DC
FIELD TEST KIT FOR OIL-BRINE EFFLUENTS
FROM OFFSHORE DRILLING PLATFORMS
by
R. T. Rewick, J. Gates, K. A, Saho
T. W. Chou, and J, H. Smith
SRI International
Menlo Park, California 94025
EPA Grant No. R8Q6091010
Project Officer
Leo T, McCarthy, Jr.
Oil and Hazardous Materials Spills Branch
Municipal Environmental Research Laboratory
Edison, New Jersey 08817
MUNICIPAL ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This report has been reviewed by the Municipal Environmental Research
Laboratory, U.S. Environmental Protection Agency, Edison, New Jersey, and
approved for publication. Approval does not signify that the contents neces-
sarily reflect the views and policies of the U.S. Environmental Protection
Agency, nor does mention of trade names or commercial products constitute
endorsement or recommendation for use.
ii
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FOREWORD
The U.S. Environmental Protection Agency was created because of increas-
ing public and government concern about the dangers of pollution to the health
and welfare of the American people. Noxious air, foul water, and spoiled land
are tragic testimonies to the deterioration of our natural environment. The
complexity of that environment and the interplay of its components require a
concentrated and integrated attack on the problem.
Research and development is that necessary first step in problem solution;
it involves defining the problem, measuring its impact, and searching for
solutions. The Municipal Environmental Research Laboratory develops new and
improved technology and systems to prevent, treat, and manage wastewater and
solid and hazardous waste pollutant discharges from municipal and community
sources, to preserve and treat public drinking water supplies, and to minimize
the adverse economic, social, health, and aesthetic effects of pollution.
This publication is one of the products of that research and provides a most
vital communications link between the researcher and the user community.
The objectives of the present research program were (1)_ to develop and
evaluate a field test kit for characterizing oil-brine effluents from offshore
drilling platforms and (2) to deliver to EPA the completely assembled kit with
detailed operating instructions for conducting each test method.
iii
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ABSTRACT
This research program was initiated to evaluate test methods for charac-
terizing oil-brine effluents from offshore oil production platforms and to
package and deliver a field test kit for on-site oil-brine analyses. After
an initial laboratory evaluation and selection of test methods and equipment,
two on-site oil-brine analyses of production water were conducted in Kenai,
Alaska—one at the AMACO Dillon Offshore Production Platform, and the other
at the Shell MGS Joint Onshore Facility. This report describes the methods
developed for the field test site, including detailed procedures for conduct-
ing each test method, and the results from the two on-site analyses.
This report was submitted in fulfillment of Grant No. R806091010 by SRI
International under the sponsorship of the U.S. Environmental Protection
Agency. This report covers the period October 9, 1978 to April 8, 1981, and
work was completed as of April 8, 1981.
IV
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CONTENTS
Foreward iii
Abstract iv
Figures vi
Tables vi
Acknowledgments vii
1. Introduction 1
2. Conclusions 3
Methods Review and Development 3
Recommended Tests for Field Test Kit 3
Field Results 5
3. Recommendations 6
4. Experimental Results 7
Methods Review and Development 7
Total Oil Content 7
Infrared Method 7
Gravimetric Method 7
Solvent Extraction Efficiency 11
Soluble Oil 11
Particle Size 11
Field Results 12
Oil-in-Water Results. ....". 12
Soluble Materials 12
Suspended Solids 12
Physical Properties of Oil and Water 15
Bacterial Culture 20
References ,,....., 22
Appendices
A. Instrumentation and Materials Provided in the Field Test Kit. . 23
B. Laboratory and Field Procedures 25
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FIGURES
Number Page
1 Assembled Field Test Kit—Suitcase No. 1 13
2 Assembled Field Test Kit—Suitcase No. 2 14
TABLES
Number Page
1 Summary of OOC Test Methods 2
2 Recommended and Modified Procedures for the Field Test Kit .... 4
3 Comparison of Three Oil-In-Water Analyzers 8
4 Comparison of the Infrared and Gravimetric Methods 9
5 Solvent Extraction Efficiency For No. 6 Oil 10
6 Field Test Kit Dimensions and Weight 15
7 Physical Properties of Oil and Water ,.,.,. 15
8 Oil-In-Water Results ,,,,,,.,« 16
9 Extraction Efficiency of Freon 113 for Dillon and Shell Oils ... 17
10 Soluble Materials Results ...,,... 18
11 Suspended Solids CSS) Results ,.,,....,,, 19
12 Bacterial Culture Results .... 21
vi
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ACKNOWLEGMENTS
The assistance and counsel of the U.S. Environmental Protection Agency
Project Officer, Mr. L. T. McCarthy, Jr., of the Municipal Environmental
Research Laboratory, Edison, New Jersey, have been invaluable in this work.
The assistance of Mr. Bill H. Lamoreaux, Environmental Engineer, U.S. Environ-
mental Protection Agency, Anchorage, Alaska, in arranging the test kit evalua-
tion sites is also gratefully acknowledged. Helpful discussions with
Dr. Michael J. Wade of Texas Instruments Ecological Services, Dallas, Texas
are appreciated.
VII
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SECTION 1
INTRODUCTION
Offshore drilling facilities are becoming increasingly numerous as new
oil reserves are needed to replace depleted land-based sources. As a result,
the possibilities of drilling and production accidents, such as the Santa
Barbara Channel disaster, are also expected to increase. Another pollution
concern is the presence of brine in the crude oil obtained from deep-well
drilling sites. On offshore platforms, the crude is routinely pass through
an oil/water/gas separator, and the brine is then discharged into the ocean.
After varying degrees of additional treatment this brine contains a fine sus-
pension of oil droplets that is not removed in the separator. Inefficient
brine treatment could results in a serious contamination source.
As one phase of a U.S. Environmental Protection Agency (EPA), contract
with Exxon Research and Engineering, a study was made of pollution control
technology for offshore drilling and production platforms and test methods
were recommended for evaluating the efficiency of the oil-brine separation
process. The Offshore Operators' Committee (OOC) reviewed the Exxon procedures
and recommended several modifications. Additional changes have been proposed
and verified by field evaluation by Texas Instruments Incorporated.
A summary of the OOC test methods is given in Table 1. Specifically,
the work at SRI has consisted of the following tasks:
1. Evaluate the OOC-modified test methods (Table 1, Status 11 for
characterizing oil-brine effluents from offshore oil production
facilities.
2. Recommend and package into a field test kit suitable equipment
and instrumentation for conducting the oil-brine characterizations.
3. Evaluate the field test kit at a suitable onshore or offshore oil
production facilitiy.
4. Deliver the field test kit to EPA with detailed instructions for
performing the tests.
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TABLE 1. SUMMARY OF OOC TEST METHODS
Test
No.
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
;14.
i
i
i
Test
Oil-in-water
Suspended solids
Particle size
Surface tension
Viscosity
Specific gravity
Salinity
PH
Temperature
Brine composition
Bacterial culture
Oil separation
Soluble materials
Flow rate
*
Status 1: OOC modified
Status 2: OOC modified
Status 3: OOC approved
Method /Apparatus
Gravimetric; infrared
Filtration
Microscopy
Method^
Status
1
3
Type of Test
Field !
Lab
1 Field
Tensiometer 3 Field
Ostwald; Brookfield 3 ; Field
Centrifuge; hydrometer I 2 Field ;
Centrifuge; titration 3 Field
pH meter 3 ; Field
Thermometer 3 Field
Atomic absorption 2 Lab
API RP-38 2 Lab :
API 734-53 2 ? ;
Column and Si02 adsorption;
spectrophotometry
Shell PSM
1
2
Field
Field |
I
i
- evaluate at SRI.
- standard procedures.
- standard procedures.
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SECTION 2
CONCLUSIONS
METHODS REVIEW AND DEVELOPMENT
The OOC-recommended test procedures, a brief description of the test as
suggested by the Texas Instruments report , and our recommendations and mo-
difications to these tests are summarized in Table 2.
RECOMMENDED TESTS FOR FIELD TEST KITS
The following tests (Table 2) are included in the field test kit:
(1) Oil in water (IR and gravimetric)
(2) Soluble materials (.equilibration and filtration)
(3) Specific gravity
C4) PH
(5) Temperature
(6) Suspended solids
(.7) Bacterial culture (includes laboratory evaluation of samples
collected in the field)
The following tests are recommended to be performed onshore or in the
laboratory because vibration on the platform interferes severely with the
method.
(.1) Surface tension
(2) Viscosity
Containers for collecting the required samples are included in the test kit.
The following OOC test procedures were not included in the SRI test kit;
(1). IR oil-in-water, using the Horiba and Turner spectrophotometers.
(2) Gravimetric oil-in-water, using balance at test site.
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(31 Particle size
(41 Brine, composition
(5) Flow rate: site specific equipment for each, platform should be
used for these measurements.
(6) Water cut
(7) Boiling range
FIELD RESULTS
The test kit evaluated and assembled at SRI performed satisfactorily at
the two test sites. Only minor modifications to the test procedures, as out-
lined in Section 4, were required. Approximately 8 labor-hours are required
to conduct one on-site oil-brine characterization.
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SECTION 3
RECOMMENDATIONS
During this study, it became apparent that the complete field test kit
is rather bulky (J.32.3 Ib) for one person to transport easily. Therefore, we
recommend that the kit be simplified to focus only on the oil-in-water ana-
lysis. A field test kit for measuring the oil content of the platform efflu-
ent by the infrared method would probably consist of one suitcase (28 Ib),
the Miran spectrometer (21 Ib), and the Freon solvent bottles (40 Ib). The
on-site analysis time required to conduct the single measurements would also
be shortened from about 8 labor-hours (_to conduct all the tests) to about
2 labor-hours.
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SECTION 4
EXPERIMENTAL RESULTS
METHODS REVIEW AND DEVELOPMENT
Total Oil Content
Infrared Method—Three spectroscopic oil-in-water analyzers were compared
for field application: the Horiba, Model OCMA-200; the Wilks Miran, Model
1A-FF; and the Turner Spectronic, Model 350. The results, shown in Table 3,
suggest that the Miran spectrophotometer provides more reproducible results
and is the instrument of choice for the infrared method. It is powered by
120 VAC, can probably be obtained as a battery-powered model, but is not
explosion proof.
The Miran analyzer has definite advantages over the Horiba instrument
and some advantages over the Turner. The Miran's reproducibility, range, and
easily cleaned sample cell are similar to the Turner analyzer; it also gives
similar extinction coefficients for the same oils. The largest difference in
extinction coefficients found on the Miran was 30% between No. 2 fuel oil and
light Arabian crude. The Turner instrument uses visible and near UV light
and requires different wavelengths for No. 2 and No. 6 fuel oils.
The requirement to adjust the wavelength for different oils could cause
errors in the total oil measurements from small variations in the oil composi-
tion during a sampling period. For optimum results, all three instruments
require calibration with an oil that is similar to the oil being sampled. A
critical review of the Horiba recommended that the automatic extractor should
not be used. The Miran performs the same measurement as the Horiba and uses
the extraction procedure recommended in the review.
Gravimetric Method—Table 4 compares the infrared and gravimetric methods
for analysis of oil in seawater. For the comparison, we chose to use No. 6
fuel oil because of the unavailability of crude samples with similar properties
to the oil from the Alaskan production sites. It seemed reasonable that
methods developed with No. 6 fuel oil should be applicable to crude oil
samples. For a sample of Freon 113 containing a known weight of No. 6 fuel
oil, the gravimetric method, which involved evaporation of the Freon and
weighing the residuals, gives 95% recovery of the oil. These results suggest
that some volatiles (5%1 are lost during evaporation. In extraction experi-
ments, however, the oil recovery by both the infrared (extraction and measure-r
ment by the Miran) and gravimetric (extraction, evaporation, and weighing),
methods is significantly lower, presumably because of the poor extraction
efficiency of Freon 113.
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TABLE 3. COMPARISON OF THREE OIL-IN-WATER ANALYZERS
— — ^_I^TRUMENT
FEATURE " ~~ ' -— _
Weight (kg)
Wavelength (nm)
Solvent
ppm oil measured
directly on scale
A
Oil analysis Cppm) 1.
2.
3.
4.
5.
6.
Average deviation
Horiba
8.9
3400-3500
CC1, or Freon
0-100
592 ± 12
640 ± 12
656 ± 10
490 ± 40
562 ± 10
516 ± 10
+ 16
Mir an
6.5
3400-3500
CC14 or Freon
0-3500
588 ± 5
552 ± 6
648 ± 6
536 ± 0
488 ± 0
576 ± 10
+ 5
Turner
7.4
620 for No. 6 oil
340 for No. 2 oil
CHC13
0-4000
656 ± 16
676 ± 5
664 ± 0
582 ± 2
478 ± 2
526 ± 14
+ 7
Oil-in-water samples from six different EPA dispersant effectiveness
tests^ were analyzed on all three instruments. Each test was dupli-
cated, and the average and the deviation are reported.
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TABLE 4. COMPARISON OF THE INFRARED AND GRAVIMETRIC METHODS
Infrared Method
No. 6 Oil
Added
(mg)
-
A
41
32
38
Average
Std. Dev.
% Std. Dev
No. 6 Oil
Recovered
(mg)
Recovery
(%)
i
34 82
27 85
31 : 80
82
-
-
3
4
Gravimetric Method
No. 6 Oil
Added
(mg)
No. 6 Oil
Recovered
(mg)
42+ 40
Recovery
(%)
95
4
* ;
41 36
32 25
38
-
-
26
-
-
- 1
87
78
68
78
10
13
Oil extracted from 500 ml seawater with Freon 113 + 3 ml 12M HC1.
Oil dissolved directly in Freon 113.
-------
TABLE 5. SOLVENT EXTRACTION EFFICIENCY FOR. No. 6 OIL
* Oil
Extractant Added (mg)
CC14 57
53
62
56
j
Average \ -
Std. Dev.
% Std. Dev.
Freon 113 j 43
34
44
Average • -
Std. Dev. ;
% Std. Dev. |
Freon 113 * 41
32
38
Average -
Std. Dev.
% Std. Dev.
i
Oil
Recovered (mg)
54
52
59
54
-
-
-
31
29
25
-
-
34
27
31
-
-
-
Percent
Recovery
95
98
95
96 i
96 j
1
1
72
85
57
71
14
20
83
84
82
83
1
1
Oil extracted from 500 ml seawater.
ml 6M..HC1
10
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Solvent Extraction Efficiency
As shown in Table 5, CC1, is more efficient than Freon 113 in dissolving
No. 6 fuel oil suspended in seawater. With Freon 113, small black flakes of
residual material remain undissolved.
We also observed that the purity of the Freon used in the extraction
process affects, the oil analysis results. The ahsorhance- background for
Freon TF (an impure grade of Freon 113) was considerably greater than spectral
grade Freon 113; a nonlinear calibration curve for No. 6 fuel oil was observed
with the impure solvent. Since the nonlinear calibration is less sensitive
to small differences in oil content, we suggest that more accurate results
can be obtained using the higher priced Freon 113.
Soluble Oil
There has been some concern that a water-soluble fraction of the oil
might cause an inaccuracy in the oil measurement since the composition and,
therefore, the extinction coefficients of dispersed and dissolved oils are
expected to be different. A sample of No. 6 fuel oil was shaken vigorously
for four days in the presence of 400 ml of synthetic seawater. The aqueous
phase was centrifuged to bring any dispersed oil to the surface, and the re-
sultant film of oil was skimmed off the water surface. Microscopic analysis
of the water showed that no oil droplets remained. A sample of the aqueous
phase was extracted with CC14 and analyzed for oil content with the Miran
lA-FF. The results showed that only 3 ppm soluble oil was present. This
suggests that the major fractions measured by the oil-in-water analyses are
dispersed oil, not dissolved oil.
In a similar test, little change was observed in the apparent oil content
of a standard No. 6 oil sample in CC14 before and after treatment with Si02
gel. Since a similar low level of soluble oil is expected with a crude oil,
the OOC-recommended silica gel adsorption task is not necessary.
Particle Size
Particle size distribution of dispersed oil was measured using a photo-
graphic method. A sample of oil dispersed in water was placed on a capillary
slide. At least three representative areas in the sample were photographed
within 15 minutes at a magnification great enough to distinguish the sizes of
the smaller particles. Statistical analysis requires more than 100 particles
to be counted from each sample; when fewer particles are present, more photo-
graphs should be taken.
To calibrate the photographs of the oil droplets, we placed a transpa-
rent reticule on the photographs for size determination. The reticule had
been calibrated on a picture of a stage micrometer taken at the same magnifi-
cation as the oil droplets. A log normal distribution best described the
data, allowing the median to be found graphically. Using this technique, we
11
-------
found that the median particle diameter decreased 10% in one hour, probably
because the larger particles rise to the surface of the capillary slide and
out of focus of the camera. This introduces an uncertainty in the measurement.
The simple and portable method we have developed can best be used to document
the presence of droplets, but is probably not useful for measuring the abso-
lute size distribution.
FIELD RESULTS
The assembled suitcase portion of the field test kit is shown in Figures
1 and 2. The approximate weight and volume of the entire kit is given in
Table 6. The tests, conducted on July 7, 1980, at the Dillon offshore Produc-
tion Platform, Kenai, Alaska, and on July 8, 1980, at the Shell MGS Joint
Onshore Facility, Kenai, Alaska, are outlined in Table 2. Water samples were
withdrawn for analysis from the final production water stream before discharge
into the ocean. Field results were generally replicated three times during
the 8-hour testing period. A complete listing of the instruments and materials
provided in the field test kit is given in Appendix A. The experimental pro-
cedures for each test are given in Appendix B.
Oil-in-Water Results
Table 8 summarizes the total oil content of the Dillon and Shell produc-
tion water effluents using the infrared and gravimetric methods. The results
have been corrected for the extraction efficiency of Freon 113 for the
Dillon and Shell oils in seawater (Table 9). As shown in Table 8, the oil
concentration (ppm, w/w) measured by the infrared method for the Dillon pro-
duction water is higher than that for the Shell water (47.9 versus 38.2 ppm).
The gravimetric results for both samples are appreciably lower than the in-
frared data, suggesting that oil is lost during the solvent evaporation pro-
cedure (Appendix A). Similar low results for the gravimetric method for
No. 6 oil have been previously noted (Table 4).
Soluble Materials
Table 10 gives the results for soluble materials. The field method
gives comparable results using the infrared and gravimetric techniques, des-
pite a large statistical spread. The laboratory results are somewhat lower,
suggesting a loss of material during transportation of the samples to SRI.
Suspended Solids
Suspended solids results are shown in Table 11. For an unexplained
reason, the total suspended solids results for the Shell samples are in
better agreement than those for the Dillon samples. Other suspended solids
results shown in Table 11 are perhaps 10% low because of a filtration problem.
Since the original procedure did not call for adequate drying of the filter
paper following solvent rinsing, the wet paper adhered to the holder and a
small portion was lost for weighing. This difficulty has been corrected in
the revised procedure given in Appendix B.
12
-------
(a) TOP
(b) BOTTOM
FIGURE 1 ASSEMBLED FIELD TEST KIT — SUITCASE NO. 1
13
-------
TABLE 6. FIELD TEST KIT DIMENSIONS AND WEIGHT
Item
Suitcase no. 1
Suitcase no. 2
Miran spectrometer
and container
Freon 113 sample bottles
and container
Bacterial culture
bottles and container
Two gallons Freon 113
and container
Total Weight
Dimensions
(.cm)
70 x 50 x 21
70 x 50 x 21
29 x 28 x 24
36 x 25 x 29
25 x 18 x 12
40 x 25 x 40
Weight
(kg)
12.6
11.0
9.5
7.4
1.4
18.1
60.0 (132.3 Ib)
Physical Properties of Oil and Water
The physical properties (temperature, pH, salinity, density, and viscos-
ity) of the water and oil samples taken at the Dillon and Shell sites are
given in Table 7.
TABLE 7. PHYSICAL PROPERTIES OF OIL AND WATER
^v Test
Site ^v
Dillon
Shell
Production Water
Tern. (°C)
48
34
PH
7.45
8.03
c o / *
b /OO
30.6
25.7
Density
(g/cc, 20°C)
Water Oil
1.015
1.012
0.8605
0.8430
Viscosity
Ccp, 20°C)
Oil
9.3
6.5
Salinity calculated from Standard Methods for the Examination of Water
and Wastewater. 14th edition, M. C. Rand, A. E. Greenberg, and M. J.
Taras, editors, American Public Health Assoc., Washington, D.C., 1976.
15
-------
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TABLE 10. SOLUBLE MATERIALS RESULTS
^\. Method
Sample ^^>^
Dillon No. 1
No. 2
No. 3
Average
Std. Dev.
% Std. Dev.
Shell No. 1
No. 2
No. 3
Average
Std. Dev.
% Std. Dev.
Infrared
mg/£ (ppm)
Field
21.0
23.8
16.4
20.4
3.7
18.1
17.2
13.2
12.8
14.4
2.4
16.7
Lab
9.0
7.5
-
8.3
1.1
13.3
5.3
13.0
17.8
12.0
6.3
52.5
Gravimetric
mg/2, (ppm)
Field
11.6
35.2
11.2
19.3
13.7
71.0
18.6
11.0
10.6
13.4
4.5
33.6
18
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Bacterial Culture
Table 12 gives the bacterial culture test results, expressed in terms of
the sulfate-reducing bacteria count. Because of a delay in the air shipment
of the samples to SR.I, incubation was not initiated wi.thin the recommended
24-hour period. As a result, some of the samples arrived at the laboratory
indicating an initial positive test. Subcultures were taken of the positive
samples and incubated for 1 week at 49°C. Samples, regardless of their
condition upon arrival, were also incubated for the prescribed 5-week period
at 49°C. The results, however, may not accurately represent the actual mi-
crobial content of the production water at the time of sampling, since testing
procedures were not initiated within 24 hours.
20
-------
TABLE 12. BACTERIAL CULTURE RESULTS
Sample
Dillon No.l
Bacteria/ml
Shell No. 1
Bacteria/ml
Shell No. 1
Bacteria/ml
Shell No. 3
Bacteria/ml
Dilution
10
102
io3
io4
IO5
IO6
10
2
10
IO3
IO4
IO5
io6
10
io2
io3
10
io2
IO3
io4
Original Condition
on Arrival
+
_
_
—
_
-
+
-
_
_
_
-
+
+
+
+
+
_
_
After Incubation
5 Weeks at 49 °C
+
+
_
_
_
—
IO2 - IO3
+
+
_
_
^
—
2 1
10 - 10J
+
+
+
ca. IO3
+
+
_
_
IO2 - IO3
*
Subculture
+
+
+
+
+
+
+
Subcultures were made of any culture that arrived at the lab already
indicating a positive result. These subcultures were made after the
original culture was incubated for 1 week at 49°C.
+ Positive test, sulfate-reducing bacteria present.
- Negative test, no bacteria present.
21
-------
REFERENCES
1. "Study of Pollution Control Technology for Offshore Oil Drilling and
Production Platforms," Exxon Research and Engineering, Linden, New
Jersey, EPA Contract No. 68-03-2337 (February 1977).
2. Offshore Operators' Committee Comments on: "Study of Pollution Control
Technology for Offshore Oil Drilling and Production Platforms," EPA
Contract No. 68-03-2337 (June 1977).
3. "Field Verification of Pollution Control Rationale for Offshore Oil and
Gas Production Platforms," Texas Instruments, Inc., Ecological Services,
Dallas, Texas, EPA Contract No. 7-3-002-8 (May 30, 1979).
4. T. S. Yu and W. H. Coleman, "Evaluation of the Horiba Model OCMA-200 Oil
Content Analyzer," David W. Taylor Naval Ship Research and Development
Center, Report MAT-77-63 (November 1977)
5. L. T. McCarthy, I. Wilder, and J. S. Dorrler, "Standard EPA Dispersant
Effectiveness and Toxicity Tests," EPA-R2-73-201, May 1973.
22
-------
APPENDIX A
INSTRUMENTATION AND MATERIALS PROVIDED IN THE FIELD TEST KIT
2 Separatory funnels, 1 liter, Teflon
4 Erlemneyer flasks, 125 ml, glass
4 Volumetric flasks, 100 ml, glass
2 Funnels, small, glass
1 Repipet, 10 ml
1 Ring stand, metal
2 Rings, metal
1 Miran spectrophotometer, oil analyzer
1 Graduated cylinder, 1000 ml, plastic
1 Graduated cylinder, 500 ml, plastic
1 Graduated cylinder, 100 ml, plastic
1 Box disposable pipets, glass
1 Package disposable pipet bulbs
1 Buchner funnel
2 Buchner support rings (.Filter-vac)
2 Hand vacuum pumps
1 Box filter paper, 7 cm, Whatman No.l
1 Filter flask
12 Glass filters in holders
1 Forceps
1 Wash bottle for distilled water, 500 ml
2 Liters distilled water
1 Portable pH meter
2 pH electrodes
3 Buffer solutions, pH 4, 7, and 10
2 Beakers, 100 ml, polyethylene
23
-------
2 Beakers, 500 ml, polyethylene
1 Mercury thermometer, -20 to +100°C
1 Dial thermometer, 0 to 100°C
25 Disposable sterile syringes, 1 cc
1 Insulated sample box
24 Sample bottles for bacterial culture medium, 10 ml
1 Hydrometer set
6 Square glass bottles, 250 ml
24 Glass bottles with Teflon-lined caps, 2 oz
1 Pair gloves, neoprene
1 Box large Kimwipes
1 Box small Kimwipes
100-g Alconox cleaner
500-ml Hand cleaner
1 Sponge
1 Pack Kimtowels
2 Bottle brushes
1 Roll electrical tape
1 Box labels
24
-------
APPENDIX B
LABORATORY AND FIELD PROCEDURES
OIL-IN-WATER
Field Equipment
Graduated cylinders,500 ml, 100 ml
Separatory funnel, 1 liter
Freon 113
Ring stand
Erlenmeyer flask, 250 ml
Volumetric flask, 100 ml
Miran spectrophotometer
Sample bottle with Teflon-lined cap
Disposable pipets
Field Procedure
(1) Purge sample port. Fill 500-ml graduated cylinder from sample port.
(2) Transfer sample directly to a 1-liter Teflon separatory funnel,
rinse, graduate with 25 ml of Freon 113. Add Freon rinse to
separatory funnel along with the sample.
(3) Swirl separatory funnel about 5 times and invert 10 times to extract
the oil from the brine. Place separatory funnel upright in the
ring stand and allow layers to separate completely.
(4) Drain lower Freon layer into a 250-ml Erlenmeyer flask, being
careful not to include any brine. Repeat extraction two more times
with 25-ml aliquots of Freon.
(5) Transfer solvent sample from Erlenmeyer to a 100-ml volumetric
flask. Rinse the Erlenmeyer with more Freon and add it to the
volumetric flask; then add enough Freon to fill the flask to the
mark.
(6) Zero spectrophotometer using Freon from the same batch used for
the extraction of the oil. Place the cell in the Iliran spectro-
photometer and zero the reading at all sensitivities. Zeroing
should be done every time the spectrophotometer is turned on
and once every few hours, if used continuously.
(7) Use a disposable pipet to transfer the Freon extract to a spectral
cell and place the cell in the Miran. Adjust the range to obtain
the highest reading without going off scale. Record this meter
reading and the setting of the spectrophotometer.
25
-------
(8) Save sample for lab analysis. Rinse a sample bottle with Freon.
Transfer the sample in the cuvette and the volumetric flask into
the sample bottle. Rinse both the cuvette and volumetric with
additional Freon and add to sample.
(9) Seal the bottle and label it with the sample no., where and when
the sample was taken, and who performed the analysis.
Laboratory Procedure (1R Method)
(1) To calibrate the spectrophotometer, obtain a sample of the crude
oil produced on the platform of interest. Draw 200-yl of crude oil
into a syringe and weigh it on an analytical balance to the
nearest 0.001 g; record the weight. Empty the contents of the
syringe into a 500-ml volumetric and reweigh the empty syringe.
Record this weight below the previous weight and subtract to obtain
the actual weight of the oil. Fill the volumetric to the mark with
Freon 113. Pipet 10-, 25-, 50-, and 75-ml aliquots into four 100-
ml volumetrics and bring them to the mark with Freon.
(2) Measure the absorbance of each of the solutions by the same method
cited in the field procedure. Plot these data to determine the
curve for oil concentration (mg/cc) versus absorbance.
Correction Factor for Extraction Efficiency
(1) Prepare 2 liters of synthetic brine of the same salinity and pH
reported on the platform by dissolving NaCl in distilled water
(see specific gravity and pH sections). Adjust pH with NaOH or
HC1.
(2) Place 500 ml of brine into four separatory funnels; then use the
same procedure used in the spectrophotometer calibration section
to weigh a known amount of oil. This amount should be the
average amount of oil that was found on the platform. Record
the absorbance, setting, and the weight of the oil added to each
separatory funnel for calculation. Extract with Freon as described
in the field procedure.
Laboratory Procedure (Gravimetric Method)
(1) Pour a Freon sample into a tared 250-ml Erlenmeyer flask. Rinse
the sample bottle with 10 ml of Freon and add this to the flask.
Peel off the label and tape it into the lab book.
(2) Place the flask in a thermostated water bath at 50°C and allow
almost all of the Freon to evaporate. Remove the flask from the
bath and run clean N« gas over the surface at room temperature
until no more Freon is visible. Place in a vacuum desiccator
overnight to remove any water present. Weigh the flask with the
residue and record the weight.
26
-------
Calculations
(1) Oil-ln-Water (IR Method)
( la \ mg oil in Freon x ml Freon sample
original brine sample volume (£)
(2) Oil-in-Water (Gravimetric Method)
, ,.-. _ mg oil residue
original brine sample volume (£)
(3) Extraction Efficiency
„ _.., ^ mg/cc oil in Freon x ml Freon sample , _n
% Oil Recovery = —=" rq , , , -— x 100
mg oil added
SOLUBLE MATERIALS [(FILTRATION AND EQUILIBRATION)]
Field Equipment
Buchner funnel
Filter papers, 7 cm
vacuum filtration apparatus
Graduated cylinder, 1 liter
Separatory funnel, 1 liter
Freon 113
Ring stand
Erlenmeyer flask, 250 ml
Volumetric flask, 100 ml
Miran spectrophotometer
Sample bottles with Teflon-lined caps
Field Procedure
(1) Assemble vacuum filtration apparatus. Place filter paper in a
Buchner funnel and wet it with distilled water.
(2) Purge sample port. Fill 1-liter graduated cylinder with brine
sample.
(3) Fill Buchner funnel with brine; filter and discard filtrate.
Filter 500 ml of sample. Extract this filtrate sample with
Freon 113 as described in the oil-in-water field procedure
and measure the absorbance accordingly.
(4) Transfer sample to Teflon-capped bottle. Label with sample number,
date, location, time, volume, and person who performed test. Then
transport samples to the lab for gravimetric analysis.
27
-------
Laboratory Procedure
(1) Place 400 ml of synthetic brine (use the same salinity and pH
described in the lab procedure of the oil-in-water test) in a
500-ml stoppered Erlenmeyer flask.
(2) Syringe 5 ml of the crude oil from the platform of interest
into each of the brine solutions. Shake the flasks vigorously
for 4 days.
(3) Transfer to a separatory funnel and drain the aqueous phase into
centrifuge tubes. Set up a vacuum trap with a disposable pipet
at the end and siphon off any oil film present. Centrifuge this
solution at 3.8 x 10-^ g for 1 hr.
(4) Remove the oil film again. Measure 200 ml of the brine in a
volumetric and transfer it to a separatory funnel. Rinse the
volumetric flask with Freon and add to separatory funnel.
Extract the sample with three 10-ml aliquots of Freon and fill
to the mark of a 50-ml volumetric flask. Measure and record the
absorbance from the spectrophotometer.
Calculations
(1) Soluble materials (IR field method)
.. /n, mg/cc oil in Freon x sample volume
ppm (mg/A) = -^ - — - n - . - % - -
original brine sample volume (.£)
(2) Soluble materials (Lab Method)
, ,., mg/cc oil in Freon x sample volume
ppm (mg/£) = — ^ - : — : - =— T — : - — «- - = - 7T\
original brine sample volume (£)
TEMPERATURE AND pH
Field Equipment
pH meter
Buffer solutions (pH 4, 7, 10)
Dial thermometer
Mercury thermometer
Graduated cylinder, 1 liter
Field Procedure
(1) Calibrate the pH meter immediately before each use. Immerse
the combination electrode into pH 7 buffer. Adjust temperature
knob to the temperature of the sample. Adjust the calibration
knob to pH 7 reading. Remove electrode, rinse with deionized
water, and wipe clean. See operator's manual for additional
28
-------
information regarding pH meter.
(2) Calibrate the dial thermometer against a mercury thermometer once
a day. Record any difference in the readings.
(3) Purge sample port. Collect 1 liter of sample in a graduated
cylinder and immediately insert the dial thermometer. Wait 1
min until the thermometer has equilibrated and read the temperature.
NOTE - If the sample site has a temperature well, place the
thermometer directly into the port, wait 1 min, and read the
temperature.
(4) Immerse combination electrode in sample and agitate gently for 30
sec. Read pH after steady state has been achieved. Remove
electrode, rinse with deionized or clean tap water, and wipe clean.
If the pH is > 10, calibrate using the pH 10 buffer.
SPECIFIC GRAVITY (OIL AND WATER), SALINITY
Field Equipment
Graduated Cylinder, 1 liter
Thermometer, mercury, -20 to +100°C
Hydrometer Set
3 Square sample bottles, 250 ml
2 polyethylene bottles, 1 liter
Field Procedure
(1) Fill square sample bottles with crude oil to be used in laboratory
analysis. Also, fill polyethylene bottles with production water
for laboratory determination of salinity. Label and seal all
samples for transport.
(2) Purge sample port. Fill a 1-liter graduated cylinder from sample
port without splashing, to avoid the formation of air bubbles.
(3) Insert a thermometer into the sample and allow time for equilibra-
tion. Record the temperature after gently stirring the sample
with the thermometer.
(4) Lower the hydrometer into the sample. Take care to avoid wetting
the stem above the level to which it will be immersed in the
liquid. Depress the hydrometer about two scale divisions into
the liquid, and with a slight spin, release it. When the hydro-
meter has come to rest, floating freely away from the walls of
the cylinder, estimate the scale reading to the nearest 0.0001 sp.gr.
(5) Immediately after observing the hydrometer scale value, stir the
sample with the thermometer and record the temperature. Should
this temperature differ from the previous reading by more than
0.5 °C, repeat the measurement until the temperature is stable
within 0.5°C.
(6) With an opaque liquid, take a reading by observing, with the eye
slightly above the plane of the surface of the liquid, the point
on the hydrometer scale to which the sample rises. Correct this
29
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reading based on the meniscus calibration for the particular
hydrometer being used.
Laboratory Procedure
(1) Follow the field procedure for measuring specific gravity, and
determine the density of the production water obtained in the
field.
(2) Convert findings to salinity (°/oo) from the tables included in
No. 209B "Hydrometrie Method for Salinity Determination," in
Standard Methods for the Examination of Water and Wastewater,
14th Edition (American Public Health Association, Washington,
D.C., 1976).
VISCOSITY
Laboratory Equipment
Brookfield Model LVF Spindle Viscometer
U.S. Bureau of Standards calibrated oils for viscosity testing
Beaker, 600 ml
Thermometer, 0 to 11Q°C
Oil Sample from platform of interest
Laboratory Procedure
(1) Follow the operating instructions for the viscometer.
(2) Calibrate the viscometer with a certified standard having
a specific gravity close to that of the oil in question.
(3) The temperature of the test oil should be controlled to
within ± 0.02°C.
(4) Report results in units of centipoise (cps).
SUSPENDED SOLIDS
Field Equipment
Preweighed glass fiber filters/holders
Vacuum filtration apparatus
Forceps
Distilled water
Graduated cylinder, 1 liter
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Field Preparation
(1) Desiccate filters overnight before field expedition.
(2) Weigh filters, using an analytical balance, and then place each
filter in a holder. Label the holders numerically, recording
the weight of each respective filter.
Field Procedure
(1) Purge sample port and fill a 1-liter graduated cylinder with brine.
(2) Assemble the vacuum filtration apparatus. Place a previously
weighed glass filter in a Buchner funnel with forceps and wet it
with distilled water.
(3) Apply a vacuum and filter the brine until the paper begins to clog.
If there are few solids present, use the full liter. Record the
volume of brine filtered.
(4) Rinse the filter with 100 ml of distilled water; then draw air
through to partially dry it. Replace filter in its holder with
forceps; close the lid.
(5) Record the date on the holder and the conditions under which the
sample was taken. At the end of the sampling period, all the
filter holders should be firmly taped together so that they do
not open during transport back to the lab.
Laboratory Procedure
(1) Remove the tops of the filter holders and dry the filters in a
vacuum desiccator overnight; then weigh the filter and record
the weight (A).
(2) Assemble the vacuum filtration apparatus. Place the filter in
the buchner funnel right side up, and wash with three 25-ml
aliquots of CHC1 . Dry the filters with air; then return to
the desiccator overnight. IMPORTANT - Do not place filters
into the plastic holders to desiccate because the CHC1_ will
cause the filter to adhere to the holder. Remove the following
day, reweigh, and record the weight (B).
(3) Wash the filter with 100 ml 6N HC1 and vacuum dry. Desiccate
the filter overnight. Weigh the filter for a final time and
record this weight (C).
Calculations
Using the original weight of the filter as T, calculate the following:
Total suspended solids = A - T
Organic suspended solids = A - B
Acid-soluble suspended solids = B - C
Fixed suspended solids = C - T
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Convert findings to parts per million (mg/£):
„ /„„/,) \ - weight (mg)
ppm (mg/£) - total volume filtered (A)
BACTERIAL CULTURE: SULFATE-REDUCING BACTERIA
Field Equipment
Serum bottles containing culture medium, 10 ml
Disposable, presterilized syringes, 1 ml
Sterile sample bottle
Insulated sample box.
Field Preparation
(1) Before expedition, prepare the following medium by dissolving
the ingredients with gentle heating. Adjust the pH to 7.3
with NaOH. If excessive precipitation occurs, the medium
should be discarded.
Sodium lactate, USP, 4.0 ml
Yeast extract 1.0 g
Ascorbic acid 0.1 g
MgSO,«7H20 0.2 g
K HPO, (anhydrous) 0.01 g
Fe(S07)9(NH,) •6H90 0.2 g
NaCl 10.0 g
Distilled water 1,000.0 ml
(2) Add reduced iron powder, reagent grade, to the serum bottle and
fill with 9 ml of hot broth. Flush the bottles with N« gas.
Use butyl-type rubber to stopper them; then cap with disposable
metallic covers. Sterilize the bottles and contents at 15 psi
steam pressure for 15 min.
Field Procedure
(1) Purge sample port.
(2) Use sterile bottle to collect sample. Record time, date, tempera-
ture, and water appearance at this time.
(3) All work should be done in duplicate. Using a sterile, disposable
syringe, transfer 1 ml of sample to a serum bottle containing the
culture medium. Agitate the bottle to mix the inoculum; then
using a new syringe, aseptically transfer 1 ml from this bottle
to a second one and mix as before. Continue this serial transfer
until a dilution of 1 to 1,000,000 is reached (6 bottles).
(4) Place the inoculated bottles in the insulated sample box for
transport to the laboratory. Note any bottles that turn black
within 2 hours. These should not be considered positive since
this probably is due to the presence of sulfide ion in the sample
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Subcultures of these false positive samples may be made after
1 week.
Laboratory Procedure
(1) Incubate all bottles at the temperature of the water at the time
of sampling, ±5°C, for a minimum of 4 weeks.
(2) Examine the bottles on the third day and at the end of each week
for the appearance of sulfate-reducing bacteria, indicated by
intense black color. After 1 week, make any necessary subcultures
(See Field Procedure, Step 4).
Calculations
(1) Report the data as the highest dilution indicating growth, as
compared with the lowest dilution showing no growth. The data
are reported as a range in numbers (i.e., 100-1,000 sulfate-
reducing bacteria per ml).
(2) The maximuum time between sampling and examination should not
exceed 24 hr. If an examination cannot be initiated within this
period, include the following statement in the report: "These
results do not necessarily represent the actual microbial content
of the water at the time of sampling."
Reference
American Petroleum Institute, API Recommended Practice for Biological Analysis
of Subsurface Injection Water (American Petroleum Institute, Dallas, Texas,
1975), p. 7.
U..U
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