1. Real Time, Low
Costs Technologies
for Determining
Treated Oil & Gas
Produced Water
Stability
Master of Science Research Project
Allana Robertson
2. Road Map through Oil & Gas Project
I. Introduction
A. Statement of Problem
B. Approach to Solve the Problem
C. Research Objectives
D. Significance of Study
II. Description of Work
A. Research Design
i. Examples of Treatment Systems
B. Operation Strategy and Sampling
Locations Sampling Scheme
C. Instrumentation: Experimental Filtration
Unit Setup
D. Instrumentation: Chemical Analysis
Instrumentation
E. Results & Discussion
F. Findings Related to Objective One:
Microbial Activity Post Continuous
Treatment
G. Findings Related to Objective One:
Reduction of Microbial Electron Donors
and Acceptors
H. Findings Related to Objective One:
Reduction of Microbial Electron Donors
and Acceptors
I. Findings Related to Objective One:
Problems/ Successes
i. Filtration Technology Demonstration
J. Findings Related to Objective Two:
Equipment Failure
K. Findings Related to Objective Two:
Storage in Open and Sealed
Containment
i. Examples of Containment
L. Findings Related to Objective Two:
Problems/ Successes
III. Conclusions
A. Main Issues
B. Lessons Learned
C. Future Outlook
4/19/20162
4. I. A. Statement of Problem
• Oil & Gas production in arid locations is forcing many companies to
consider produced water reuse. Microbial activity has been overlooked
when evaluating produced water quality for reuse. In addition, general
standards do not exist for grading produced waters even after treatment.
• Because of this, the following has been documented:
• Higher incidence of MIC related corrosion
• Larger expenditures on equipment maintenance and replacement
• More frequent equipment malfunctions
4/19/20164
5. I. B. Approach to Solve the Problem
• Evaluate the use of membrane filtration to reduce microbial activity in
treated produced waters. Chemical components related to microbial
growth will be monitored to determine activity potential in treated
produced waters during storage. Results will be adapted to current field
procedures during future A&M field trials.
4/19/20165
6. I. C. Research Objectives
• Determine water stability during continuous treatment
• Microbial activity
• Reduction of microbial electron donors and acceptors
• Reduction of dissolved TIC & TOC
• Total hardness reduction (QC)
• Microbial nutrient levels post treatment
• Determine water stability during suspended treatment
• Short term and Long term equipment failures
• Storage in open and sealed containment
4/19/20166
7. I. D. Significance of Study
• Concluding this study, the
following will be understood from
the experimental work:
Broader understanding of microbial
activity in produced waters.
Better understanding of the need
to treat produced waters prior to
reuse.
Open access to research data for
use in developing treatment
process SOP’s.
Enhanced environmental awareness
4/19/20167
10. II. A. i. Research Design
Examples of Treatment Systems
4/19/2016
NF Treatment System
MF Treatment System
10
11. II. B. Operation Strategy and Sampling Locations
• Pre-treatment:
• Two stage pre-treatment process and stored in the MF feed tank
• Microfiltration (MF):
• Pretreated water pumped into MF system running in concentrate mode
• MF permeate transferred to the NF feed tank in 5 gallon increments
• Nanofiltration (NF):
• MF permeate pumped into NF system running in concentrate
• NF permeate was collected and stored in 5 gallon increments
Ideally tanks would be used to collect all process waters when running a system with
larger flow rates and feed volumes greater than benchtop scale.
4/19/201611
12. II. B. Operation Strategy and Sampling Locations
• Samples were taken from the
following locations:
1 Raw feed
2 Pretreat
3 MF feed
4 MF permeate
5 NF feed
6 NF permeate
• Single samples were taken of
the following:
• Raw feed
• Pretreat
• Replicate samples were taken
of the following:
• MF feed
• MF permeate
• NF feed
• NF permeate
4/19/201612
13. II. B. Operation Strategy and Sampling Locations
Run Number of
Replicates for
MF
Concentrate
Number of
Replicates for
MF Permeate
Number of
Replicates for
NF
Concentrate
Number of
Replicates for
NF Permeate
Failure Trial 3 4 1 1
Trial 1 2 4 2 2
Trial 2 3 3 3 3
4/19/201613
15. II. D. Instrumentation: Chemical Analysis
Instrumentation
Field Technologies
• HACH HQ40d
• HACH 2100P Turbidometer
• Fischer Scientific Accumet AP74 DO
meter
• Bactiquant-WATER Meter
Laboratory Benchtop
• HACH Spectrophotometer DR 5000
• GE InnoVox TOC Analyzer
Commercial Laboratory
• Potassium
• Alkalinity
• Carbonate
• Bicarbonate
• Total phosphorus
• Total dissolved iron
• Sulfate
• Magnesium
• Calcium
• Total hardness
• Chloride
4/19/201615
16. II. D. Instrumentation: Chemical Analysis
Instrumentation
New Microbial Field Technology
• Bactiquant-WATER meter
• Total active biomass
• Mobile, field ready
• Yields results in 10-30 minutes
4/19/201616
17. II. E. Results & Discussion
Treatment of Produced Water
• Continuous Processing Trials
i. Trial 1
ii. Trial 2
• Failure Test
i. Minor and major equipment failures
ii. Storage during failures
4/19/201617
18. II. F. Findings Related to Objective One: Microbial
Activity Post Continuous Treatment
i. Trial 1
ii. Trial 2
a. Reduction of total biomass activity
• Continuous processing yields best results for
reduction of microbial activity
• Linear decline in microbial activity with each
processing step
• MF treatment reduces raw water microbial
populations
• NF treatment reduces microbial populations
from contamination during open air
processing
171.40
3.57
5.44
3.25
174,381.20
22,255.60
68.80
0.15
58,815.00
2,041.30
303.70
0.83
0.1
1
10
100
1000
10000
100000
1000000
MF_Raw_Feed Pretreated MF_Permeate NF_Permeate
BactiquantValue(ml^-1)
Failure Test
Trial 1
Trial 2
4/19/201618
19. II. G. Findings Related to Objective One: Reduction
of Microbial Electron Donors and Acceptors
i. Trial 1
ii. Trial 2
b. Reduction of microbial nutrients
• Metabolic cycling of electron donors
• Total soluble iron exhibited the highest
reduction
18.91
0.01
10.0225
1.925.70
10.05
1.37 0.04
0
10
20
30
40
50
60
70
80
90
100
Species(mg/l)
Trial 1 Total Soluble Iron
Trial 2 Total Soluble Iron
Trial 1 Ammonium, Ammonia,
Nitrite
Trial 2 Ammonium, Ammonia,
Nitrite
4/19/201619
20. II. H. Findings Related to Objective One: Reduction
of Microbial Electron Donors and Acceptors
i. Trial 1
ii. Trial 2
b. Reduction of microbial nutrients
• Metabolic cycling of electron acceptors.
• Improved water quality as a result of
increased DO levels
0.73
0.73
0.7375
0.55
0.31
0.33
0.32
0.20
0.04
3.37
2.33
2.61
0.04
0.04 0.04 0.04
2.07
2.72
5.4625
5.72
0.79
2.97
5.37
0
1
2
3
4
5
6
7
0
50
100
150
200
250
300
Species(mg/l)
Trial 1 Manganese
Trial 2 Manganese
Trial 1 Nitrate
Trial 2 Nitrate
Trial 1 Dissolved Oxygen
Trial 2 Dissolved Oxygen
Trial 1 Sulfate
Trial 2 Sulfate
4/19/201620
21. II. I. Findings Related to Objective One: Problems/
Successes
iii. Problems/Successes
• Problems
• Lack of digital flow meter integration
• Inconsistent replicate numbers
• Successes
• Larger volume of permeate from new NF treatment system
• Data collected during all 3 treatments was consistent
4/19/201621
22. III. I. i. Filtration Technology Demonstration
Raw Produced
Water
MF Permeate
Water
MF Permeate
Water
NF Permeate
Water
5 minutes
after
collection
4/19/201622
23. II. J. Findings Related to Objective Two: Equipment
Failure
i. Minor and Major Equipment
Failures
• Minor equipment failure
• 1 hour downtime
• Total biomass activity
• Major equipment failure
• 4 day downtime
• Total biomass activity
171.40
3.57
5.44
11.83
3.25
1
10
100
1000
Raw Feed Pretreated MF Permeate
Minor Failure
Stored Water
Major Failure
NF Permeate
BactiquantValue(ml-1)
4/19/201623
24. II. K. Findings Related to Objective Two: Storage in
Open and Sealed Containment
ii. Storage During Failure
• Storage in simulated open air
containment
• Elevated total biomass activity levels
• Storage in simulated sealed
containment
• Lower total biomass activity levels
2.77
4.68
20.6
0
5
10
15
20
25
0 4
BactiquantValue(ml-1)
Time (days)
Sealed Water Sample
Open Air Water Sample
4/19/201624
25. II. K. i. Findings Related to Objective Two:
Examples of Containment
Sealed ContainmentOpen Air Containment
4/19/201625
26. II. L. Findings Related to Objective Two: Problems/
Successes
iii. Problems/Successes
• Problems
• Replicate sampling
• NF system limited the volume of NF treated permeate
• MF and NF systems are analog not digital
• Data appears to be collected in a scattered pattern, not consistent
• Select HACH field kit analysis appeared to be inconsistent with commercial laboratory
• Successes
• Data supported steady state assumption
• Data analysis re-directed chemical analysis efforts
• Commercial laboratory results made testing more manageable per trial
• Bactiquant analysis was consistent throughout the trial
• Replicate averaging yielded consistent chemical ion data for data analysis.
4/19/201626
28. IV. A. Main Issues
• Down Market
• Oil & Gas companies must cut production costs to survive.
• Maintenance costs for maturing and matured producing wells are rising
• Environmental Awareness
• Water supplies in arid oil & gas producing locations
• Reuse without treatment and treatment standards
• Oil & Gas currently experiencing pre-regulation phase
4/19/201628
29. IV. B. Lessons Learned
• Treatment of raw produced water prior to use in drilling and completions
is necessary to lower maintenance costs
• Reduced MIC corrosion
• Reduced reservoir plugging
• General treatment guidelines will be needed to guide companies during
treatment assessment and design
• Pretreatment-necessary
• Treatment levels- recommended according to need
• Quality control throughout treatment process- necessary
4/19/201629
30. IV. C. Future Outlook
• 2017 market increase (hopefully)
• Everyone can go back to work!
• Publication of Produced Water
Treatment Guidelines
• Increased produced water reuse
• Reduced MIC
• Reduced scaling
• Ease of tensions between
municipal and Oil & Gas
4/19/201630
32. Special Thanks
to
Committee Members
Dr. Xingmao “Samuel” Ma
Associate Professor
Zachry Department of Civil Engineering
Specialty: Environmental Engineering
Dr. Bill Batchelor
R.P. Gregory ’32 Chair Professor
Zachry Department of Civil Engineering
Specialty: Environmental Engineering
David Burnett
Harold Vance Department of Petroleum Engineering
TEES Associate Research Scientist
Director of Technology GPRI
4/19/201632
33. Special Thanks
to
Technical Support
Petroleum Engineering Staff for helping with
technical logistics
Jennifer Fichter for inviting me attend her
microbial field trial and sharing data
GPRI Staff for helping run filtration equipment and transport
raw produced water.
Mikah Bradford for networking and connecting
me with Jennifer Fichter
Ecolyse microbiologists for help with metagenomic
analysis of raw SWD water. Also without their help, the
amazing results achieved from Jennifer’s field trial would
not have been possible.
Thank you for supporting our research by
providing SWD water at no cost for all
treatment runs.
4/19/201633
35. V. A. Findings Related to Objective One: Reduction
of Dissolved Organic Carbon
i. Trial 1
ii. Trial 2
c. Reduction of total dissolved organic
carbon
• TOC levels increase during the failure
test
• TOC levels decrease during both trial 1
and trial 2.
• Post MF treatment, produced water
contains roughly 84-88% TOC
• Post NF treatment, produced water
contains roughly 45-54% TOC
36.69%
98.75%
126.26%100.00%
86.94%
84.16%
54.19%
104.43%
88.75%
45.84%
0.00%
20.00%
40.00%
60.00%
80.00%
100.00%
120.00%
140.00%
%TotalOrganicCarbon
Failure Test Total Organic
Carbon
Trial 1 Total Organic Carbon
Trial 2 Total Organic Carbon
4/19/201635
36. V. B. Findings Related to Objective One: Reduction
of Dissolved Inorganic Carbon
i. Trial 1
ii. Trial 2
c. Reduction of total dissolved inorganic
carbon
• TIC appears to decline as treatment
progresses for all three trials.
• Post MF treatment, produced water
contains roughly 91-94% TIC
• Post NF treatment, produced water
contains roughly 66-67% TIC
100.00%
12.92%
68.41%
42.92%
102.37%
91.97%
66.18%
92.67%
94.25%
67.56%
0.00%
20.00%
40.00%
60.00%
80.00%
100.00%
120.00%
%TotalInorganicCarbon
Failure Test Inorganic
Carbon
Trial 1 Inorganic Carbon
Trial 2 Inorganic Carbon
4/19/201636
37. V. C. Findings Related to Objective One: Total
Hardness Reduction
i. Trial 1
ii. Trial 2
d. Reduction of total hardness
• Calcium and magnesium appear to
decline linearly with respect to treatment
stages.
• Produced waters exhibit reduced scaling
potential post treatment with NF
technology.
• Total hardness reduction acts as QC for
treatment scheme
29185.71
21648.92
29130.77
22278.24
2045.27 2057.76 2039.45 1503.36
4817.96 4134.39 4857.08 1570.99
0
5000
10000
15000
20000
25000
30000
35000
0
10000
20000
30000
40000
50000
60000
HardnessSpecies-CaCO3(mg/l)
Trial 1 Calcium-CaCO3
Trial 2 Calcium-CaCO3
Trial 1 Magnesium-CaCO3
Trial 2 Magnesium-CaCO3
Trial 1 Total Hardness-
CaCO3
Trial 2 Total Hardness-
CaCO3
4/19/201637
38. V. D. Findings Related to Objective One: Microbial
Nutrient Levels Post Filtration Treatment with MF and
NF Systems
Nanofiltration
Failure Test Trial 1 Trial 2
Carbon: 100.00% 100.00% 100.00%
Nitrogen: 21.27% 146.36% 23.35%
Sulfur: 1.36% 60.56% 3.31%
Phosphorus: 1.61% 20.76% 3.48%
Sulfate: 4.07% 181.30% 9.92%
Iron: 0.02% 3.63% 0.02%
Manganese: 0.09% 1.04% 0.11%
Oxygen: 3.29% 10.80% 3.13%
Microfiltration
Failure Test Trial 1 Trial 2
Carbon: 100.00% 100.00% 100.00%
Nitrogen: NA 85.12% 16.25%
Sulfur: 17.12% 85.93% 4.40%
Phosphorus: 3.30% 14.54% 3.41%
Sulfate: 51.24% 257.28% 13.18%
Iron: 0.10% 12.83% 0.47%
Manganese: 0.45% 0.94% 0.11%
Oxygen: NA 6.99% 1.01%
4/19/201638
