Analysis of Cations in Hydraulic Fracturing Flowback Water from the Marcellus Shale Using Ion Chromatography
This presentation describes the determination of cations in hydraulic fracturing flowback water using ion chromatography. In this work, sodium was most abundant, followed by calcium, strontium, magnesium, potassium, barium, ammonium, and then lithium, respectively. The quantity of scale-forming ions, such as calcium, strontium, and barium, is particularly informative because it can be used to determine the amount of anti-scaling agent in fracturing fluid mix that will maximize hydrocarbon recovery.
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Analysis of Cations in Hydraulic Fracturing Flowback Water from the Marcellus Shale Using Ion Chromatography
1. 1
Analysis of Cations in Hydraulic
Fracturing Flowback Water from the
Marcellus Shale Using Ion
Chromatography
Art Fitchett
Director of NASS Operations and Compliance
Chromatography and Mass Spectrometry
Thermo Fisher Scientific
Bannockburn, IL
The world leader in serving science
2. Environmental Impact of Hydraulic Fracturing
2
• Challenges
• Potential for contamination of water, soil, and air
• Compliance to clean water act and shale gas regulations
• Optimization of fracturing processes
• Solution
• Water quality monitoring
• Anion and cations
• Metals
• Organics
• Radiation
3. 3
Hydraulic Fracturing Workflow
Well 1
Waste
Disposal
Desalination
Well 2
Frack Chemicals
Frack Chemicals Pre-Injection Site
assessment
Recycle
Flowback / Produced
Brines
Deep Well
Injection
Gas Production
Water
Monitoring Well Monitoring Well
Fresh Water
4. 4
Hydraulic Fracturing Workflow Monitoring
Inorganic
Metals
Anions
Organic
Surfactants
Site Monitoring Produced Water
13C-CH4 , 18O 87Sr/86Sr
stable gas IRMS HR-ICP-MS, TIMS, MC-ICP-MS
Cl-, Br-, SO4
-
IC, Discrete Analyzer
Ethoxylated phenols, acrylamide
LC-MS/MS, LC-CAD
Sr, Ba, Ca, Mn, Ar, etc.
Cations IC, AAS, ICP-OES, ICP-MS, HR-ICP-MS
Analytes
Radiation
Water Chemistry
Sediments HF Water
Composition
Frack Design
Flowback and
Wastewater
Natural Gas Methane, BTEX
GC
Gross Alpha, Beta, Gamma, Radium 226, 228
GM, NaI
Isotopes ratios
Organic acids
IC
Brines
TDS, alkalinity, pH, conductivity, DO
multiple
Instrumentation
5. Analytes in Flowback Wastewater Measured by IC
5
• Inorganic anions
• Chloride
• Impacts effectiveness of additives (reuse)
• Disrupts nitrification processes
• Bromide
• Ozonation, chlorination -> disinfection by-products: brominated
trihalomethanes, bromate
Carcinogenic
• Sulfate
• Can disrupt anaerobic digestion processes
• Organic acids
• Formic and acetic acids
• pH balance is important for efficient fracking
10. Obtaining Accurate Data From High Salt Samples
Manual Analysis
• Post-run
• Determine concentration from chromatogram peak area
10
• Exceed limit → dilute → re-run sample
• Pre-run
• Manual conductivity measurement
• Exceed limit → dilute → run sample
• Tedious
• Dilution prone to errors
11. Obtaining Accurate Data From High Salt Samples
Automated Analysis
• “AutoDilution”
• Post-run analysis using ion chromatograph software
• Exceeding peak height or area -> re-run with less sample loaded
• In-line Conductivity
• Conductivity measured prior to loading sample onto column
• Exceeding upper limit -> less sample loaded
Injecting Less Sample
• Smaller sample loop
• Partial loop
• Automated sample dilution
• Lower amount of sample loaded
11
Thermo Scientific™
Dionex™
Chromeleon™
Chromatography Data
System (CDS) Software
18. Conclusion
• Wastewater containing high salt can be challenging to
analyze
18
Automated sample pre-screening and dilution
Accurate and consistent determination of anions,
organic acids, and cations
Formulate wastewater reuse or treatment strategy
19. Technical and Application Notes
• TN 138: Accurate and Precise Automated Dilution and In-line
Conductivity Measurement Using the AS-AP Autosampler
Prior to Analysis by Ion Chromatography
• TN 139: Determination of Anions in Fracking Flowback Water
From the Marcellus Shale Using Automated Dilution and Ion
Chromatography
• AN 1094: Determination of Cations in Hydraulic Fracturing
Flowback Water from the Marcellus Shale
19
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