene
1401
0.12
*Dimethynaphthal ene
1416
0.34
33

-------
935
-mi r
ft
F2 (Aromatic) Fraction
\V
afcftffcaiisi** w sIr c se 7 * % 5
""" "'Us?::*? # s'l: j #* j k < I
*3-
co
FIGURE V C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID MILGEL®.

-------
V D. DISSOLVED BIOASSAY PHASE - TUTAL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS4
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Componei
(mg/1)
MIBLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
'6.63
P-l
.358
.'603
P-2
.005
CO
o
o
P-3
1.09
6.49
P-4
CM
O
O
.011
P-5
.166
1.16
P-6
.043
0
P-7
.175
0
P-8
.161
2.42
Concentrations expressea per unit volume of wet samole.
Dissolvea Bioassay Phase sample were not fractionated into
a-'.ohatic (F1). aromatic (F2) or polar (F3) fractions due
tc the chromatographic simplicity of the samples.
35

-------
V D (cont.) MILGEL* ADDITIVE SAMPLE
- DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Name

KOVAT No.
Concentration ;_a/i
Cy Alcohol

909
.3
Cg-Alcohol

1022
7.6
Ethylhexanol

1034
¦ .4
Cg-Ketone
Benzoic Acid
Methoxybenzaldehyde
Molecular Iorr m/e - 170
Methoxybenzoic Acid
Molecular Ion m/e » 199
Cig-Carboxylic Acid
CjQ-Carboxylic Acid
1065
1219
1413
1556
1600
1674
2159
2443
.1
4.4
1.7
.1
.3
.1
.5
.2

oncentrations expressed per unit volume of wet sample.
86

-------
00
* M
t * * 2 r
iii ! i t
IkUUli
FIGURE V 0. ^»«J#C01UJ« W CHROMATOGRAM Of THE -OISSOIVED PHASE" eiOASSAY PREPARATION

-------
MUD IDENTIFICATION: SV 76-2-5
LAB NUMBER	83-326
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	Dissolved Bioassay Phase Organic Concentrations
83

-------
VI A. DRILLING MUD ELEMENTAL CONCENTRATIONS
SV 76-2-5 (Sample I.D.: 83-326)
Element
Whole Muda
'
Particulate Phase
3ioassay Preparation"
Dissolved Phase
Bioassay Preoaration'
A1
0.61(2)
482.
0.030
3a
37.5(S)
12.5
0.407
Cd
1.62
0.315
0.009
Ca
0.82(S)
>
	
Cr
1345.
457.
43.6
Cu
86.1
15.0
1.27
Fe
3.63(2)
1975.
1.85
Pb
151.
18.4
0.161
Sr
536.
	
	
Zn
495.
93.1
0.487
O
CM
1
58.1 (*)
. -


Concentrations exDressed as ug/g dry weight unless otherwise indicated.
^Concentrations expressed as ug/g wet weight unless otherwise indicated.

-------
VI B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

AT iphatic
Fraction

Aromatic Fraction
Sample #
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
UCM (mg/1 ¦
MIBLKA51 Ai-7
34,5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mi 1 gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
F-l
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
646.

207.
183.
P-6
10.1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
P-8
204.
270.

86.9
164.
*A11 concentrations expressed per unit volume of wet sample.
90

-------
VI B. (cont.) WHOLt DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ng/1)*
Sample #
n-c9
N-C10
N-CU
N-C12
N"C13
N~C 14
N"C15
NC16
N-C17
Pristane
n-C,8
Phytane
n-c19
MIBLKA51 AI-7

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN3I-1-6
IB2
2600
3300
6440
8310
9790
1? "00
14,000
10,800
7110
8780
4250
7880
Milge1
55
5400
137
91
]H2
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151,000
201,000
197,000
94,000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
^ P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
VI B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (mQ/D*
Sample if
NC20
n-c2i
n-c22
N-C23
n-c24
n-c25
n-c26
N-C27
n-c28
n-c29
N-Cjo
n-c31
NIBLKAS1 At-/
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-
-
M11ge1
55
55
55
-
-
56
-
-
"
-
-
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
P-2
P-3
P-4
ro
P-5
P-6
P-7
P-8
96,400
8000
53,700
4280
11.400
393
1550
4260
65,700
6380
44,600
2520
7900
353
1120
3060
41,300
4730
34,800
1580
5440
327
744
1860
23,300
3320
23,300
1060
3270
322
434
1040
10,700
2050
14,500
728
1480
268
234
518
5090
1810
8860
615
283
299
1040
6540
458
234
949
716
315
398
461
141
795
655
207
719
118
144
*A11 concentrations expressed per unit volume of wet sample.

-------
VI B (cont). SV76-2-5 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
Methylethylbenzene
~Trimethylbenzene
~Trimethylbenzene
Methylpropylbenzene
*0 i me t hy 1 et hy 1 ben zene
~Dimethyl ethyl benzene
Methyl-(methyl ethyl)-benzene
Dimethyl propyl benzene
~Tetramethylbenzene
Methylpropenylbenzene
~Te t rame t hy 1 be n zen e
Naphthalene
2-Methylnaphthalene
1-Methyl naphthalene
1,1'-Bi Dheny1
*Dimethylnaphthalene
~Dimethyl naphthalene
~Dimethylnaphthalene
~Dimethyl naphthalene
Methyl-1,1'-biphenyl
Methyl ethyl naphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Methyl -(methylethyl)-Naphthalene
KOVAT No
952
986
1015
1045
1052
1078
1098
1109
1113
1141
1144
1178
1291
1307
1391
1402
1418
1437
1452
1484
1503
1525
1530
1546
1580
1649
Concentration (ug/1)a
129
730
288
218
184
401
257
467
551
522
150
1290
9430
5020
3120
8950
6320
2740
2620
1790
2830
2660
4280
1500
1020
1290
~Methyl -(methylethyl)-Naphthalene
1671
1720
Phenanthrene
1779
2590
Methyldibenzothiophene
1853
1280
~Methylphenanthrene
1895
1900
~Methylphenanthrene
1920
1650
~Dimethylphenanthrene
2017
918
~Dimethylphenanthrene
2036
1860
~DimethylDhenanthrene
2042
598
~Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
Concentrations expressed per unit volume of wet sample.
93

-------
FIGURE VI B. CAPILLARY COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND
AROMATIC (B) FRACTIONS OF WHOLE DRILLING FLUID SV76-2-5.

-------
VIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mil gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-l
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
o
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0
0.039
P-7
0.063
0
0.063
P-8
1
0.690
0.68
1.37
I
95

-------
VI
C. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample H
n-c;9
o
f
i
NCn
N(-I2
NC13
NCM
"cl5
NCi6
NC17
MIBIKA51 Al-7
—
0.12
0.29
0.46
0.88
0.73 .
0.34
0.20
0.25
AN31-1-6
—
2.37
7.0
10.7
15.4
18.3
21.7
23.41
23.39
Mi 1 gel
0.09
0.25
0-43
0.51
0.69
0.84
0.84
0.91
0.90
SV76-2-5
	.
7. 58
27.2
52.6
1)6.7
110
129
119
113
P-1
12.0
72.6
198
274
362
391
448
489
481
P-2
2.7
7.6
14
22
33
42
50
54
51
P-3
— ...
15
65
124
194
239
289
279
280
P-4
0.96
3.8
8.3
11
19
26
36
46
51
P-5
—
7.0
15
30
62
93
113
132
127
P-6
0.20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.57
^ P-7
	
0.37
0.68
0.97
1.6
2.3
3.2
4.2
4.4
P-8
2.7
8.4
20
28
37
43
46
47
41

-------
VI c. DRILLING FLUID SUSPENDED SOLIDS
Sample #
MIBLKA51 Al-7
AN31-1-6
Mi lye I
SV76 2-5
P-l
P-2
P-3
P-4
P-5
P-6
p-;
P-8
Pristane NC|3 Phytane NCjg
		O.ll	__	0.15
14.8	17.9	9.0	15.1
0.45	O.YO	0.29 0.58
54.8	85.6	30.1	66.6
142	368	119	302
30	41	15	33
135	229	92	196
17	36	11	24
43	101	39	79
0.32 0.52	0.17 0.61
2.0	3.3	1.2 2.5
23	32	10	25
ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
nc20 nc2] nc22
	
0.14
0.50
9.6
6.8
4.6
0.39
0.28
0.21
43.4
33.0
20.6
203
143
78
24
17
11
171
119
84
13
7.5
4.3
54
37
22
0.50
0.56
0.76
1.6
1.1
0.83
18
13
8.2

-------
VI C. DRILLING FLUID SUSPENDED SOLIDS
bt)ni|j|e ff
AH31-1-6
Mi I gel
SV76-2-5
P-l
P-2
P-3
P-4
P-5
SP-6
P-7
P-8
		
nc23
7
1.2

3.5

11.9

36

6.8

54

3.3

12

1.30

0.86

5.3
NC
24
NC25
2.0
3.6
7.6
17
5.3
44
3.5
6.3
1.9
1.1
4.1
2.9
3.9
0.32
5.2
7
4.4
28
3.9
2.4
4.2
ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
NC26 nc27 nc28 nc29 nc3(j nc31 NC32
4.3	6.0								
4.3	5.1	3.0	3.2	2.5
4.2	4.8	3.0	3.2	3.1
26							_		
4.3	5.8	3.8	3.4	2.7	__
1.9	4.2	2.8	2.6	2.1	1.9

-------
83 - 326 R
vV
LP
F1 (Aliphatic) Fraction
« ? i m i?
3 i i 5 P CC
FIGURE VI C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENOED PHASE" BIOASSAY PREPARATION OF
SPENT ORILLING FLUID SV76-2-5.

-------
VI C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS AROMATIC FRACTION
Sample *
Resolved (mg/1)
Unresolved (mg/1) ! Total (mg/1)
MIBLKA51 Al-7
AN 31-1-6
MiIgel
SV76-2-5
3.060
100

-------
VI c. SV76-2-5 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
Methyl propyl benzene
1045
1.56
~Tetramethy1 benzene
1113
0.74
~Tetrymethylbenzene
1146
0.95
Naphthalene
1179
8.82
2-Methylnaphthal ene
1291
44.4
1-Methynaphthalene
1307
29.9
1,1'Biphenyl
1390
10.1
~Dimethyl naphthalene
1402
34.0
~Dimethyl naphthalene
1417
24.6
~Dimethyl naphthalene
1436
10.3
~Dimethyl naphthalene
1452
9.2
Methyl-1,11-biphenyl
1485
7.6
Methyl ethyl naphthalene
1502
7.6
~Trimethyl naphthalene
1524
8.2
~Trimethy1naphthalene
1529
11.7
~Trimethyl naphthalene
1545
5.7
~Methyl-(methylethyl)-Naphthalene
1648
2.6
~Methyl-(methyl ethyl)-Naphthalene
1669
3.6
~Methylphenanthrene
1897
3.5
~Methylphenanthrene
1921
1.2
~Dimethylphenanthrene
2038
0.64
~Dimethylphenanthrene
~
~
2044
i
0.30
101

-------
83 - 326 f?
F2 (Aromatic) Fraction
FIGURE VI C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID SV76-2-5.

-------
VI C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR TRACTION
Sample #
Resolved (ug/1)
Unresolved(ug/1)
Total (ug/1)
MIBLKA51 Al-7
25.0
0
25.0
AN 31-1-6
497
0
497
Mi 1 gel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
0
165
P-6
13.6
0
13.5
P-7
478
0
CO
f^.
P-8
836
0
836
103

-------
83 - 326 y 3
F3 (Polar) Fraction
FIGURE VI C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID SV76-2-5.

-------
VI D. DISSOLVED BIOASSAY PHASE - TUTAL RESOLVED A.H0 UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Components
(mg/1)
MISLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mi 1 gel
.0783
0
SV76-2-5
.920
'6.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
P-5
-166
1.16
P-6
.043
0
P-7
.175
0
P-8
.161
2,42
^Concentrations expressed per unit volume of wet sample.
Dissolves Bioassay Phase sample were not fractionated into
alipnafic (F1}, aromatic {F2; or polar (F3) fractions Que
to the chromatographic simplicity of the samples.
105

-------
VI D (cont.) SV76-2-5 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Name
KOVAT No.
icncentration (ug/';a
C7-Alcohol
Cg-Alcohol
Ethylhexanol
Cg-Ketone
Benzoic Acid
Methoxybenzaldehyde
C^3-Ketone
Molecular Ion m/e » 170
Methoxybenzoic Acid
Molecular Ion m/e = 199
Hexadecanoic Acid
Cjg-Alcohol
C^g-Carboxylic Acid
C2Q-Carboxylic Acid
912
1021
1033
1065
1225
1411
1496
1560
1593
1676
1975
2066
2161
2442
39.5
33.9
5.9
20.4
13.8
24.8
'.7.5
35.0
59.7
28.3
1.0
1.8
6.3
10.3
a
Concentrations expressed per unit volume of wet sample.
106

-------
•5 % • i i *.l
!j« J I 8 3 J
i
I
i
^liJflofoFSPOT ffif;G6FSl2FsI56-?JSSOLVED PHASE" BI0ASSAY

-------
MUD IDENTIFICATION: PI-1-3
LAB NUMBER:	83-2000
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	Dissolved Bloassay Phase Organic Concentrations
103

-------
VII A. DRILLING tlUD ELEMENTAL CONCENTRATIONS
Pl-1-3 (Sample I.D.: 83-2000)
Element
Whole Muda
Particulate Phase
Bioassay Preparation"
Dissolved Phase
Bioassay Preparation
A1
1.01(2)
555.
0.047
Ba
36.9(3)
10.7
0.460
Cd
1.85
0.260
0.004
Ca
0.86(%)
	
	
Cr
814.
221.
3.34
Cu
62.3
15.9
0.119
Fe
3.44(%)
1566.
1.49
Pb
129.
13.3
0.093
Sr
303.
	

Zn
410 .
52.5
0.075
h2o
59.9 (%)
	
1
	
Concentrations expressed as ug/g dry weight unless otherwise indicated.
^Concentrations expressed as yg/g wet weight unless otherwise indicated.
1C 9

-------
VII B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

AT iphatic
Fraction

Aromatic Fraction
Sample 4
Resolved (mg/l)
IICM (mg/l)

Resolved (mg/l)
UCM (mg/l)
MIBLKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mil gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
P-l
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
646.

207.
183.
P-6
10.1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
P-8
204.
270.

86.9
164.
*A11 concentrations expressed per unit volume of wet sample.
110

-------
VII B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/1)*
Sample #
n-c9
NC10
N-C,i
N-C12
N"C13
n-cm
N-C15
N"C16
N-C17
Pristane
N-Cla
Phytane

MIBLKA51 Al-7

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-1-6
182
2600
3300
6440
8310
9790
13,600
14,000
10,800
7110
8780
4250
7880
Milgel
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36 , 500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151,000
201,000
197,000
94,000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
^ P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
" P-4
181
1650
3170
36 40
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
VII B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (m9/U*
I
Sample #
0
CSJ
(->
1
NC21
n-c22
NC23
n-c24
n-c25
n-c26
n"C27
n-c28
n-c29
N-Cjq
NC31
M1BLKA51 Al-7
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
"
-
Milgel
55
55
55
-
-
56
-
-
-
-
"
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
^ P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
-
P-6
393
353
327
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
-
-
-
~
*A11 concentrations expressed per unit volume of wet sample.

-------
VII B. (cont.)P-l WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Comoound Name
KOVAT No
Concentration (yg/1
Methyl ethyl benzer\e
*Trimetnylbenzene
*Trimethylbenzene
*Methylpropyl benzene
Dimethyl ethyl benzene
*Methylpropyl benzene
Methyl-(methylethyl)-benzene
Dimethylethylbenzene
Methyl -(methylethyl)-benzene
Dimethylpropylbenzene
*Tetramethylbenzene
Methylpropenylbenzene
*Tetramethylbenzene
Dimethyl propyl benzene
Naphthalene
2-Methylnaphthalene
1-Methylnaphthalene
l.r-Biphenyl
*Dimethylnaphthalene
*Dimethylnaphthalene
^Dimethylnaphthalene
*Dimethylnaphthalene
Methyl-1,1'-biphenyl
Methyl ethyl naphthalene
*Trimethylnaphthalene
*Trimethylnaphthalene
*7rimethylnaphthalene
*	Trimethy1 naphthalene
*	Trimethylnaphthalene
*	Methyl -(methylethyl)-Naphtha'
*	Methyl -(methylethyl)-Naphthal
Phenanthrene
Methyldibenzothiophene
*	Methylphenanthrene
*	Methylphenanthrene
*	Methylphenanthrene
*	DimethylDhenanthrene
*	DimethylDhenanthrene
*	Dimethylphenanthrene
ene
ene
959
496
990
2,280
1017
2,170
1048
1,420
1056
1,570
1063
1,220
1074
5,170
1082
3,600
1101
4,030
1110
1,510
1112
2,840
1139
5,480
1143
1,710
1158
1,920
1173
5,290
1285
34,700
1301
18,100
1372
6,120
1396
35,600
1411
15,200
1429
7,580
1444
8,500
1479
17,800
1496
14,600
1518
9,710
1522
16,700
1538
3,910
1555
28,700
1571
7,870
1641
5,760
1662
7,840
1766
6,350
1840
4,700
1883
6,130
1888
4,900
1907
4,320
2003
2,570
2022
8,160
2028
1,180
*Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
Concentrations expressed per unit volume of wet sample.
113

-------
i
FIGURt VII B. CAPILLARY COLUMN GAS CHROMATQGRAMS OF TIC ALIPHATIC (A) AND AROMATIC (B)
FRACTIONS OF WHOLE DRILLING FLUID P-l.

-------
VII C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mi 1 gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-i
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
0 j
0.462
P-5
! 1.55
2.19
3.74
P-6
0.039
0 :
1
0.039
P-7
0.063
0 j
0.063
P-8
0.690
0.68
1.37
115

-------
VII c. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (|ig/l)
Sample #
N-C9
NC
10
NC
11
nc,2
NC 13
NC
14
NClb
NC|6
NC
17
MIBLKA51 Al-7

0.12
0.29
0.46
0.88
0.73
0.34
0.20
0.25
AN31-1-6

2.37
7.0
10.7
15.4
18.3
21.7
23.41
23.39
MiIgel
0.09
0.25
0.43
0.51
0.69
0.84
0.84
0.91
0.90
SV76-2-5

7.58
27.2
52.6
86.7
110
129
119
113
P-l
12.0
72.6
198
274
362
391
448
489
481
P-2
2.7
7.6
14
22
33
42
50
54
51
P-3
_
15
65
124
194
239
289
279
280
P-4
0.96
3.8
8.3
11
19
26
36
46
51
~>-5
ct>

7.0
15
30
62
93
113
132
127
P-6
0.20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.5/
P-7

0.3/
0.68
0.97
1.6
2.3
3.2
4.2
4.4
P-8
2.7
8.4
20
28
37
43
46
47
41

-------
VII C. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample #
Pristane
NC|8
Phytane
nc19
nc20
NC21
nc22
MIBLKA51 A1-7

0.11

0.15

0.14
0.50
AN31-1-6
14.8
17.9
9.0
15.1
9.6
6.8
4.6
Hilyel
0.45
0.70
0.29
0.58
0.39
0.28
0.21
SV76-2-5
54.8
85.6
30.1
66.6
43.4
33.0
20.6
P-l
142
368
119
302
203
143
78
P-2
30
41
lb
33
24
17
11
P-3
135
229
92
196
171
119
84
P-4
17
36
11
24
13
7.5
4.3
Lll
43
101
39
79
54
37
22
P-6
0.32
0.52
0.17
0.61
0.50
0.56
0.76
P-7
2.0
3.3
1.2
2.5
1.6
1.1
0.83
P-8
23
32
10
25
18
13
8.2

-------
VII C. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample 0
nc23
nc24
NC25
^26
nc27
* 28
nc29
nc30
NCj,
NC32
M1BLKA5I Al-7
1.2
2.0
2.9







AN31-1-6
3.5
3.6
3.9
4.3
6.0
	
	

	
	
Mi Igel
.
.
0.32
	
	
	
	
—
	

SV76-2-5
11.9
7.6
5.2
4.3
5.1
3.0
3.2
2.5
	

P-l
3b
17
7







P-2
6.8
5.3
4.4
42
4.8
3.0
3.2
3.1


P-3
!>4
44
28
26

__
_


	

3.3
3.5
3.9
4.3
5.8
3.8
3.4
2.7


00 P-5
12
6.3




__


	
P-6
1.30
1.9
2.4
1.9
4.2
2.8
2.6
2.1
1.9

P-7
0.86
1.1




_
... ...
	
. . .
P-8
5.3
4.1
4.2
	
	
—

—
	


-------
83 - 2000 F1
F1 (Aliphatic) Fraction
FIGURE VII C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-l.

-------
VII C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (rag/1)
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
.088
0
cr>
CO
o
Mi 1 gel
.15
0
,147
SV76-2-5
.48
.433
.912
P-l
2.5
3.060
5.53
P-2
.29
.134
.426
P-3
1.36
1.50
2.86
P-4
.28
0.17
'
.442
P-5
. 5:
1.83
1.37
P-6
.038
0
.038
P-7
. 030
0
.030
0-8
1. 1C
1
0.61
1.71
12C

-------
VII C. P-l SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (yg/l)
Methyl ethyl benzene
959
10.9
*Trimethyl benzene
992
23.6
~Methylpropyl benzene
1050
4.8
Dlmethylethylbenzene
1058
11.1
~Methyl propyl benzene
1065
7.9
Metby1-(methyethyI)-benzene
1076
2.4
fcmethyl ethyl benzene
1083
23.1
Methyl-(methyethyl)-ben«na
1100
7.9
~Tetramethylbenzene
1114
11.0
~Tetramethylbenzene
1144
3.1
Oimethylpropylbenzene
1158
28.0
Naphthalene
1174
4.4
2-Methylnaphthalene
1291
25.3
1-Methylnaphthalene
1300
29.4
1,1'-biphenyl
1372
8.5
~Dimethylnaphthalene
1410
7.6
*Dimethylnaphthal ene
Methyl-1,1'-biphenyl
1445
2.1
1481
3.7
Methyl ethylnaphthalene
1494
26.8
*Tri methyl naphtha 1 ene
1519
29.5
~Trimethylnaphthal ene
1524
32.0
~Trimethvlnaphthalene
1554
6.4
*Trimethy1 naphtha 1ene
1570
6.6
~Methyl-(methyl ethyl) -naphthalene
1664
1.8
Methyldibenzothi ophene
1839
12.8
~Methylphenanthene
1883
2.4
121

-------
VII c. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
Resolved (ug/1)
Unresolved (ug/1)
Total (ug/1)
MIBLKA51 Al-7
25.0
0
25.0
AN 31-1-6
497
0
497
Mi 1 gel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
0
165
P-6
13.6
0
13.6
P-7
478
0
478
P-8
836
0
336
122

-------
83 - 2000 F3
F3 (Polar) Fraction
FIGURE VII C CAPILLARY COLUMN GAS CHRGMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-l.

-------
83 - 2000 1-2
F2 (Aromatic) Fraction
FIGURE VII C. CAPILLARY COl UMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-l.

-------
,,,	o.	^	,.olssOLm	fHAs£„	BiMssA(

-------
VII D.. DISSOLVED BIOASSAY PHASE - TUTaL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Components
(mg/1)
MIBLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
'6.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
P-5
.166
1.16
P-6
.043
0
P-7
.175
0
P-8
.161
2.42
•"Concentrations expressed per unit volume of wet sample.
Dissolved Bioassay Phase sample were not fractionated into
aliphatic (Fl), aromatic (F2) or polar (F3) fractions due
to tne chromotograpnic simplicity of the samples.
126

-------
VII D (cont.). P-I DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Name
K0VA7 No
Concentration ;uc/! -a
C7-Alcohol
Ethylhexanol
Benzoic Acid
Methoxybenzaldehyde
Ci 3-Ketone
Molecular Ion m/e = 170
Methoxybenzoic Acid
Molecular Ion m/e = 199
Hexadecanoic Acid
Cjg-Alcohol
Cjg-Carboxylic Acid
Cjg-Carboxylic Acid
C2Q-Carboxylic Acid
911
1034
1219
1415
1500
1559
1590
1682
1977
2071
2162
2305
2447
25.6
43.6
97.2
14.1
167.
148.
99.0
287.
12.2
35.6
6.9
7.1
52.0
Concentrations expressea per unit volume of wet sample.
127

-------
VIII. MUD IDENTIFICATION: P2-1-3
LAB NUMBER :	83-2001
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	Dlssoved Bloassay Phase Organic Concentrations

-------
VIII A. DRILLING HUD ELEMENTAL CONCENTRATIONS
P2-1-3 (Sample I.D.: 83-2001)
Element
Whole Muda
Particulate Phase
Bioassay Preparation"
Dissolved Phase
Bioassay Preparation
A1
0.76(55)
793.
0.009
8a
37.2(»)
8.05
'
3.32
Cd
11.8
2.38
0.007
Ca
0.65(S)
	
	
Cr
483.
237.
0.896
Cu
39.7
11.8
0.019
Fe
0.70(2)
1784.
1.27
Pb
291.
40.6
0.046
Sr
226.
	
	
Zn
2064.
338.
0.007
h2o
58.b:sO
t

Concentrations expressed as ug/g dry weight unless otherwise indicated.
{
bConcentrations expressed as ug/g wet weight unless otherwise indicated.
129

-------
VIII B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic Fraction

Aromatic Fraction
Sample *
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
'JCM (mg/1)
MIBLKA51 Ai-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mil gel
.004
0

o
o
0
SV76-2-5
464.
966.

166.
330.
5-l
2,700.
4,200.

636.
964.
P-2
252.
o
o
CO

47.6
228.
F-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
646.

207.
183.
P-6
10.1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
P-8
204.
270.

86.9
164.
*A11 concentrations expressed per unit volume of wet sample.
130

-------
VIII B. (conl.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (wg/1)*
Sample #
N-Cg
N-C,0
N-Cn
n-c12
N-Cn
N-Cj4
N~C15
«-C16
N~C 17
Pristane
n-c18
Phytane
N-C19
MIBLKA51 Al-7

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-I-6
182
2600
3300
6440
8310
9/90
l3,bU0
14,000
10,800
7110
8780
4250
7880
Milgel
55
5400
137
91
182
182
128
73
72
3b
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151.000
201,000
197,000
94,000
42,900
148.000
43.400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
a.
131
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26.400
62,700
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
•All concentrations expressed per unit volume of wet sample.

-------
VIII B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/O*
Sample
n-c20
1
j
1 1
o
ro 1
n-c22
n-c23
N"C24
n-c25
MC26
n-c27
N-C2a
n-c29
N_C30
N"C31
MIBLKA51 A1- 7
940
780
478
289
144
111
-
-
-
-
-
-

AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-
"

Milgel
SV76-2-5
55
13,800
55
11,300
55
8040
5330
3460
56
2280
1440
1740
725
1160
429
1530

P-l
P-2
96,400
8000
65,700
6380
41,300
4730
23,300
3320
10,700
2050
5090
1810
1040
949
398
795
719


O. Q-
132
53,700
4280
44,600
2520
34,800
1580
23,300
1060
14,500
728
8860
615
6540
458
w
716
461
655



i i
c> tn
11,400
393
7900
353
5440
327
3270
322
1480
268
283
234
315
141
207
118
144

P-7
1550
1120
744
434
234
-
-
-
-
-
-
-

P-8
4260
3060
I860
1040
518
299
-
-
-
-
-
-

*A11 concentrations expressed per unit volume of wet sample.

-------
VIII B(cont). P-2 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
Methyl ethyl benzene
*Trimethylbenzene
~Trimethylbenzene
~Methylpropyl benzene
Dimethyl ethyl benzene
*Methylpropyl benzene
Methyl-(methyl ethyl)-benzene
Dimethylethylbenzene
Methyl-(methylethyl)-benzene
Dimethyl propyl benzene
~Tetramethylbenzene
Methylpropenylben zene
~Tetramethylbenzene
D i met hy1propy1 ben zene
Naphthalene
2-Methy1 naphthalene
1-Methylnaphthalene
1,1'-Biphenyl
~Dimethylnaphthalene
~Dimethylnaphthal ene
~Dimethylnaphthalene
~Dimethylnaphthal ene
Methyl-1,1'-biphenyl
Methylethylnaphthalene
~Trimethylnaphthal ene
~Trimethylnaphthal ene
*Trimethylnaphthalene
*Trimethylnaphthalene
*Trimethylnaphthalene
*	Methyl-(methylethyl)-Naphtha 1ene
*	Methyl -(methyl ethyl)-Naphthalene
Phenanthrene
Methyldibenzothiophene
*	Methylphenanthrene
*	Methylphenanthrene
*	Methylphenanthrene
*	Dimethylphenanthrene
*	DimethylDhenanthrene
*	DimethylDhenanthrene
KOVAT No.
Concentration (ug/l)3
959
989
1017
1047
1055
1062
1074
1081
1100
1110
1115
1142
1146
1161
1175
1286
1302
1373
1397
1413
1431
1446
1480
1497
1520
1524
1540
1557
1573
1643
1664
1768
1841
1884
1889
1908
2005
2024
2030
122.
269.
231.
149.
118.
80.1
295.
247.
126.
101.
148.
334.
136.
216.
528.
2370.
1670.
232.
2920.
641.
615.
759.
1200.
1010.
637.
1200.
86.5
3090-
389-
434-
574-
600-
232.
397.
206.
262.
132.
295.
46.8
~Structural isomer(s) of the comDOund indicated. Exact identification of individual isomer
not oossible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
a
Concentrations expressed per unit volume of wet sample.
133

-------
FIGURE VIII B. CAPILLARY COLUMN GAS CHKOMATOGRAMS OF THE ALIPHATIC (A) AND AROMATIC
(B) FRACTIONS OF WHOLE DRILl ING FLUID P-2.

-------
VIIIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mil gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-l
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0
0.039
P-7
0.063
0
0.063
P-8
0.690
0.68
1.37
135

-------
VMIC. DRILLING TLUID
SUSPFNDFD SOI IDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample #
MIBLKAbJ AI-7
AN3I-1-6
Mi l go 1
SV76-2-5
P-l
P-2
P-3
P-4
^P-5
cr>
P-6
P-7
P-8
N-C9
NC
10
NC
11
0.09
12.0
2.7
0.96
0.20
2.7
0.12
2.37
0.25
/. b8
72.6
7.6
15
3.8
7.0
0.21
0.37
8.4
0.29
7.0
0.43
27.2
198
14
65
8.3
15
0.24
0.68
20
NC| 2
0.46
10.7
0.51
52.6
274
22
NC13
NC
14
NC
15
NC|6
NC
17
124
11
30
0.21
0.97
28
0.88
15.4
0.69
86.7
362
33
194
19
62
0.24
1.6
37
0.73
18.3
0.84
110
391
42
239
26
93
0.25
2.3
43
0.34
21.7
0.84
129
448
50
289
36
113
0.28
3.2
46
0.20
23.41
0.91
119
489
54
279
46
132
0.39
4.2
47
0.25
23.39
0.90
113
481
51
280
51
127
0.57
4.4
41

-------
VIIIC. DRILLING FLUID SUSPENDED SOLIDS -
U>
Sample #
MlliLKA51 Al-7
AN31-1-6
Mil ye I
SV/6-2 5
P-l
P-2
P-3
P-4
P-5
P-6
P- 7
P-8
Pristane
14.8
0.45
54.8
142
30
135
17
43
0.32
2.0
23
nc18
0.11
17.9
0.70
85.6
368
41
Phytahe NC
19
229
36
101
0.52
3.3
32
9.0
0.29
30.1
119
15
92
11
39
0.17
1.2
10
0.15
15.1
0.58
66.6
302
33
196
24
79
0.61
2.5
25

ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
nc2o	nc2,	nc22
_	0.14	0.50
9.6	6.8	4.6
0.39	0.28	0.21
43.4	33.0	20.6
203	143	78
24	17	U	
171	119	84
13	7.5	4.3
54	37	22
0.50	0.56	0.76
1.6	1.1	0.83
18	13	8.2

-------
V1IIC. DRILLING FIIJID SUSPENDED SOLIDS
Sample It
MIBLKA'jI Al-7
AN31-1 6
Mi I ye 1
SV/6-2-5
P-1
P-2
P-3
P-4
P-5
P-6
P-7
P 8
NC
23
NC<
24
1.2
3.5
11.9
3b
6.8
54
3.3
12
1.30
0.86
5.3
2.0
3.6
7.6
17
5.3
NC25
2.9
3.9
0.32
5.2
7
4.4
44
3.5
6.3
1.9
1,1
4.1
28
3.9
2.4
4.2
A!1PHATIC FRACTION CONCENTRATIONS (Mg/1)
NCZ6	NC27 NC28 NC29 NC3()
4.3	6.0			__		
4.3	5.1	3.0	3.2	2.5
4.2	4.8 3.0	3.2	3.1
26		
4.3	5.8
1.9	4.2
3.8	3.4	2.7
2.8	2.6	2.1

-------
83 2001 - F1
*
mm ii
F1 (Aliphatic) Fraction
I < <
t ?
c c

FIGURE VIII C. CAPILLARY COLUMN GAS CHR0MAT0GRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-2.

-------
VIIIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7

.072
0
.073
AN 31-1-6

.088
0
.089
Mi 1 gel

.15
0
.147
SV76-2-5

.48
.433
.912
P-l

2.5
3.060
5.53
P-2

.29
.134
.426
P-3

1.36
1.50
2.86
P-4

.28
0.17
.442


K —
1.83
1.37
P-6
i
.
.038
0
.038
P-7

.030
0
.030
P-8
,
i
i ...
1.1C
.
0.61
1.71
140

-------
VIII C. P-2 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
Dimethylethylbenzene
1055
0.81
Methyl-(methyl ethyl-benzene
1100
0.89
*Tetramethylbenzene
1114
1.8
Methylpropenylbenzene
1142
0.33
~Tetramethylbenzene
1146
1.87
Naphthalene
1175
0.72
2-Methylnaphthalene
1291
33.8
1-Methylnaphthalene
1300
2.5
l,l'-Biphenyl
1377
3.4
~Dimethyl naphthalene
1444
0.37
Methyl-l,l'-biphenyl
1480
0.34
Methyl ethyl naphtha1ene
1500
0.61
~Trimethylnaphthalene
1519
1.43
*Trimethyl naphthalene
1524
2.8
*Methylphenanthene
1891
0.73
~Dimethylphenanthene
2032
0.31
141

-------
83 - 2002 F2
F2 (Aromatic) Fraction
riGURE VIII C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-2.

-------
VIlie. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
Resolved (ug/1)
Unresolved (ug/1)
Total (ug/1)
MIBLKA51 Al-7
25.C
0
25.C
AN 31-1-6
497
0
497
Mil gel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
0
165
P-6
13.6
0
13.6
P-7
CO
0
478
P-3
836
0
836
143

-------
83 - 2001 F3
M

t » ax
V'.
Jill
F3 (Polar) Fraction
FIGURE VIII C. CAPILLARY COLUMN GAS CHROMAT0GRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-2.

-------
VIIID. DISSOLVED BIOASSAY PHASE - TUTAL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Sample *
Total Resolved Components
(mg/1)
Total Unresolved Components
(mq/1)
MIBLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
6.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
p-5
.166
1.16
P-6
.043
0
P-7
.175
0
P-8
.161
2.42
*Concentrations expressed per unit volume of wet sample.
Dissolved Bioassay Phase sample were net fractionated into
aliphatic (Fl), aromatic (f'F2; or polar (F3) fractions cue
to the chromotograpnic simplicity of the samples.
145

-------
VIII D (cont.). P-2 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Name
K0VA7 No
Concentration (-jg/i;a
Cy-Alcohol
C0-Alcoho1
Ethylhexanol
Benzoic Acid
Met hoxy ben za1de hyde
Molecular Ion m/e = 170
Methoxybenzoic Acid
Molecular Ion m/e = 199
Hexadecanoic Acid
Ci0-Alcohol
Cj3-Carboxylic Acid
CjQ-Carboxylic Acid
909
1022
1034
1218
1423
1566
1600
1687
1977
2070
2162
2440
<0.1
0.1
<0.1
<0.1
.8
1.0
.2
.5
<0.1
<0.1
<0.1
<0.1
j
I
Concentrations expressed per unit volume of wet sample.
146

-------

FIGURE VIII D. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "DISSOLVED "PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-2.

-------
IX. MUD IDENTIFICATION: P3-1-3
LAB NUMBER:	33-2002
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
0. Oi solved Bloassay Phase Organic Concentrations
143

-------
IX A. DRILLING MUD ELEMENTAL CONCENTRATIONS
P3-1-3 (Sample I.D.: 83-2002)
Element
Whole Muda
Particulate Phase ,
Bioassay Preparation"
Di ssolved Phase
Bioassay Preoarationt
A1
1.30(2)
661.
0.132
Ba
35-1(%)
22.9
0.813
Cd
2.10
0.053
0.002
Ca
0.74(»)
	
	
Cr
459.
138.
2.60
Cu
90.4
11.1
0.243
Fe
5.67(%)
1810.
1.84
Pb
100.
10.2
0.104
Sr
383.
	
	
Zn
439.
41.8
0.140
h20
57.8 ('•)
	

Concentrations expressed as ug/g dry weight unless otherwise indicated.
^Concentrations expressed as ug/g wet weight unless otherwise indicated.
149

-------
IX B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic
Fraction

Aromatic Fraction
Sample #
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
UCM (mg/1)
MIBLKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mi 1 gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
?-l
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
?-5
284.
646.

207.
183.
P-6
10.1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
P-8
204.
270.

86.9
164.
*A11 concentrations expressed per unit volume of wet sample.
150

-------
IX B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)*
Sample f
N-Cg
N-Ciq
N-Cn
n-c12
N-Ci3
N-C14
N"C15
•"ifi
N-C17
Pristane
N-Cjg
Ptiytane
N-Cjg
MIDLKA51 Al-7
.
3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-1-6
182
2600
3300
6440
8310
9790
1J.bOO
14,000
10,BOO
7110
8780
4250
7880
MiIgel
55
5400
13/
91
182
182
128
73
72
36
56
36
J u
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36.500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101.000
112,000
141,000
151,000
201,000
197,000
94,000
42,900
148,000
43,400
121,000
P-2
3B5
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96 , 300
92,400
39,500
76,500
26,400
62,700
£ P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
IX D. (tout.) WHOLE DRILLING FIUID - ALIPHATIC FRACTION CONCENTRATIONS
(ng/n*
Sample i
N-c20
n-c21
n-c?2
nc23
n-c24
n-c25
n-c26
n-c27
n-c28
n-c29
N-C3Q
NC31
MIBLKA51 A1- 7
940
780
478
289
144
in
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-
"
Hi Igel
SV76-2-5
55
13,800
55
11,300
55
8040
5330
3460
56
2280
1440
1740
725
1160
429
1530
P-l
£ P-2
% ,400
8000
65,700
6380
41,300
4730
23,300
3320
10,700
2050
5090
1810
1040
949
398
795
719

P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
P-6
11,400
393
7900
353
5440
327
3270
322
1480
268
283
234
315
141
207
118
144
P-7
1550
112Q
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
-
-
-
-
*A11 concentrations expressed per unit volume of wet s
amp1e.

-------
IX B. (cont.) P-3 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT No.
Concentration (ug/1)a
Trimethylbenzene
990
443
Methyl propyl benzene
1048
226
Dimettylethylbenzene
1055
316
~Methyl-(methylethyl )-benzene
1074
708
Dimethylethylbenzene
1081
540
~Methyl -(methylethyl)-benzene
1101
910
Dimethyl propyl benzene
1111
313
~Tetramettylbenzene
1115
427
Methylpropenylbenzene
1142
1,170
~Tetramethylbenzene
1146
263
Dimethyl propyl benzene
1161
- 454
Naphthalene
1174
1,360
2-Methylnaphthalene
1285
12,600
1-Methylnaphthalene
1,1'-Biphenyl
1X1
7,550
1371
1,260
~Dimethylnaphthalene
1396
15,300
~Dimethylnaphthalene
1411
6,550
~Dimethyl naphthalene
1429
2,930
~Dimethyl naphthalene
1444
3,760
Methyl-1,1'-bi phenyl
1479
5,270
Methyl ethyl naphthalene
1495
5,780
~Trimethylnaphthalene
1517
3,730
~Trimethylnaphthalene
1522
6,130
~Trimethylnaphthalene
1538
857
~Trimethylnaphthalene
1554
11,100
~Trimethylnaphthalene
1571
2,570
~Methyl -(methyl ethyl)-Naphtha!ene
1641
4,390
~Methyl -(methyl ethyl)-Naohthalene
1662
2,460
Phenanthrene
1766
4,170
Methyldibenzothiophene
1841
2,160
~Methylphenanthrene
1883
3,490
~Methylphenanthrene
1887
2,690
~Methylphenanthrene
1906
1,990
~OimethylDhenanthrene
2003
3,310
~Dimethylphenanthrene
2021
3,400
~Dimethylphenanthrene
2028
814
^Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
a
Concentrations expressed per unit volume of wet sample.
153

-------
I
FIGURE IX B. CAPILLARY COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND
AROMATIC (B) FRACTIONS OF WHOLE DRILLING FLUID P-3.

-------
IXC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-5
0.325
0
0.325
Mi 1 gel
0.016
0
i 0.016
SV76-2-5
1.56
1.96
I
3.52
P-l
6.43
7.78
14.2
?-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0
0.039
P-7
0.063
0
0.063
P-8
0.690
0.68
;
1.37
155

-------
IX
C. DRILLING TLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (ug/1)
Sample tt
MIBLKA51 Al-7
AN31-1-6
Mi l ye1
SV76-2-5
P-l
P-2
P-3
N-Cg
NC
10
NC
11
nc12
NC 13
NC
14
NC
15
NCJ6
NC
17
0.09
12.0
2.7
0.12
2.37
0.25
/. 58
72.6
7.6
15
0.29
7.0
0.43
27.2
198
14
65
0.46
10.7
0.51
52.6
274
22
124
0.88
15.4
0.69
86.7
362
33
194
0.73
18.3
0.84
110
391
42
239
0.34
21.7
0.84
129
448
50
289
0.20
23.41
0.91
119
489
54
279
0.25
23.39
0.90
113
481
51
280
P-4
£ P-5

P-6
P-7
P-8
0.96
0.20
2.7
3.8
7.0
0.21
0.37
8.4
8.3
15
0.24
0.68
20
11
30
0.21
0.97
28
19
62
0.24
1.6
37
26
93
0.25
2.3
43
36
113
0.28
3.2
46
46
132
0.39
4.2
47
51
127
0.57
4.4
41

-------
Sample #
M1BLKA51 Al-/
AN31-1-6
Hi lye1
SV76-2-5
P-l
P-2
P-3
^ P-4
(_n
^ P-5
P-6
P-/
P-8
IXC. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Pristane NCjq Phytane NCjg	NC^q NC21	NC22
	
0.11
	
0.15

0.14
0.50
14.8
17.9
9.0
15.1
9.6
6.8
4.6
0.45
0.70
0.29
0.58
0.39
0.28
0.21
54.8
85.6
30.1
66.6
43.4
33.0
20.6
142
368
119
302
203
143
78
30
41
15
33
24
17
11
135
229
92
196
171
119
84
17
36
11
24
13
PN.
4.3
43
101
39
79
54
37
22
0.32
0.52
0.17
0.61
0.50
0.56
0.76
2.0
3.3
1.2
2.5
1.6
1.1
0.83
23
32
10
25
18
13
8.2

-------
DRUIING Fl IJID SUSPENDED SOLIDS
Sample #
MIBLKA51 A1-7
AN31-1-6
SV76-2-5
P-l
P-2
P-3
HCll
1.2
3.5
11.9
36
6.8
54
Nt
24
2.0
3.6
7.6
17
5.3
44
NC25
2.9
3.9
0.32
5.2
1
4.4
28
P-4
£ P-5
P-6
P-7
P-8
3.3
12
1.30
0.86
5.3
3.5
6.3
1.9
l.l
4.1
3.9
2.4
4.2
ALIPHATIC FRACTION CONCENTRATIONS („9/l)
NCZfi	Nf.27	NC28	^NC29	NC3(|	N C^ NC32
4.3	6.0 	 							
4.3	5.1	3.0	3.2	2.5		
4.2	4.8	3.0	3.2	3.1				
26		 					
4.3	5.8	3.8	3.4	2.7				
1.9	4.2	2.8	2.6	2.1	1.9

-------
nt -	11
t ! S ! t t
F1 (Aliphatic) Fraction
U"»

-------
IX c. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample *
Resolved (mg/1)
Unresolved (ng/1)
Total (mg/1)
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
.088
0
.089
Mi 1 gel
. 15
0
..147
SV76-2-5
.48
.^33
.912
P-l
2.5
3.060
5.53
P-2
90
• w ^
.134
.426
P-3
1.36
1.50
2.86
P-4
.28
0.17
.442
P-5
cs
~ v w
1*83
1.37
P-6
. 038
0
.038
P-7
. 03 C
0
.030
P-8
! i.io
i
C .61
1.71
160

-------
IX C. P-3 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
Dimethyl ethyl benzene
1083
4.1
*Methy1-(methyl ethyl)-benzene
1101
1.6
*Tetramethylbenzene
1115
3.7
*Tetramethylbenzene
1146
4.5
Napthalene
1174
1.3
2-Methylhaphthalene
1291
171
1-Methylnaphthalene
1300
8.9
1,1'-Bi phenyl
1371
2.0
~Dimthylnaphthalene
1393
3.4
~Dimethyl naphthalene
1410
2.1
Methyl-1,1-biphenyl
1481
3.1
Methyl ethyl naphthalene
1494
12.0
~Trimethylnaphthalene
1519
8.2
*Trimethylnaphthalene
1524
18.2
*Trimethylnaphthalene
1538
4.8
~Trimethylnaphthalene
1554
1.9
~Trimethylnaphthalene
1570
1.6
Methldi benzothi ophene
1838
4.9
161

-------
IX C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
.
Resolved (ug/1)
Unresolved(ug/1)
Total (ug/1)
MIBLKA51 A1-7
25.0
0
25.0
AN 31-1-6
497
0
497
Mil gel
118 •
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
c
165
P-6
13.6
0
13.6
P-7
478
0
478
P-8
836
0
836
162

-------
83 - 2002 F2
F2 (Aromatic) Fraction
FIGURE IXC. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY
PREPARATION OF SPENT DRILLING FLUID P-3.

-------
83 - 2002 F3
F3 (Polar) Fraction
FIGURE IX C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-3.

-------
IX D. DISSOLVED BIOASSAY PHASE - TUTaL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Components
(mg/1)
MIBLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
-6.63
= -1
.358
.603
P-2
in
O
0
.008
P-3
1.09
6.49
P-4
.002
.011
P-5
.166
1.16
P-6
.043
0
P-7
.175
0
P-8

2.42
•Concentrations expressed per unit volume of wet sample.
Dissolved Bioassay Phase sample were not fractionated into
alipnatic (F1), aromatic (F2) or polar (F3) fractions due
to the chromotographic simplicity of the samples.
I65

-------
IX D (cont.) P-3 DRILLING FLUID -
DISSOLVED BIOASSAY PHASE COMPONENTS
Comoound Name
K0VA7 No
Concentrator ?ua/"!a
C7-Alcohol
Cg-Alcohol
Benzoic Acid
Methoxybenzaldehyde
Ci3-Ketone
Molecular Ion m/e = 170
Methoxybenzoic Acid
Molecular Ion m/e = 199
C^g-Carboxylic Acid
909
1020
1226
1410
1488
1553
1590
1676
2162
2.3
31.3
48.5
68.5
3.0
4.7
15.8
11.5
7.8
Concentrations expressed per unit volume of wet sample.
166

-------
FIGURE IX D. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "DISSOLVED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-3.

-------
X. MUD IDENTIFICATION: P4-1.3
LAB NUMBER:	83-2003
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	Dissolved Bloassay Phase Organic Concentrations
I6S

-------
X A. DRILLING MUD ELEMENTAL CONCENTRATIONS
P4-1-3 (Sample I.D.: 83-2003)
Element
Whole Muda
Particulate Phase
Bioassay Preparation®
Dissolved Phase
Bioassay Preparation13
A1
1.56(«)
1083.
2.41
6a
48,7(%)
11.7
10.7
Cd
8.27
3.06
0.004
Ca
0.18(%)
	
	
Cr
532.
197.
41.8
Cu
32.7
12.3
0.059
Fe
1.15(2)
2896.
32.4
Pb
221.
28.2
1.56
Sr
207,
	
_
Zn
1384.
476.
^ 0.804
h2o
60.2 {%)


Concentrations expressed as ug/g dry weight unless otherwise indicated
Concentrations expressed as ug/g wet weight unless otherwise indicated
169

-------
X B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

AT iphatic
Fraction

Aromatic Fraction
Sample #
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/I)
L'CM (mg/1 )
VIBLKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mil gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
P-l
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
?-3
1,260.
5.970.

230.
445.
P-4
132.
548.

106.
103.
3-5
284.
646.

207.
183.
?-6
10.1
12.3

6.5
4.5
°-7
32.2
69.1

14.4
25.6
?-8
204.
270.

86.9
164.
*Ail concentrations expressed per unit volume of wet sample.
170

-------
X B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (wg/1)*
Sample #
n-c9
N-C10
N-Cn
N-Ci2
NC13
n-c14
NC15
N-C!6
N-C17
Pristane
N-Cib
Phytane
N-C,9
M1ULKA51 A17

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN 31-1-6
182
2600
3300
6440
8310
9790
1 J,600
14,000
10,800
7110
8780
4250
7880
Mi lgel
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101.000
112,000
141,000
151,000
201,000
197,000
94,000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
^ P- 3
-»-j • j
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
•—»
P 4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24.700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-/
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
XB. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (m9/D*
Sample 8
N C2(J
h-c21
h-c22
M"C23
N-c24
n-c25
nc26
n-c27
n-c28
N-C29
N-C30
N'C31
MIBLKAbl AI /
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
52/0
3900
2510
1570
836
521
245
285
-
-
-

Ml 1 gel
55
55
55
-
-
56
-
-
-
-
-
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
P-3
b3,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
-
P-6
393
353
327
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
I860
1040
518
299
-
-
-
~

;	
*A11 concentrations expressed per unit volume of wet sample.

-------
X B(cont). P-4 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
i
KOVAT No. j
Concentration
Me t hy 1 e t hy 1 ben zene
959 j
94.7
Trimethylbenzene
990 1
126.
*Methylpropyl benzene 1
1048
102.
Dimethylethylbenzene
1055
52.2
•Methyl propyl benzene
1063
56.6
•Methyl-(methylethyl)-benzene
1074 !
168.
Dimethylethylbenzene
1081
118.
~Methyl-(methylethyl)-benzene
1101
190.
Tetramethylbenzene
1115
49.0
Methylorooenylbenzene
1143
267.
Dimethylpropylbenzene
1161
168.
Naphthalene
1175
196.
2-Methylnaphthalene
1285
1420.
1-Methyl naphthalene
l»l'-Biphenyl
1X1
820.
1372
355.
•Dimethylnaphthalene
1395
1880.
•Dimethylnaphthalene
1413
97.7
~Dimethyl naphthalene
1429
422.
*01 methylnaphthal ene
1445
436.
Methyl-1,1'-biphenyl
1479
766.
Methyl ethylnaphthal ene
1496
756.
~Trimethy1naphthalene
1518
477.
~Trimethylnaphthalene
1523
764.
~Trimethylnaphthalene
1539
1980.
~Trimethylnaphthalene
1555
1800.
~Trimethylnaphthalene
1572
466.
•Methylethylnaphthalene
1642
681.
~Methyl ethylnaphthal ene
1663
434.
Phenanthrene
1767
556.
Methyldibenzothiophene
1841
378.
~Methylphenanthrene
1883
436.
~Methylphenanthrene
1888
255.
~MethylPhenanthrene
1907
253.
~Dimethylphenanthrene
2004
341.
~Dimethylphenanthrene
2022
382.
!
!
i
•Structural i-somer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized *or
comparison and evaluation of isomers among samples.
a
Concentrations expressed per unit volume of wet sample.
173

-------
FIGURE X B. CAPILLARY COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND AROMATIC (B)
FRACTIONS OF WHOLE DRILLING FLUID P-4.

-------
X C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample «
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
C.046
0
0.046
AN31-1-6
0.325
0
0.325
M;Igel
0.016
0
0.016
SV76-2-5
1.56
1.96
3-. 52
2-1
6.43
7.78 i
14.2
P-2
0.694
0 1
0.694
P-3
4.35
11.45 !
15.8
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
j 0.039
i
0.039
P-7
! 0.063
0
0.063
P-8
0.690
0.68
1 .37
175

-------
XC. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (uy/1)
Sample #
MIBLKA5I A1 -/
ANJ1-1-6
Mi lye)
SV76-2-5
P-l
P-2
.^P-3
~P-4
P-5
P-6
P-7
P 8
N-C9
NC
10
NC
11
0.09
12,0
2.7
0.96
0.12
2.37
0.25
7.58
72.6
7.6
15
3.8
0.29
7.0
0.43
27.2
198
14
65
8.3
0.20
2.7
7.0
0.21
0.37
8.4
15
0.24
0.68
20
NC12
0.46
10.7
0.51
52.6
274
22
124
11
NC 13
NC
14
NC
15
NCie
NC
17
30
0.21
0.97
28
0.88
15.4
0.69
86.7
362
33
194
19
62
0.24
1.6
37
0.73
18.3
0.84
110
391
239
26
93
0.25
2.3
43
0.34
21.7
0.84
129
448
50
289
J6
113
0.28
3.2
46
0.20
23.41
0.91
119
489
54
279
46
132
0.39
4.2
47
0.25
23.39
0.90
113
481
51
280
51
127
0.57
4.4
41

-------
X c. DRILLING FLUID
SUSPENDED
SOLIDS -
Sample I
Pristane
NC,b
Phytane NC
19
M1RLKA51 Ai-/
AN31-1-6
Mihjel
SV;6-2-S
P-l
P-2
P-3
P-4
P-S
P-6
P -7
P-8
14,8
0.45
54.8
142
30
135
17
43
0.32
2.0
23
0.11
17.9
0.70
B5.6
368
41
229
36
101
0.52
3.3
32
9.0
0.29
30.1
119
15
92
n
39
0.17
1.2
10
0.15
15.1
0.58
66.6
302
33
196
24
79
0.61
2.5
25
ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
nc20 nc21 nc22
	
0.14
0.50
9.6
6.8
4.6
0.39
0.28
0.21
43.4
33.0
20.6
203
143
78
24
17
11
171
119
84
13
7.5
4.3
54
37
22
0.50
0.56
0.76
1.6
1.1
0.83
18
13
8.2

-------
DRILLING HUM SUSPlNDfcD SOLIDS
Sample 0
nc23
NC?4
NC25
MIBUA5I A1 - 7
1.2
2.0
2.9
AN31-1-6
3.5
3.6
3.9
MiIgel
	
		
0.32
SV/6-2-5
11.9
7.6
5.2
P-l
36
17
7
P-2
6.8
5.3
4.4
H—»



^ P- \
00 r J
54
44
28
P-4
3.3
3.5
3.9
P-5
12
6.3

P-6
1.30
1.9
2.4
P-7
0.86
1.1

P-8
5.3
4.1
4.2




ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
nc26 nc2, nc?8 nc29 nc3o nc31 . NC32
4.3	6.0				
4.3	5.1	3.0	3.2	2.5
4.2	4.8	3.0	3.2	3.1		
26								
4.3	5.8	3.8	3.4	2.7
1.9	4.2	2.8	2.6	2.1	1.9

-------
83 - ?003 F1
H&niU'i
F1 (Aliphatic) Fraction
R -
s# «i * i i i
3 8 t B * ? ®
Lui_i.iLLI I"
f P
|L
FIGURE X C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING TLUID P-4.

-------
X C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
00
oo
o
0
.089
Mi 1 gel
.15
0
.147
SV76-2-5
.48
.<33
.912
P-l
2.5
3.060
5.53
P-2
.29
.134
.426
P-3
1.36
1.50
2.86
P-4
.28
0.17
.442
P-5
E ^
1.83
1.37
P-6
CO
o
o
.038
P-7
.030
0
.030
P-8
1.1C
0.61
1.71
180

-------
X C. P-4 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
Trimethylbenzene
993
0.60
Dimethyl ethyl benzene
1055
0.25
Tetramethylbenzene
1115
0.41
Methylpropenylbenzene
1143
0.15
Naphthalene
1175
0.19
2-Methylnaphthalene
1284
0.25
1-Methylnaphthalene
1206
7.9-
1,1'Biphenyl
1371
0.38
~Dimethyl naphthalene
1393
0.38
~Dimethylnaphthalene
1416
7.7
Methyl-1,1'-biphenyl
1480
0.17
Methyl ethylnaphthalene
1494
1.8
~Trimethylnaphthalene
1519
0.9
~Trimethylnaphthalene
1524
2.9
~Trimethylnaphthalene
1553
0.36
~Trimethylnaphthalene
1570
0.27
~Methyl ethyl naphtha 1ene
1640
0.28
~Methylphenanthene
1891
1.3
~DimethylDhenanthene
2004
0.21
181

-------
83 - 2003 r-2
F2 (Aromatic) Fraction
FIGURE X C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-4.

-------
X C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample «
Resolved (ug/1)
Unresolved (ug/1)
Total (ug/1;
MIBLKA51 Al-7
25.0
0
25.C
AN 31-1-6
497
0
497
Mil gel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
0
1120
P-4
147
0
147
P-5
165
0
165
P-6
13.6
0
13.6
P-7
478
3
478
P-3
836
0
836
183

-------
83 2003 F3
F3 (Polar) Fraction
FIGURE. X C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-4.

-------
X D. DISSOLVED BIOASSAY PHASE - TUTaL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Components
(mg/1)
MIBLKA51 Al-7
.358
.813
AN31-1-6
.136
1.24
Mi 1 gel
.0783
0
SV76-2-5
.920
6.63
»-l
.358
.603
3-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011

.166
1.16
P-6
.043
0
7
.175
0
°-8
.161
2.42
•Concentrations expresses oer unit volume of wet sample.
Dissolvea Bioassay Phase sample were not fractionated into
aiiohatic ;F;], aromatic ;J2) or oolar (F3) fractions due
tc tre chroT:otograpnic simplicity of the samdes.
185

-------
X D. (cont) p.4 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Narre
i
KOVAT No.
Concentration v'-_g/1 ! a
Cy-Alcohol '
910
<0.1
Cg-Alcohol
1023
<0.1
Ethylhexanol
1037 i
<0.1
Methoxybenzaldehyde
1415
<0.1
C^- Ketone
1497 ;
<0.1
Molecular Ion m/e s 170
1556
<0.1
Methoxybenzoic Acid
1589
<0.1
Hexadecanoic Acid
1978
<0.1
Cig-Carboxylic Acid .
2161
<0.1
Ceo-Carboxylic Acid
2442
'
1
<0.1
1
d
Concentrations expressed oer unit volume of wet sample.
136

-------
I
n«E ,	OF m "DISSOLVED PHASE" B.OASSAV

-------
MUD IDENTIFICATION: P5-1-3
LAB NUMBER:	83-2004
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	Dissolved Bioassay Phase Organic Concentrations
188

-------
XI A. DRILLING MUD ELEMENTAL CONCENTRATIONS
P5-1-3 (Sample I.D.: 83-2004)
Element
I
Whole Muda
Particulate Phase
Bioassay Preparation"
Dissolved Phase
Bioassay Preparation^
A1
0.71(S)
1
376.
0.354
Ba
37.5 (»)
15.9
1.04
Cd
2.34
0.075
0.003
Ca
0.57(S)
	
	
Cr
187.
34.6
0.513
Cu
126.
10.6
0.373
Fe
7.63(£)
1996.
1.60
Pb
104.
9.07
0.054
Sr
346.
	
	
Zn
175.
27.5
0.007
H2O
57.5 {%)
	

Concentrations expressed as yg/g dry weight unless otherwise indicated
Concentrations expressed as yg/g wet weight unless otherwise indicated
189

-------
XI B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

A1iphatlc
Fraction

Aromatic Fraction
Sample #
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
UCM (mg/'J
MI5LKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Mi 1 gel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
P-I
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
646.

207.
:s3.
P-6
10.1
12.3

6.5
4.5
P-7
32.2
69.1

14.4
25.6
P-8
204.
270. ,
<

86.9
164.
•All concentrations expressed per unit volume of wet sample.
190

-------
XI B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ng/1)
Sample H
N-Cg
N-Cio
N-Cn
N-C,2
N-Cl3
M ~C 14
"C15
N"C16
N-C17
Prtstane
N-C18
Phytane
n-c19
MIRLKAbl Ai - /

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-16
18?
2600
3300
6440
8310
9790
13,oOO
14,000
10,800
7110
8780
4250
7880
Ml Igel
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
35/
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151,000
201,000
197,000
94,000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
£ P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P 5
_
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420
*AM concentrations expressed per unit volume of wet sample.

-------
XI B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (pg/1)*
Sample #
N-C20
N-C21
n-c22
n-c23
n-c24
n-c25
n-c26
h-c27
n-c28
NC29
nc30
NC31
M1BI.KA51 A1 - 7
940
780
478
289
144
in
-
-
-
"
-
-
AN31-1-6
52/0
3900
2510
1570
836
521
245
285
-
"
-
-
Milgel
SV76-2-5
55
13,600
55
11,300
55
8040
5330
3460
56
2280
1440
1740
725
1160
429
1530
P-l
^ P-2
vo
96,400
8000
65,700
6380
41,300
4730
23,300
3320
10,700
2050
5090
1810
1040
949
398
795
719
_
no
P-3
P-4
53,700
4280
44,600
2520
34,800
1580
23,300
1060
14,500
728
8860
615
6540
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
-
P-6
393
353
327
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
••



*A1I concentrations expressed per unit volume of wet sample.

-------
XI B. (cont.) P-5 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT No
Concentration (ug/1)a
Methylethyl benzene
Trimethylbenzene
Methyl propyl benzene
~Methyl-(methyl ethyl)-benzene
Dimethylethylbenzene
~Methyl-(methylethyl)-benzene
MethylDropenylbenzene
Naphthalene
2-Methylnaphthalene
1-Methylnaphthalene
1,11-Biphenyl
~Dimethyl naphthalene
~Dimethyl naphthalene
~Dimethylnaphthalene
~Dimethylnaphthalene
Methyl-1,11-biphenyl
Methyl ethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Methyl -(methylethyl)-Naphthalene
~Methyl -(methylethyl)-Naphthalene
Phenanthrene
Methyldibenzothiophene
~Methylphenanthrene
~Methylphenanthrene
~Methylphenanthrene
~Dimethylphenanthrene
~Dimethylphenanthrene
961
991
1049
1076
1083
1102
1143
1174
1283
1299
1370
1394
1409
1428
1443
1478
1495
1517
1522
1538
1554
1571
1642
1663
1767
1841
1883
1888
1907
2005
2023
634
815
554
867
683
525
1330
1010
8090
4030
1420
8130
4930
1320
2050
4090
3960
2750
4020
7820
6720
2190
2760
1720
2430
1670
2370
1310
1490
2560
2310
~Structural isomer(s) of the comoound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed, KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
Concentrations expressed per unit volume cf wet sample.
193

-------
FIGURE XI B. CAPILLARY COLUMN GAS CHROHATOGRAMS OF THE ALIPHATIC (A) AND
AROMAVlC (B) FRACTIONS OF WHOLE DRILLING FLUID P-5.

-------
XI C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample r
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Milge1
0.316
0
0,016
SV76-2-5
1,56
1.96
3-. 52
P-:
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
n.45
15.B
P-4
0.462
0
0.462
P-5
1.55
2.19 I
3.74
P-6
0.039
0 !
0.039
P-7
0.063
0
0.063
P-8
0.690
0.68 !
1.37
195

-------
XI C. DRIII ING FLUID SUSPENDFD SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample JH
n <; 9
NC1(J
MC„
N£)2
NC13
NC,4
NC,S
NC16
NC i?

HIBI KASI A1 -7

0,12
0.29
0.46
0.88
0.73
0.34
0.20
0.25

AN 31-1-6
	 ,
2.37
7.0
10.7
15.4
18.3
21.7
23.41
23.39

Mi 1 gel
0.09
0.25
0.43
0.51
0.69
0.84
0.84
0.91
0.90

SV/6 2-5
	
1.58
27.2
52.6
86.7
no
129
119
113

P~1
12.0
/2.6
198
274
362
391
448
489
481

P-2
2.7
7,6
14
22
33
42
50
54
51

P~3
	
15
65
124
194
239
289
279
280


0.96
3.8
8.3
11
19
26
36
46
51

P-5

7.0
15
30
62
93
113
132
127

P~6
0.20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.57

P-/
	
0.37
0.68
0.97
1.6
2.3
3.2
4.2
4.4

P-8
2.7
8.4
20
28
37
43
46
47
41


-------
XI C. DRUIING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample H
Pristane
Nf.|8
Phytane
nc19
nc20
NC?1
NC22
MIBLKA51 Al-/

0.11

0.15

0.14
0.50
AN31-1-6
14.8
17.9
9.0
15.1
9.6
6.8
4.6
Mi Igel
0.45
0.70
0.29
0.58
0.39
0.28
0.21
SV/6 2-5
54.8
85.6
30.1
66.6
43.4
33.0
20.6
P-l
142
368
119
302
203
143
78
P-2
30
41
15
33
24
17
11
m
Q.
197
135
229
92
196
171
119
84
P-4
17
36
11
24
13
7.5
4.3
P-5
43
101
39
79
54
37
22
P-6
0.32
0.52
0.17
0.61
0.50
0.56
0.76
P-7
2.0
3.3
1.2
2.5
1.6
1.1
0.83
P-B
23
32
10
25
18
13
8.2

-------
DRIll ING FLUID SUSPLNDCO SOLIDS
Sample 0
M1BLKA51 A1 - 7
AN31 -1-6
Mi Iyo1
SV76-2-5
P-l
P-2
P-3
P-4
P-5
P-6
VI
P-H
nc23_	NC24	NC25
1.2	2.0	2.9
3.5	3.6 3.9
0.32
11.9	7.6	5.2
36	17	7
6.8	5.3	4.4
54	44	28
3.3	3.5	3.9
12	6.3
1.30 1.9	2.4
0.86 1.1
5.3	4.1	4.2
ALIPHATIC TRACTION CONCENTRATIONS (ug/1)
NC26 NC27 NC28 NC29 NC30
4.3	6.0			_	_
4.3	5.1	3.0	3.2	2.5
4.2	4.8	3.0	3.2	3.1
26							_
4.3	5.8	3.8	3.4	2.7
1.9	4.2	2.8	2.6	2.1

-------
63 - 2004 H
i ,: ; ; S)et 11
; U »: ffi cM'
F1 (Aliphatic) Fraction
$
^ w
i • I 5 b
I ' J 5 ! W,
FIGURE XI C. CAPILLARY COLUMN GAS CHR0MAT0GRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-5.

-------
XI C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample #
Resolved (mg/1;
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
.08S
0
.089
Mi 1 gel
.15
0
.147
SV76-2-5
.48
.433
.912
P-l
2.5
3.060
5.53
P-2
.29
.134
.426
P-3
1.36
1.50
2.86
P-4
.28
0.17
.442
P-5
- -
1.83
1.37
P-6
. C-8
0
.038
P-7
. C3C
0
.030
P-S
^ i r>
»
0.61
1.71
ZOO

-------
XI c. P-5 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT §
Concentration (ug/1)
*Methyl-(methyl ethyl)-benzene
1076
0.27
Dimethy1 ethyl benzene
1083
1.9
Methylpropenylbenzene
1143
0.31
Naphthalene
1174
0.34
2-Methy1 naphthalene
1291
0.84
1-Methy1 naphtha1ene
1,1'-Biphenyl
1299
0.84
1372
0.75
~Dimethyl naphthalene
1393
0.31
*Dimethyl naphthalene
1409
0.84
Methy-l»r-bi phenyl
1476
0.36
Methyl ethylnaphthalene
1494
2.9
*Trimethylnaphthalene
1514
1.5
*Trimethylnaphthalene
1520
2.4
*Trimethy1 naphtha 1ene
1538
1.2
*Trimethylnaphthalene
1554
0.88
*Trimethylnaphthalene
1571
1.0
~Methyl-(methyl ethyl)-naphthalene
1662
0.73
Phenanthene
1770
0.44
Methyldibenzothi ophene
1840
2.5
*Methylpehnanthene
1B85
0.96
*Methylphenanthene
1890
0.31
201

-------
XI c. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample *
Resolved (ug/1)
Unresolved(ug/1)
Total (ug/1)
MIBL;
-------
83 - 2004 F3
ro
O
CO
-*~
m	•
i F3 (Polar) Fraction
JL_
FIGURE XI C. CAPII LAKY COLUMN GAS CHROMATOGRAM OK THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-5.
A

-------
XI D. DISSOLVED 5I0ASSAY PHASE - TUTaL RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS*
Sample *
Total Resolved Components
(mg/1)
Total Unresolved Components
(mg/1)
MIBLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
6.63
P-l
.358
.603
P-2
o
o
l/l
00
o
o
3-3
I •»
o
6.49

.002
.011
P-5
.166
1.16
>-6
.043
0
P- 7
.175
0
P-8
.161
2.42
*Concentrations expressed per unit volume of wet saj.ple.
D-.ssc'vea Bioassay Phase sample were not fractionated intc
al i or.at-: c f r 1; , aromatic (FZ) or polar (F3) factions due
to tne cromctcgraphic simplicity of the samples.


-------
XI D. (cont.) P-5 DRILLING FLUID - DISSOLVED BIOASSAV PHASE COMPONENTS
ompounc Name
KOVAT No
Concentration !.c.
. » a
C 7—A1 cohol
Cg-Alcohol
Ethylhexanol
Cg-Ketone
Benzoic Acid
Methoxyben za1dehyde
C^-Ketone
Molecular Ion m/e 3 170
Cis-Carboxylic Acid
C^g-Carboxylic Acid
Ci9-Carboxy1ic Acid
911
1022
1035
1066
1234
1411
1500
1550
2162
2304
2447
13.5
6.0
2.3
2.8
.3
3.4
15.7
.8
1.2
1.0
4.1
a
Concentrations expressed per unit volume of wet sample.
205

-------
ro
o
en
fe i
1 "	m
P I	I S IS ft =
""" °- ^„W^Sr!T-« °f « ¦°'«0l»E0 P„«5E" BIOASSAY P«EPMAT,0((

-------
XII. HUD IDENTIFICATION: P6-1-2
LAB NUMBER:	83-3312
A.	Drilling Hud EloMntal Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
D.	lissolved Bloassay Phase Organic Concentrations
207

-------
XII A. DRILLING MUD ELEMENTAL CONCENTRATIONS
P6-1-2 (Sample I.D.: 83-3312)
Element
— ...
Whole Muda
1
Particulate Phase
Bioassay Preparation"
Oi sso"I ved Phase
Bioassay Preoarat'co-
A1
5.10(%)
1012.
0.021
Ba
18.8(%)
15.8
0.134
Cd
10.5
0.556
0.017
Ca
0.19(30
	
	
Cr
41.8
1.06
0.227
Cu
35.1
2.18
0.002
Fe
2.51 (%)
1243.
0.108
Pb
210.
10.2
0.003
Sr
120.
	
	
Zn
1755.
80.4
0.007
h2o
78.1(2)
	

Concentrations expressed as ug/g dry weight unless otherwise indicated
Concentrations expressed as ug/g wet weight unless otherwise indicated
208

-------
83 - 3312 F1
,ZS

F1 (Aliphatic) Fraction
ro
O

8B
i
:u
iiiiidiiii
h

•
r

s
<
t

i
t
1




i i
E




i

It





•
1
m
•
r*



I
i
4
<•
i
-
-
u

-I

*
r r
[i
c
c
L
FIGURE XII C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-6.

-------
XT! B. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

A1 iphatlc
Fraction

Aromatic Fraction
Sample *
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1!
UCM {mg/1)
.HISLKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
IBS.
419.

98.5
194.
Wi1 gel
.004
0

.004
0
SV76-2-5
464.
966,

166.
330.
P-l
2,700.
4,200.

636.
964,
P-2
252.
800.

47.6
228.
P-3
1,250,
5,970.

230.
445.
P-4
132.
548.

106.
103.
P-5
284.
546.

207.
183.
P-6
10.1
12.3

6.5
4.5
P-7
32. i
69.1

14.4
25.6
P-8
204,
270.

86.9
'64,
*A11 concentrations expressed per unit voljme of wet samole.
210

-------
XII B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (»g/l)*
Sample I

HIDLKA51 Al-7
AN31-1-6
Milgel
SV76-2-5
P-l
P-2
P- 3
P-4
P-5
P-6
P-7
P-6
N-Cg
N-Cio
N-Cu
_
3640
1100
182
2600
3300
55
5400
137
357
6220
9990
3450
28,400
101,000
385
2440
6340
-
5810
28,200
181
1650
3170
-
2060
4570
30.9
699
684
-
493
690
1930
4450
8790
N-C
12
1540
6440
91
19,200
112,000
9050
45,500
3640
7370
	116^
602
10,400
N-C
13
1810
8310
182
27,600
141,000
13,100
63,900
5430
13,200
161
N-C
14
1130
12,600
2030
9790
182
33,000
151,000
17,200
77,500
6800
18,500
214
1800
13,000
N-C
15
2420
13,600
128
41,500
201,000
20,000
97,500
9470
24,700
299
2610
15,800
N-C
16
2420
14,000
73
36,500
197,000
21,100
96,300
12,000
27,600
350
3130
14,900
N-C
17
vV
2250
10,800
72
26,200
94,000
12,200
92,400
11,400
24,400
360
3240
12,800
Prlstane
925
7110
36
13,900
42,900
6890
39,500
3260
7410
120
723
6720
N-Cia
Phytane
N-Ci9
1780
593
1330
8780
4250
7880
56
36
55
22,900
7960
19,200
148,000
43,400
121,000
11,900
4060
10,100
76,500
26,400
62,700
8490
2640
6390
18,800
5800
14,000
391
107
373
2670
808
2010
8850
2560
6420
*AM concentrations expressed per unit volume of wet sample

-------
XII B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (»g/1):*
Sample I
N_C20
n-c21
n-c22
N-C23
n-c24
n-c25
NC26
N-c27
N-C2B
n-c29
H-Cao
h-c31
HIBLKA5I Al-7
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-

Hllgel
55
55
55
-
-
56
-
-
-
-
-
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
i
a.
212
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
_
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-

P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
-
P-6
393
353
327
322
268
283
234
315
141
207
118
144
i i
GD
1550
4260
1120
3060
744
1860
434
1040
234
518
299
-
-
-
-
-

*AH concentrations expressed per unit volume of wet sample.

-------
XII B. (cont. )P-6 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT No.
Concentration (ug/1)a
Trimethylbenzene
992
10.7
Naphthalene
1178
11.3
2-Methylnaphthalene
1288
30.4
1-Methylnaphthalene
1304
24.0
~Dimethyl naphthalene
1398
33.6
~Dimethyl naphthalene
1413
14.5
~Dimethyl naphthalene
1433
23.5
~Dimethyl naphthalene
1448
10.1
Methyl-1,1'-biphenyl
1482
13.4
Methyl ethyl naphthalene
1498
9.01
*Trimethylnaphthalene
1521
7.69
~Trimethylnaphthalene
1525
15.8
~Trimethylnaphthalene
1541
35.6
~Trimethylnaphthalene
1557
42.1
Methyl-(methyl ethyl)-Naphthalene
1666
8.56
Phenanthrene
1771
24.2
~Methylphenanthrene
1886
9.73
~Methylphenanthrene
1911
9.27
Dimethylphenanthrene
2027
8.13
|
~Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
Concentrations expressed per jnit volume of wet sample.
213

-------
• li

l#V

- n
JU'JL
-A.
HGURE XII B. CAP I LI ARY COl UMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND AROMATIC
(B) FRACTIONS OF WHOLE DRILLING FLUID P-6.

-------
XII C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample *
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mi 1 gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P-l
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11 .45
15.8
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0 |
0.039
P-7
0.063
i
0 i
0.063
P-8
0.690
0.68
1.37
215

-------
XII C. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (u
-------
XII C. DRIIIING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (,,g/1)

Sample #
Pristane
NCja
Phytane
nc19
nc20
NC2i
nc22

MIBLKA51 A1 7

0.11

0.15

0.14
0.50

AN31-1-6
14.a
17.9
9.0
15,1
9.6
6.8
4.6

Mi lye 1
0.45
0.70
0.29
0.58
0.39
0.28
0.21

SV76-2-5
54.8
85.6
30.1
66.6
43.4
33.0
20,6

P~1
142
366
119
302
203
143
78

P~2
30
41
15
33
24
17
11

^ P-3
135
229
92
196
171
119
84

P-4
17
36
11
24
13
7.5
4.3

P 5
43
10}
39
79
54
37
22

P-6
0.32
0.52
0.17
0.61
0.50
0.56
0.76

p-;
2.0
3.3
i 2
2.5
1.6
1.1
0.83

p-e
23
32
10
25
18
13
8.2

		 		 .
	 		
			
	





-------
XII C. DRILLING FLUID SUSPENDED SOLIDS
Sample It
nc23
nc24
NC25
MIBLKA5I Al-/
1.2
2.0
2.9
AN31-1-6
3.5
3.6
3.9
MiIgel
	
	
0.32
SV76-2-5
11.9
7.6
5.2
P-I
36
17
7
P-2
6.8
5.3
4.4
£ P-3
P-4
54
3.3
44
3.5
28
3.9
P-5
12
6.3

P-6
1.30
1.9
2.4
P-7
0.86
1.1

P-8
5.3
4.1
4.2




ALIPHATIC FRACTION CONCENTRATIONS (wg/l)
NC26 NC27 NC28 NC29 NC3()
4.3	6.0
4.3	5.1	3.0	3.2	2.5
4.2	4.8
26 	
4.3	5.8
3.0	3.2	3.1
3.8	3.4	2.7
1.9	4.2	2.8	2.6	2.1

-------
XII C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
Total (mg/i)
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
.088
C
.089
Mil gel
.15
-0
..147
SV76-2-5
.48
.433
.912
P-l
2.5
3.C60
5.53
P-2
.29
.134
.426
P-3
1.36
1.50
2.86
?-4
.28
0.17
.442
P-5
^ '
• v
1.83
1.37
P-6
.038
0
.038
P-7
P-8
.030
i
i
i
0
0.61
.030
1.71
219

-------
XII C. P-6 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
2-Methylnaphthalene
1291
0.07
1-Methylnaphthalene
1307
0.06
220

-------
XII c. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample #
Resolved (ug/1)
Unresolved (ug/1!
Total (ug/1)
MIBLKA51 Al-7
25.0
0
25.2
AN 31-1-6
497
0
497
Mil gel
118
0
118
SV76-2-5
1630
0
1630
P-l
950
0
950
P-2
1380
0
1380
P-3
1120
3
1120
P-4
147
0
147
P-5
165
u
165
P-6
13.6
0
13.5
P-7
478
0
478
P-3
836
0
336
222

-------
XII D. DISSOLVED BIOASSAY PHASE - TOTAL RESOLVED AiiD UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Total Unresolved Components
(mq/1)
MIBLKA51 Al-7
.358
.813
AN31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
6.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
P-5
.166
1.16
P-6
.043
0
P-7
P-8
.175
.161
0
2.42
~Concentrations expressed per unit volume of wet sample.
Dissolved 3ioassay Phase sample were not fractionated into
aliphatic (Fl), aromatic (F2) or polar (F3) fractions due
to the chromotograohic simplicity of the samples.
224

-------
XII o, (cont.) P-6 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Compound Name
KOVAT No
.oncentr* vo*
C7-A1cohol
Cg-Alcohol
Ethylhexanol
Benzoic Add
Molecular Ion m/e « 170
C^g-Carboxylic Acid
913
1022
1033
1219
1556
2160
5.5
.1
.1
-2
.4
Concentrations expressed per unit volume of wet sample
225

-------
I D. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "OISSOLVED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-6.

-------
XIII. MUD IDENTIFICATION: P7-1-2
LAB NUMBER:	83-3313
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
0.	: issolved Bloassay Phase Organic Concentrations
227

-------
XIII A. DRILLING MUD ELEMENTAL CONCENTRATIONS
P7-1-2 (Sample I.D.: 83-3313)
Element
Whole Muda
Particulate Phase
Bioassay Preoarat:onD
Di sso* ved 3hase
Bioassay Preparation*3
A1
4.47( *)
1010.
0.011
Ba
21-0(2;)
19.4
0.328
Cd
0.21
0.018
0.001
Ca
0.46(*)
	

Cr
502.
35.6
0.436
Cu
15.6
0.932
0.021
Fe
2.25(%)
1001.
0.288
_ _pb._.
92.1
1.45
0.004
Sr
258-
	
	
Zn
144,
6.30
0.007
h2o
69.9

.
Concentrations expressed as ug/g dry weight unless otherwise indicated
Concentrations expressed as ug/g wet weight unless otherwise indicated
228

-------
XIIIB. WHOLE MUD - RESOLVED AND UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic
Fraction

Aromatic Fraction
Sample *
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/1)
UCM (ng/1)
MIBLKA51 Al-7
34.5
0

9.83
12.3
AN31-1-6
185.
419.

98.5
194.
Milgel
.004
0

.004
0
SV76-2-5
464.
966.

166.
330.
P-l
2,700.
4,200.

536.
964.
3-2
252.
300.

47.6
228.
P-3
1,260.
5,970.

- 230.
445.
P-a
132-
548.

TOE- .
103.
?-5
234.
646.

207.
133.
P-6
10.1
12.3

6.5
4.5
P-7
32.
69.1

14.4
25.6
P-3
204.
270.

36.9
164.
*A11 concentrations expressed per unit volume of wet sample.
229

-------
XIII B. (cont.) whole DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (u9/l)*
Sample I
n-c9
N-Cio
N'Cji
N Ci2
"-<43
n-c,4
*C15
N"C16
N'C, 7
Pristine
n-Ci8
Phytane
N-C,g
MIBLKA51 Al-7

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-1-6
182
2600
3300
6440
8310
9790
13,600
14,000
10,800
7110
8780
4250
7880
Milgel
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151,000
201,000
197,000
94.000
42,900
148,000
43,400
121,000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
£ P-3
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76,500
26,400
62,700
o
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18.800
5800
14,000
P-6
30.9
699
684
116
161
214
29?
350
360
120
391
107
373
P- 7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
16.600
14,900
12,800
6720
8850
2560
6420
*A11 concentrations expressed per unit volume of wet sample.

-------
w
XIII B. (cont.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/1)*
Sample H
n-c20
N"C2l
n-c22
n-c23
n-c24
i
N-C25
NC26
n-c27
n-c28
n-c29
N"C30
n-c3i
HKBLKA51 A1-7
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-
-
Milgel
55
55
55
-
-
56
-
-
-
-
-
-
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
96,400
65,700
41,300
23,300
10,700
5090
-
-
-
-
-
-
no P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
^ P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
4280
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
3270
1480
-
-
-
-
-
-
-
P-6
393
353
327
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
-
-
-
-
•All concentrations expressed per unit volume of wet sample.

-------
XIII B(cont). p.7 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT No.
Concentration (ug/1)
Trimethylbenzene
Methyl propyl benzene
Naphthalene
2-Methylnaphthalene
1-Methylnaphthalene
1,1'-Biphenyl
~Dimethyl naphthalene
~Dimethyl naphthalene
~Dimethyl naphthalene
~Dimethyl naphthalene
Methyl-1,1'-biphenyl
Methyl ethyl naphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Trimethylnaphthalene
~Methyl -(methylethyl)-Naphthalene
~Methyl-(methyl ethyl)-Naphthalene
Phenanthrene
Methyldibenzothiophene
*Methylphenanthrene
~Methy1p henan threne
~Methylphenanthrene
*Dimethylphenanthrene
~Dimethylohenanthrene
990
1143
1175
1285
1301
1372
1395
1410
1429
1444
1479
1496
1518
1522
1555
1572
1642
1663
1767
1841
1888
1883
1907
2003
2022
17.3
47.0
25.9
340.
136.
35.9
339.
169.
105.
90.2
170.
354.
106.
157.
394.
102.
224.
109.
137.
52.3
74.5
120.
71.8
107.
127,
~Structural isomer(s) of the compound indicated. Exact identification of individual isomer
not possible with the GC/MS analytical protocol employed. KOVAT index can be utilized for
comoarison and evaluation of isomers among samples.
a
Concentrations expressed per unit volume of wet sample.
232

-------
W-Mi..
FIGURE XIII B. CAP 11 LARV COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A) AND
AROMATIC (B) FRACTIONS OF WHOLE DRILLING FLUID P-7.

-------
XIIIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (ng/1)
Unresolved (..g/1)
Total ( g/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Milael
0.016
0
0.016
SV76-2-5
1.56
1.96
S.52
P- :
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45 1
15.3
P-4
0.462
0
0.462
P-5
1.55
2.19
3.74
P-6
0.039
0
0.039
P-7
0.063
0
0.063
P-8
0.690
0.68 !
1.37
234

-------
XI lie. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (uq/1)
Sample tt
N f.g
NC10
NC|i
NC12
NC13
NCm
NC,5
NC16
ncI7
MIBLKA51 Al-7
_.
0.12
0.29
0.46
0.88
0.73
0.34
0.20
0.25
AN31-1-6

2.37
7.0
10.7
15.4
18.3
21.7
23.41
23.39
Mi igel
0.09
0.25
0.43
0.51
0.69
0.84
0.84
0.91
0.90
SV 76-2-5
_
/. b8
27.2
52.6
86.7
no
129
119
113
P-l
12.0
72.6
198
274
362
391
448
489
481
P-2
2.7
7.6
14
22
33
42
50
54
51
P-3
_
15
6b
124
194
239
289
279
280
P-4
no ' ^
0.96
3.8
8.3
11
19
26
36
46
51
w P-5

7.0
15
30
62
93
113
132
127
P-6
0-20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.57
P-7

0.37
0.68
0.97
1.6
2.3
3.2
4.2
4.4
P-8
2.1
8.4
20
28
37
43
46
47
41

-------
XI1IC. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)

Sample §
Pristdne
NC | o
Phytane
nc19
N°20
NC2i

MIBLKA51 A1 -7

0.11

0.15

0.14

AN31-1-6
14.8
17.9
9.0
15.1
9.6
6.8

MiIgel
0.45
0.70
0.29
0.58
0.39
0.28

SV76-2-5
54.8
85.6
30.1
66.6
43.4
33.0

P-l
142
368
119
302
203
143

P-2
30
41
15
33
24
17

P-3
135
229
92
196
171
119
236
P-4
17
36
11
24
13
7.5

P-5
43
101
39
79
54
37

P-6
0.32
0.52
0.17
0.61
0.50
0.56

P-/
2.0
3.3
1.2
2.5
1.6
1.1
P-8
23
32
10
25
18
13
NC.
22
0.50
4.6
0.21
20.6
78
11
84
4.3
22
0.76
0.83
8.2

-------
XIIIC
DRILLING FLUID SUSPENDED SOLIDS
Sample #
MIULKA51 A1 -7
AN31-1-6
Mi I ye I
SV76-2-5
P-l
P-2
P-3
ro
S P-4
P-5
P-6
P-/
P-8
^23_	^c25
1.2	2.0	2.9
3.b 3.6	3.9
0.32
11.9	7.6	5.2
3b	17	1
6.8	5.3	4.4
54	44	28
3.3	3.5	3.9
12	6.3
1.30	1.9	2.4
0.86	1.1
5.3	4.1	4.2
ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
NC26	NC27	HC2q	NC29	NC3o	NC31 NC32
4.3	6.0						
4.3	5.1	3.0	3.2	2.5 _		
4.2	4.8	3.0	3.2	3.1 			
26
4.3	5.8	3.8	3.4	2.7 			
1.9	4.2	2.8	2.6	2.1	1.9
vV

-------
83 - 3313 I I
F1 (Aliphatic) Fraction
& &?
*5 i ®.
s - Jrt £ir* ¦ |D >|
MM-44++4+W- W-'#
n

i
*
«
rt
i?
>
*
if
*



S 6 t t I I i *
s » a i j jjf
a iilu^
XIII C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-7.

-------
XIIIC. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample *
Resolved (mg/1)
Unresolved (mg/1)
f
Tota: ( mg/i)
MIBLKA51 Al-7
.072
0
.373
AN 31-1-6
.088
0
.089
Mi1gel
.15
0
..147
SV76-2-5
.48
.433
.912
P-i
2.5
3.060
5.53
P-2
.29
.134
.426
P-3
1.36
1.50
2.86
P-4
.28
0.17
.442
P-5

1.83
1.37
P-6
. C38
0
.038
P-7
. 03C
0
.030
5-8
T-''- | 0.61
1
1
1.71
239

-------
XIII C. P-7 SUSPENOED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
2-Methyl naphthalene
1290
4.1
1-Methyl naphtha1ene
1306
2.1
*Tr1methy1naphthalene
1524
0.48
240

-------
B3 - 3313 F2
F2 (Aromatic) Fraction
ro
XA". .i
if
¦^4^* |4 —)
FIGURE XIII C. CAPIIIARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY
PREPARATION OF SPENT DRILLING FLUID P-7.

-------
XIlie. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample *
Resolved (yg/l)
Unresolved(ug/1)
Total (ug/D
MI3L.
-------
83 - 3313 F3
F3 (Polar) Fraction

FIGURE XIII C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY
PREPARATION OF SPENT DRILLING FLUID P-7.

-------
XII ID. DISSOLVED 31 OAS SAY PHASE - T'JTAL RESOLVED AiiD UNRESOLVED COMPONENT CONCENTRATIONS*
Sample #
Total Resolved Components
(mg/1)
Tota". Unresolved Components
(mg/1)
MIBLKA51 Al-7
.358
.813
AN 31-1-6
.136
1.24
Mil gel
.0783
0
SV76-2-5
.920
6.63
P-l
.358
.603
P-2
.005
.008
P-3
1.09
6.49
P-4
.002
.011
P-5
.166
1.16
P-6
.043
0
P-7
.175
0
P-8
.161
2.42
•Concentrateons expressed per* unit volume of wet sample.
DissolveG Bioassay Phase sample were not fractionatec into
aliphatic rFl), aromatic (F2) or polar (F3J fractions aue
to the chromotograpmc simplicity of the samples.
244

-------
XIII D. (cont.) P-7 ORILLING FLUID - DISSOLVED 3I0ASSAY PHASE COMPONENTS
Compound Name
K3VA7 No
Concentrator '.c, * "a
Cy-Alcohol
Cg-AlC0h0l
Cg-Ketone
Benzoic Acid
Methoxybenzaldehyde
C^-Ketone
Molecular Ion m/e » 170
Methoxybenzoic Acid
Molecular Ion m/e = 199
Hexadecanoic Acid
Cia-Carboxylic Acid
912
1021
1065
1221
1406
1500
1552
1584
1671
1972
2161

.4
9.9
3.4
1.6
4.9
17.5
6.2
8.2
1.8
1.4
1.5
a
Concentrations expressed per unit volume of wet sample.
245

-------
~ ~
*
<4 ¦
rv>
-P»
cr>

«K S

FIGURE XIII D. CAPIILARY COLUMN GAS CHROMATOGRAM OF THE "DISSOLVED PHASE" BIOASSAY
PREPARATION OF SPENT DRILLING FLUID P-7.

-------
XIV. MUD lOOfTIFICATlOH: P8-1-1
LAB NUMBER:	83-8537
A.	Drilling Mud Elemental Concentrations
B.	Whole Drilling Mud Organic Concentrations
C.	Particulate Bloassay Phase Organic Concentrations
0.	.issolved BloassayiPtesft;Organic Concentrations
247

-------
XIV A. DRILLING MUD ELEMENTAL CONCENTRATIONS
P8-1-1 (Sample I.D.: 83-8537)
Element
Whole Muda
Particulate Phase
Bioassay Preparation*5
Gis so *ved Phase
Bicassay Preparation-3
A1
0.68(%)
398.
0.026
Ba
3.00(%)
15.9
0.302
Cd
0.410
0.024
0.002
Ca
1.54(5)

	
Cr
480.
133.
11.0
Cu
3448.
16.0
0.268
Fe
1.25(%)
802.
1.39
Pb
f)
00
<1"
5.20
0.199
Sr
1401.


Zn
144.
22.6
0.185
h2o
58.1
	
	
Concentrations expressed as ug/g dry weight unless otherwise indicated.
^Concentrations expressed as ug/g wet weight unless otherwise indicated.
243

-------
XIV B. WHOLE MUD - RESOLVED ANO UNRESOLVED ORGANIC COMPONENT CONCENTRATIONS*

Aliphatic
Fraction

Aronatic Fraction
Sample *
Resolved (mg/1)
UCM (mg/1)

Resolved (mg/i;
JCM (rng/1)
MI3LKA51 Al-7
34.5
0

9.33
;2.3
AN31-1-6
185.
419.

98.5
194.
Ml 1 gel
.004
0

.004
0
SV76-2-5
464. *
966.

:66.
330.
P-l
2,700.
4,200.

636.
964.
P-2
252.
800.

47.6
228.
P-3
1,260.
5,970.

230.
445.
P-4
132.
548.

"TO6. ;
103.
P-5
284.
646.

207.
183.
?-6
10-1
12.3

5.5
4.5
=>-7
32.2
69.1

:4.4
25.5
P-8
204.
270.

36.9
154.






*A11 concentrations expressed per unit volume of wet sample.
249

-------
XIV B. (com.) UHOLF DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (pg/1)*
Sample §
n-c9
N-Cio
N"C, i
N-Ci?
"Cl3
n-c14
NC15
NC16
N"c17
Prtstane
N-C18
Phytane
n-c19
HIBLKA51 Al-7

3640
1100
1540
1810
2030
2420
2420
2250
925
1780
593
1330
AN31-1 6
182
2600
3300
6440
8310
9790
13,600
14,000
10,800
7110
8780
4250
7880
Milgel
55
5400
137
91
182
182
128
73
72
36
56
36
55
SV76-2-5
357
6220
9990
19,200
27,600
33,000
41,500
36,500
26,200
13,900
22,900
7960
19,200
P-l
3450
28,400
101,000
112,000
141,000
151,000
201.000
197,000
94,000
42,900
148,000
43,400
121.000
P-2
385
2440
6340
9050
13,100
17,200
20,000
21,100
12,200
6890
11,900
4060
10,100
ro
P-3
o
-
5810
28,200
45,500
63,900
77,500
97,500
96,300
92,400
39,500
76.500
26,400
62,700
P-4
181
1650
3170
3640
5430
6800
9470
12,000
11,400
3260
8490
2640
6390
P-5
-
2060
4570
7370
13,200
18,500
24,700
27,600
24,400
7410
18,800
5800
14,000
P-6
30.9
699
684
116
161
214
299
350
360
120
391
107
373
P-7
-
493
690
602
1130
1800
2610
3130
3240
723
2670
808
2010
P-8
1930
4450
8790
10,400
12,600
13,000
15,800
14,900
12,800
6720
8850
2560
6420














*A11 concentrations expressed per unit volume of wet sample.

-------
XIV B. (cant.) WHOLE DRILLING FLUID - ALIPHATIC FRACTION CONCENTRATIONS (ug/D*
Sample H
n-c20
n-c2i
n-c22
NC23
N~c24
n-c25
n-c26
nc27
n-c28
n-c29
N-Cao
"-c31
M1BLKASI AI - 7
940
780
478
289
144
111
-
-
-
-
-
-
AN31-1-6
5270
3900
2510
1570
836
521
245
285
-
-
-
-
Milyel
55
5b
55
-
-
56
-
-
-
-
-
"
SV76-2-5
13,800
11,300
8040
5330
3460
2280
1440
1740
725
1160
429
1530
P-l
% ,400
65.700
41,300
23,300
10,700
5090
-
-
-
-
-
-
r\j P-2
8000
6380
4730
3320
2050
1810
1040
949
398
795
719
-
~ P-3
53,700
44,600
34,800
23,300
14,500
8860
6540
-
-
-
-
-
P-4
42B0
2520
1580
1060
728
615
458
716
461
655
-
-
P-5
11,400
7900
5440
32/0
1480
-
-
-
-
-
-
-
P-6
393
353
327
322
268
283
234
315
141
207
118
144
P-7
1550
1120
744
434
234
-
-
-
-
-
-
-
P-8
4260
3060
1860
1040
518
299
-
-
-
-
-
-













*A11 concentrations expressed per unit volume of wet sample.

-------
XIV B.(cont.)P-8 WHOLE DRILLING FLUID - AROMATIC FRACTION CONCENTRATIONS
Compound Name 1
i
KOVAT No.
Concentration (ug/1)a
Trimethylbenzene
!
991
234
Dimethyl ethyl benzene
1060
142
Methyl - (methylethyl)-benzene
1087
250
2-Methylnaphthalene
1287
3350
1-Methylnaphthalene
1303 ]
2060
l»l'-b1phenyl
1373
399
~Dimethyl naphthalene
1397
4300
*0imethyl naphthalene
1412 1
2340
~Oimethylnaphthalene
1431
1130
~Oimethylnaphthalene
1446
998
Methyl-1,1'-biphenyl
1480
1240
Methyl ethyl naphthalene
1497
1220
~Trimethylnaphthalene
1519
1280
~Trimethylnaphthalene
1523
1860
~Trimethylnaphthalene
1540
661 *
~Trimethylnaphthalene
1555
619
~Trimethylnaphthalene
1579
503
Propenylnaphthalene
1586
695
~Methyl -(methylethyl)-Naphthalene
1643
530
~Methyl -(methylethyl)-Naphthal ene
1664
811
~Methyl-(methyl ethyl)-Naphthalene
1680
319
Phenanthrene
1768
1100
~Methylphenanthrene
1884
1030
~Methylphenanthrene
1890
768
~Methylphenanthrene
1909
462
~Methy1phenanthrene
1913
171
~0imethy1phenanthrene
2005
374
~Dimethylphenanthrene
2024
784
~Dimethylphenanthrene
2138
302
~Dimethylphenanthrene
2144
¦
189
!
~Structural isomer(s) of the compound indicated. Exact identification of individual isorrer
not oossible with the SC/MS analytical orotocol employed. KOVAT index can be utilized for
comparison and evaluation of isomers among samples.
a
Concentrations expressed per unit volume of wet sample.
252

-------
FIGURE XIV B. CAPILLARY COLUMN GAS CHROMATOGRAMS OF THE ALIPHATIC (A)
AND AROMATIC (B) FRACTIONS OF WHOLE DRILLING Fl Mil) P-8.

-------
XIV C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED CONCENTRATION - ALIPHATIC FRACTION
Sample #
Resolved (mg/1)
Unresolved (mg/1)
j Total lug/1)
MIBLKA51 Al-7
0.046
0
0.046
AN31-1-6
0.325
0
0.325
Mi 1 gel
0.016
0
0.016
SV76-2-5
1.56
1.96
3.52
P- i
6.43
7.78
14.2
P-2
0.694
0
0.694
P-3
4.35
11.45
15.8
P-4
0.462
0
0.462
P-5
j 1.55
2.19
3.74
P-6
j 0.039
0
i
0.039
P-7
j 0.063
1
0
0.063
D-8
0.690
0.68
1 .37
254

-------
XIVC. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample H
n-c9
NC10
NCn
nc12
NCn
nc14
^15
NC16
NO,?
MJBLKA51 Al-/
. ..
0.12
0.29
0.46
0.88
0.73
0.34
0.20
0.25
AN31-1-6
—
2.37
7.0
10.7
15.4
18.3
21.7
23.41
23.39
MiIgel
0.09
0.25
0.43
0.51
0.69
0.84
0.84
0.91
0.90
SV76-2-5
	
/. 58
27.2
52.6
86.7
110
129
119
113
P-l
12.0
72.6
198
274
362
391
448
489
481
P-2
2.7
7.6
14
22
33
42
50
54
51
P-3

15
65
124
194
239
289
279
280
P-4
0.96
3.8
8.3
11
19
26
36
46
51
S P-5
	
7.0
15
30
62
93
113
132
127
P-6
0.20
0.21
0.24
0.21
0.24
0.25
0.28
0.39
0.57
P-7
	
0.37
0.68
0.97
1.6
2.3
3.2
4.2
4.4
P-8
2.7
8.4
20
28
37
43
46
47
41



-------
XIV c. DRILLING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (pg/1)
Sample $
Pristane
nc18
Phytane
nc19
nc20
NC2i
nc?2

MlBLKA51 Al-7

0.11

0.15

0.14
0.50

AN31-1-6
14.8
17.9
9.0
15.1
9.6
6.8
4.6

Hilyel
0.45
0.70
0.29
0.58
0.39
0.28
0.21

SV 76-1?-5
54.8
85.6
30.1
66.6
43.4
33.0
20.6

P-l
142
368
119
302
203
143
78

P-2
30
41
15
33
24
17
11

P-3
135
229
92
196
171
119
84
ro
ui
cn
P-4
17
36
11
24
13
7.5
4.3
P-5
43
101
39
79
54
37
22

P-6
0.32
0.52
0.17
0.61
0.50
0.56
0.76

P-7
2.0
3.3
1.2
2.5
1.6
1.1
0.83

P-8
23
32
10
ft
19
13
8.2

-------
XIVC. ORIILING FLUID SUSPENDED SOLIDS - ALIPHATIC FRACTION CONCENTRATIONS (Mg/1)
Sample H
nc23
NC24
NC25
NC26
NC27
nc28
nc29
nc30
nc31
NC32
MIBIKA51 Al-7
1.2
2.0
2.9







AN31-1-6
3.5
3.6
3.9
4.3
6.0
	
	

	
		
HiIgel

	
0.32
	
	
	
_—
	
	
	
SV76-2-5
11.9
7.6
5.2
4.3
5.1
3.0
3.2
2.5
. .
	
P-l
36
17
7







P-2
6.8
5.3
4.4
4.2
4.8
3.0
3.2
3.1
_____
		
P-3
54
44
28
26

_

	
	
	
ro P-4
tn
3.3
3.5
3.9
4.3
5.8
3.8
3.4
2.7
—

P-5
12
6.3
		
.. 	
. _

	
	
	
	
P-6
1.30
1.9
2.4
1.9
4.2
2.8
2.6
2.1
1.9

P-7
0.86
1.1



_
__
	
	
		
P-8
5.3
4.1
4.2










-------
83 - 8537 Fl
ro
(_n
03
M
Fl (Aliphatic) Fraction
J-*
FIGURE XIV C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY PREPARATION
OF SPENT DRILLING FLUID P-8.

-------
XIV C. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - AROMATIC FRACTION
Sample 4
Resolved (rtig/1)
Unresolved (ing/T)
(mg/D
MIBLKA51 Al-7
.072
0
.073
AN 31-1-6
.088
0
.089
Mi 1 gel
.15
0
'.147
SV76-2-5
.48
.433
.912
P-l
2.5
3.060
5.53
P-2
.29
.134
.426
P-3
1.36
1.50
2.86
P-4
.28
0.17
.442
?-5
Z, .
» — -
1.83
1.37
P-6
.038
0
.038
P-7
i .030
0
.030
P-8
	lil;	
0.61
	 . 		
1.71
l
259

-------
XIV C. P-8 SUSPENDED PHASE - AROMATIC FRACTION CONCENTRATIONS
Compound Name
KOVAT #
Concentration (ug/1)
Trimethylbenzene
993
10.1
Dimethyl ethyl benzene
1058
3.0
2-Methylnaphthalene
1292
109
1-Methy1 naphthalene
1308
70
1.1' -bipheny
1378
12.8
*01 methyl naphthalene
1394
3.3
*D1methy1naphthalene
1418
47.3
*Dimethylnaphthalene
Methyl-1,l'-bipheny
1445
1.0
1481
2.3
Methyl ethylnaphthalene
1494
8.5
*Trimethynaphthalene
1520
5.5
*Trimethynaphtha1ene
1525
15.3
*Tr1methynaphthalene
1555
1.2
*Trimethynaphthalene
1580
12.3
Propenylnaphthalene
1585
6.2
*Methyl-(methyl ethyl)-naphthalene
1642
1.3
*Methyl-(methyl ethyl)-naphthalene
1664
0.55
*Methyl-(methyl ethyl)-naphthalene
1678
1.3
*Methylphenanthene
1892
7.8
*Methylphenanthene
1906
0.45
*D1methylphenanthene
2005
0.65
~Dimethylphenanthene
2146
0.95
260

-------
83 - 8537 F2
no
cta
u	;iu
J? tttJ
i F2 (Polar) Fraction
JL
FIGURE XIV C. CAPIlLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAV PREPARATION
OF SPENT DRILLING FLUID P-8.

-------
XIV c. SUSPENDED PHASE - RESOLVED AND UNRESOLVED COMPONENT CONCENTRATIONS - POLAR FRACTION
Sample *
Resolved (ug/1)
Jnresol ved (--g/1)
Total (ug/1 /
MI3LKA51 Al-7
25.0
0
r

-------
83 - 8537 F3
F3 (Polar) Fraction

FIGURE XIV C. CAPILLARY COLUMN GAS CHROMATOGRAM OF THE "SUSPENDED PHASE" BIOASSAY
PREPARATION OF SPENT DRILLING FLUID P-8.

-------
XIV D. DISSOLVED 310ASSAY PHASE - TUTAl RESOLVED AmD UNRESOLVED COMPONENT CONCENTRATIONS*
Sample *
	
Total Resolved Components
(mg/1)
Total Unresolved Components
(mq/1)
MIBLKA51 Al-7
.358
.813
AN31-1-6
.136
1.24
Mil ge"
.0783
0
SV76-2-5
.920
"6.63
P-l
.358
.603
P-2
.005
.008
D-3
1.09
6.49
P-4
.002
.011
P-5
.166
1.16
P-6
.043
0
7
.175
0
P-8
.161
2.42
^Concentrations exoressec per unit volume cf wet sample.
'Dissolved Bioassay Phase sample were not fractionated into
a'ipr.at-c (r 1}, aromatic [F2] or polar (F3) fractions due
tc tne chromatographic simplicity of the samoles.
264

-------
XIV D (cont). P-8 DRILLING FLUID - DISSOLVED BIOASSAY PHASE COMPONENTS
Conocund Name

-------
1. REPORT NO. 2.
EPA-600/3-84-048
3 RECIPIENT'S ACCESSION NC
PB84-170000
4. title and Subtitle
DRILL MUD ASSESSMENT
CHEMICAL ANALYSIS REFERENCE VOLUME
b REPOR" DA"E
March 1984
6. PERFORMING ORGANIZATION CODE
7. AUTHOR4S)
Science Applications, Ir.c.
8 PERFORMING ORGANIZATION R E PO RT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Science Applications, Inc.
Environmental Chemistry Division
La J olla, CA ^233S
10 program element no.
11 CONTRACT-GRANT SO
R - N — o 7 3 3 — ^ 3 —
12 SPONSORING AGENCY NAME AND ADDRESS
U.S. Envi rc nner. t a L Protection Agency
Environmental Research Lacoratcry
Office of Research and Development
C-ulf Breeze, Florida 325^1
13 TYPE OF REPORT AND PERIOD COVERED
14 SPONSORING AGENCY CODE
EPA/600/04
15. SUPPLEMENTARY NOTES
TECHNICAL REPORT DATA
'Please read instructions on the reverse before completing/
16. ABSTRACT
This report presents concentrations of specific metals and hydrocarbons
in eleven drilling fluids (muds) taken from operating gas and oil rigs in
the Gulf of Mexico. Each drillinng fluid was analyzed chemically for
heavy metal and hydrocarbon content in three distinct phases: (1) the
bulk or whole mud, (2) a suspended phase derived from the bulk mud sample,
and (3) a "dissolved" or liquid phase. Aliquots of bulk muds were
removed for barium analyses by instrumental neutron activation and for
analysis for iron, aluminum, lead, zinc, cadmium, copper, strontium, and
calcium by automic absorption anaysis. Analysis of the suspended
particulate and liquid phases was similar. The aromatic and aliphatic
content of the three phases were determined by extraction and then
fractionation by column chromatogrphy.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b IDENITI FIE RS OPE N E NOE D T= RMS C COSATI T lekl'Gl Cup
18. DISTRIBUTION STATEMENT
Release to oublic
19 SECJRITV CLASS -ifus AY/»<
unclassified
21 NO. Or PA(_. ES
i 272
20 ScCuritv class ¦Tinspi.w
ur.c-assi: iec
|22 p
R CE
EPA Form 2220-1 (Re*. 4-77) previous edition 15 obsc.ete
i

-------