URTeC: 2883168

Advanced Characterization and Novel Waste Management for Drill

Cuttings from Marcellus Shale Energy Development
Mengling Stuckman*,1,2, Harry M. Edenborn1, Christina Lopano1, and J. Alexandra
Hakala1; 1. Research and Innovation Center, U.S.DOE - National Energy Technology
Lab, 2. AECOM.
Copyright 2018, Unconventional Resources Technology Conference (URTeC) DOI 10.15530/urtec-2018-2883168

This paper was prepared for presentation at the Unconventional Resources Technology Conference held in Houston, Texas, USA, 23-25 July 2018.

The URTeC Technical Program Committee accepted this presentation on the basis of information contained in an abstract submitted by the author(s). The contents of this paper
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is prohibited.

Abstract

Millions of tons of drill cuttings generated from Marcellus shale gas development are currently disposed of in
landfills, buried in-situ, or reused as road fill. This study conducted advanced solids characterization and leaching
tests to allow consideration of more diverse disposal environments. Drill cutting samples with different
mineralogical traits (e.g., high in pyrite and carbon, or high in calcite) from the lateral portion of Marcellus shale
well in WV were studied. Solid characterization (e.g., elemental distribution and mineral composition) and
geochemical leaching experiments (e.g., rainfall vs. landfill, wet vs. dry conditions) were conducted to evaluate trace
metal mobility under different disposal scenarios. The effects of added drill cuttings on soil quality, plant
germination and long-term plant growth were determined in the laboratory and on a building green roof. Results
showed that although drill cuttings passed the regulatory short-term leaching tests for landfill disposal, long-term
release of Ba in all samples and release of As, Ni, and Sb in high pyrite and low calcite samples were of
environmental concern under simulated rainfall conditions. Selected trace metal release (e.g., Ba, V, Mo, Sr and Sb)
increased 2-10 times when waste was first air-dried and subsequently underwent simulated rainfall leaching.
Residual salt content in drill cuttings inhibited plant seed germination, but plant growth on green roofs in cuttings-
amended soil was not inhibited once soluble salts were leached by rainfall. Our characterization better informs waste
managers of the different geochemical factors that control trace metal release from drill cuttings and improves the
ability to assess proposed methods of solid waste characterization and handling. Novel commercial uses, such as the
addition of drill cuttings to green roof soils to offset costs, can be considered if the long-term safety of the material
can be demonstrated.

Introduction

Unconventional Marcellus shale gas development is extensive in the state of Pennsylvania, where 16,078
unconventional wells are permitted and 9,324 unconventional wells were drilled from 2004 to March 31, 2015 [1]. It
has been estimated that over 2000 tons of Marcellus shale drill cuttings are produced from a typical 6000-ft
horizontal well-drilling operation [2, 3]. As a result, millions of tons of drill cuttings generated from Marcellus shale
gas development are currently disposed of in landfills, buried in-situ, or reused as road fill [3]. However, current
waste management practices only focus on application of one regulatory test for waste evaluation, USEPA Method
1321 [4] simulating landfill conditions, and has not explored the potential for land application. These drill cuttings
consist of residual drilling mud containing high barite (BaSO4) and fine-grained black shale rock cuttings, rich in
organic matter and pyrite [5]. Secondary release of trace metals or barium from drill cuttings may be of
environmental concern under different disposal scenarios.

Successful supplementation of existing green roof substrates with waste energy-related materials, such as Marcellus
shale drill cuttings, would provide alternatives to disposal and save construction cost [6]. A well-constructed green
URTeC 2883168 2

roof can reduce storm water runoff; lower the temperature of runoff water; reduce urban heat islands; increase
vegetation and wildlife habitat; insulate the roof and lengthen the roof life [7]. This study will characterize the soil
quality characteristics altered by drill cutting amendments, and evaluate and monitor the fate and transport of trace
metals and organics from drill cuttings to soil, roof runoff and green roof plants.

This study aimed to conduct: (1) advanced characterization of drill cuttings, adjacent shale cores and operating
drilling mud to identify the trace metal-mobilizing sources; (2) geochemical leaching experiments to simulate more
diverse disposal environments (e.g., landfill vs. rainfall disposal conditions, and wet vs. dry conditions) and to
investigate geochemical factors (e.g., mineral composition of drill cuttings, and end pH) controlling trace metal
release from Marcellus shale drill cuttings; and (3) to explore potential application of drill cuttings as a supplemental
plant growth medium on building green roofs.

Materials and Method

Drill cutting samples were obtained from the lateral portion of a Marcellus shale well, portions of Marcellus shale
core collected at the same drilling depth, along with the operating drilling mud from a long-term experimental field
site, the Marcellus Shale Energy and Environment Laboratory (MSEEL), in WV. These samples are (1) DM: the
operating drill mud, comprised of barite, n-dodecane, alkenes, tetradecane, n-undecane, and miscellaneous fatty
acids [8], (2) SWA and SWB: core samples collected at 7438 ft and 7440 ft depth from the side wall of a science
well at MSEEL, and (3) 5HA, 5HB, 5HC, and 5HD: drill cuttings with different mineralogical traits (e.g., high
carbon and pyrite, high clay, high calcite, etc.) from the 5H production well, horizontally drilled at a depth of 7438
ft, collected at a distance of 7758, 9358, 10638, and 10958 ft away from the vertical well. SWA and SWB were later
combined in a 1:1 ratio to create an averaged core sample SW for later geochemical leaching experiments.

All samples were oven-dried at 60 °C until the weight was constant and ground to <100 mesh for elemental and
mineral composition analysis. The elemental compositions of different solids were determined by LiBO2 fusion [9]
followed by ICP-OES and ICP-MS (Varian, 730ES), described by USEPA standard method 6010 [10]. A portion of
the finely-ground samples was used for mineral phase analysis by XRD (Panalytical X’Pert Pro) and for carbon and
sulfur content analysis using a CHNS/O elemental analyzer (PerkinElmer 2400 Series). Elemental associations with
different solid factions were further evaluated by Community Bureau of Reference (BCR) sequential extraction [11,
12]. Elemental distributions of air-dried raw drill cuttings were mapped by micro-X-ray fluorescence (µXRF) at
BL10-2, Stanford Synchrotron Light Source, CA.

Different leaching experiments were conducted for all solid samples to simulate diverse disposal scenarios.
Regulatory leaching tests were also performed on both wet samples as received and oven-dry samples to evaluate
elemental leachability under various environmental conditions, including (1) United State Environmental Protection
Agency (USEPA) method 1312: synthetic precipitation leaching procedure (SPLP) [7] (tumbling for 18±2 hr at 40
:1 liquid to solid (L:S) ratio with DI water adjusted to pH 4.2 with 60% sulfuric and 40% nitric acid) to simulate in-
situ disposal scenarios and road fill use exposed to acid rain, and (2) USEPA method 1311: toxicity characteristics
leaching procedure (TCLP) [10] (tumbling for 18±2 hr at 40:1 L:S ratio with 100 mM acetic acid at pH 2.88 ± 0.5)
to simulate landfill leaching conditions. Wet samples as received were leached using USEPA method 1320: multiple
extraction procedure (MEP) [13] (repetitive and continuous leaching from one-time TCLP followed by nine-time
SPLP), was used to simulate leaching of a waste that will undergo repeated precipitation of acid rain in an
improperly designed sanitary landfill. The MEP typically yields the highest concentrations of trace metals that are
likely to leach in a natural environment [13].

Further tests were conducted to evaluate trace metal fate and transport from drill cuttings when they are land-applied
as soil supplements, or when disposed of over a broad range of anticipated environmental conditions. Total trace
metal bio-availability for all solids was evaluated via Kosson et al. [14] method A.1. Ethylenediaminetetraacetic
acid (EDTA) screening test (tumbling for 48 hr at 100:1 L:S ratio with EDTA solution adjusted to pH 7.5). Trace
metal mobility as a function of pH was evaluated via Kosson et al. [14] method A.2. Alkalinity, solubility and
release as a function of pH (tumbling for 24 hr at 10:1 L:S ratio with deionized water (DI) adjusted to final pHs of 3,
5, 7, 9, and 11). The leachate from all tests was decanted from the solid after centrifugation and was filtered (0.45
µm) prior to aqueous phase analysis. Analyses included elemental analysis using ICP-OES/MS after hot-plate
digestion, cations and anions measured by ion chromatography (Thermo Dionex, ICS1500+), conductivity and pH.
URTeC 2883168 3

Buttercrunch lettuce (Lactuca sativa) seed germination studies were performed on selected drill cuttings. Thirty
seeds (Botanical Interests, Broomfield, CO) were added to moistened 50:50 mixtures of test cuttings and green roof
plant growth substrate, which consisted largely of heat-expanded shale. Petri dishes containing seeds and soil
mixtures were incubated in the dark at 23°C for 72 h. Germination rates, as well as shoot and root length, were
recorded.

5% (w/w/) drill cuttings were mixed with ca. 950 g green roof growth substrate in 2.5 L pots and placed on the
Pittsburgh NETL green roof in triplicate. A duplicate set of 3 pots received an additional 13 g Osmocote (14-14-14
N-P-K) long-term-release fertilizer each. Sedum plant cuttings were transplanted to each pot, and growth was
monitored for the next 6 months.

Results and Discussion

Solid Characterization

Table 1 shows basic solid characterization and Figure 1 shows the XRD results and carbon content for all solids. In
summary, we found drilling mud (DM) contained the highest moisture content (49%) and high halite (NaCl) and
barite (BaSO4), displaying distinguishable mineralogical composition compared to Marcellus shale core and drill
cuttings. Marcellus shale and drill cuttings contain minerals very consistent with typical shale assemblages
(predominantly mixed clay (e.g., chlorite, muscovite/ illite), dolomite, quartz, calcite, and trace pyrite) [15].
Elevated Ba content (Table 1) and detectable barite in XRD analysis (Figure 1) were found in four drill cutting
samples 5HA, 5HB, 5HC and 5HD, evidence of drilling mud residuals in these cuttings. Different mineralogical
traits were detected in different drill cuttings: 5HA with high clay and low TOC content; 5HB with highest pyrite
and highest TOC content; 5HC with highest calcite content; and 5HD with lowest calcite content and moderate
TOC. Consequently, trace metal analysis reveals that 5HB, due to its high pyrite and TOC content, contained the
highest As, Cd, Co, Cu, Fe, Mo, Ni, Pb, Sb, U, B and Zn in all collected samples. The Ca (8.8-13.5%), Ba (4.1-
6.2%) and Sr (900-1200ppm) contents in drill cuttings are noticeably higher compared to core samples (SWA, SWB
with 0.9-1.5% Ca, 0.1% Ba and 153-180 ppm Sr), because of Ca variability along the horizontal direction of the
Marcellus shale formation, and the Ba and Sr residuals from the drilling mud retained by drill cuttings.

Table 1. Summary of solid characterization for all tested samples.

Ba Ca Fe
Sample Mineralogical traitsa %Dry solidb Carbon %c Sulfur % c
ppmd ppm ppm
DM High Ba and Na 51.10% 1.6 3.8 122500 45365 10882
SWA 100% 3.2 1.9 1256 9345 39244
SWB 100% 3.2 2.3 1225 15159 43589
5HA High Clay, low TOC, mod calcite 89.30% 5.2 1.4 41065 88782 32190
5HB High pyrite, high TOC 84.80% 13.9 6 62455 49036 43510
5HC high Calcite 88.30% 8.8 1.7 46725 134895 18760
5HD low calcite, mod TOC 83.20% 9.6 4 48595 29804 32440

a: Mineralogical traits from XRD analysis (Figure 1), and carbon content analysis.
b: % dry solids: ratio of weight of oven-dried solids vs. weight of wet solids as received.
c: Carbon % and Sulfur % measured by CHNS/O analyzer.
d: Ba, Ca, Fe content measured by LiBO2 digestion followed by ICP-MS.
URTeC 2883168 4

100%
5 5 11
90%
Gypsum
80%
Chlorite
70% Muscovite/Illite
1.6
60% Dolomite
50% Quartz
49 TOC
40%
Halite
30%
3.5 Calcite
10.3
20% Pyrite
2 1.7 7 17 7
10% 16 10 3 Barite
3.2 3.2
0% 4 5 4 4
DM SWA SWB 5HA 5HB 5HC 5HD
Figure 1: Mineralogical composition from semi-quantitative XRD analysis and total carbon content (TOC) for all samples.

Preliminary µXRF elemental maps revealed that barium (~ 5 wt%) primarily formed coatings on mineral grains
(Figure 2) in drill cuttings and trace metals tended to be associated with pyrite and calcite. For example, Pb, As, and
Se were found to be co-localizing with the Fe and S distribution; whereas U and Cu co-localized with the Ca
distribution (Figure 2).

Preliminary sequential extraction data further showed that Ba was >99% non-extractable via BCR extraction. The
mobile barium (100-400 mg/kg) was mainly associated with exchangeable and carbonate phases, sensitive to acidic
leaching conditions. As, Cu, Co, and Zn were mainly associated with sulfide and organic carbon phases (30-60 %),
consistent with findings from µXRF elemental maps that these elements co-localized in Fe grains (likely pyrite),
whereas Ni, U and Sr were partially associated with exchangeable and carbonate phases (10-20 %), consistent with
findings from µXRF elemental maps that Ni and U co-localized in Ca grains.
 URTeC 2883168 5

Figure 2: µXRF elemental maps for one region of interest in 5HC drill cutting thin section taken at an excitation energy of 18100eV, 100m sec
dwell time and 50 µm beam and step size. Scale bar is 1000 µm. Top panel: tricolored map distribution of Fe (in red), Ca (in blue), and Ba (in
green); Middle panel: arsenic distribution map with color scale from blue, yellow to red to represent XRF intensity from low to high. The Se and
Pb distribution maps are similar to As map; Bottom panel: uranium distribution map, with similar distribution of Cu.

Regulatory Leaching Tests

Results showed that all solids passed TCLP protocol, suggesting that they can be disposed of at a municipal solid
waste landfill, consistent with our previous results with other Marcellus shale drill cuttings [2]. However, selected
elements (e.g., Ba, V, Mo, Sr, Sb) released from the SPLP extraction may be of environmental concern [16], mostly
when the waste is first dried (see red symbols vs. PA limit in Figure 3). The SPLP extraction indicated greater
potential for increased leaching (2-10 times) from dried drill cuttings versus wet drill cuttings, likely due to the
oxidation of pyrite in the shale, evidenced by the increased Fe and sulfate release from dried samples in SPLP tests
(Figure 3). Information from site operators indicate that drill cuttings are oftentimes aired-dried before disposal. The
results obtained through this study may allow improved waste management practices and disposal guidelines for
Marcellus shale drill cuttings.
URTeC 2883168 6

Figure 3: Trace metals released (µg/L) from SPLP tests for all solid samples. PA SPLP limits were adapted from PA Department of Environmental
Protection Statewide Health Standards [16]. Data not plotted in this figure indicated release concentrations below detection limit of ICP-MS.

USEPA1320: Multiple Extraction Procedure (MEP)

Although drill cuttings passed regulatory short-term leaching tests, long-term release of Ba in all samples persists
after multiple extractions (10 times) using the MEP procedure (10X MEP; Figure 4). The long-term release of Ba
agrees with the sequential extraction results that leachable barium (100-400 kg/mg) still exists in these drill cuttings,
mainly associated with exchangeable and carbonate phases, and it is susceptible to leaching under acidic conditions.

The long-term behavior of other trace metals was controlled by the pH buffering capacity of different solids, due to
varied mineralogical composition (e.g. calcite). Figure 4 shows that the final pH was buffered between 7 - 8 during
10X MEP for drill cuttings 5HA, 5HB and 5HC due to their high calcite content. On the other hand, the final pHs
for 5HD, DM, and SW decreased over the course of the extraction procedure. Consequently, oxyanions from drill
cuttings have cumulative release potential (e.g., As, Sb, V and Mo) higher than DM/SW due to their high pH
buffering capacity. The results agree with the fact that oxyanion release is promoted under alkaline conditions [17,
18]. For example, Figure 4 shows highest As release from sample 5HC associated with the highest calcite content.
Figure 4 also shows the limited amount of Pb release from drill cuttings compared to SW and DM, as high pH
environments inhibit Pb mobilization [19]. Additionally, there exist concerns of long-term release of Ni, Cd, Zn and
Cr from 5HD, because the pH gradually decreased from 7 to 4.5 during 10X MEP, increasing the potential for cation
release [20].
URTeC 2883168 7

Figure 4: End pH and Trace metal released (µg/kg) from USEPA 1320: multiple extract procedure (MEP) for all solid samples.

Potential Use of Drill Cuttings as Green Roof Materials

The total bio-availability of trace metals based on the EDTA screening test varied among samples based on different
mineralogical traits. Figure 5 shows that 5HA (with highest clay content) released the most Fe, Cr and Pb; 5HB
(with highest pyrite & TOC) released the most As, Cd, Co, Cu, Mo, Ni, Sb and Zn; and 5HC (with highest calcite)
released the most Ca, Sr, U and V. Ba was significantly extracted by EDTA (20 – 110 mg/L in solution and 5 - 24%
released) due to its chemical affinity to organic chelators, and EDTA has been used as an anti-scaling agent in the oil
and gas industry to prevent barite precipitation [21]. Based on the results of the EDTA test, trace metals estimated to
have potential high bio-availability include Sr (54-70% released from all drill cuttings), U (up to 40% released from
5HC), and Pb (up to 51% released from 5HA).
URTeC 2883168 8

Figure 5: Trace metal released (µg/L) from EDTA extraction for all solid samples.

Preliminary plant growth and green roof studies

Studies using 50% drill cuttings mixed with green roof substrate showed complete inhibition of lettuce seed
germination. As a result, green roof plant growth studies were carried out with only 5% (w/w) mixtures of drill
cuttings and green roof material. Initial rainfall leachate analyses revealed that high concentrations of sodium
chloride were washed from the plant pots, and these concentrations decreased over time. Initial salinity of the drill
cuttings is considered to be the primary inhibitor of seed germination potential. Subsequent plant growth studies
have shown to date that added drill cuttings had no further effect on Sedum growth relative to control pots. The
addition of fertilizer produced massive plant growth in all drill cutting treatments, suggesting that the addition of
nutrients was a more limiting factor than inhibitory substances in the added drill cuttings, and/or that fertilizer
components may neutralize the negative influences of some inhibitory substances. Further research will quantify the
potential uptake of drill cutting constituents into plant roots and shoots.

Conclusions

This study demonstrates that trace metals can be co-localized with pyrite and calcite grains coated with barite
enriched muds in drill cuttings. Consequently, the trace metal behavior was controlled by these mineral components
in different drill cutting samples. For example, samples with high calcite content will have higher pH buffering
capacities that result in limited divalent trace metal release and elevated As and U release, whereas samples
containing limited amounts of calcite will have long-term release concerns in terms of Ni, Cd, Zn and Cr.

Trace metal mobility from drill cuttings is impacted by leaching pre-conditions such as moisture content. To date, all
drill cuttings studied passed regulatory TCLP testing for landfill disposal. However, selected elements (e.g., Ba, V,
Mo, Sr, Sb) may be of greater environmental concern when drill cuttings are disposed of after drying, which results
in 2-10 times greater release of Ba, V, Mo, Sr and Sb, compared to wet drill cuttings.
URTeC 2883168 9

Drill cutting characterization serves to better inform waste managers of the different geochemical factors that control
trace metal release from drill cuttings and improves the ability to assess proposed methods of solid waste
characterization and disposal. Significant environmental benefits may be realized if drill cuttings are kept wet prior
to disposal in landfills, as a low cost option for disposal pretreatment. Novel commercial uses, such as the addition
of drill cuttings to green roof growth substrates to offset costs, can be considered if the long-term safety of the
material continues to be demonstrated.

Acknowledgement

This technical effort was performed in support of the National Energy Technology Laboratory’s ongoing research in
Unconventional Activities under the RES contract DE-FE0004000. Thanks to Tracy Bank at Pittsburgh Analytical
Lab for conducting ICP-MS and CNS analysis, and to Dustin Crandall and Johnathan Moore who helped with core
logging and provided MSEEL background information. The synchrotron work was conducted on beamlines 10-2 at
the Stanford Synchrotron Radiation Lightsource (SSRL), a national user facility operated by Stanford University on
behalf of the Department of Energy, Office of Basic Energy Sciences, through the Structural Molecular Biology
Program, supported by DOE Office of Biological and Environmental Research and the National Institutes of Health.

Disclaimer

This project was funded by the Department of Energy, National Energy Technology Laboratory, an agency of the
United States Government, through a support contract with AECOM. Neither the United States Government nor any
agency thereof, nor any of their employees, nor AECOM, nor any of their employees, makes any warranty,
expressed or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of
any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately
owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark,
manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring
by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not
necessarily state or reflect those of the United States Government or any agency thereof.

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