IN THE MATTER OF THE JOINT REVIEW PANEL ("JOINT PANEL") ESTABLISHED TO REVIEW THE JACKPINE MINE EXPANSION PROJECT

("PROJECT") PROPOSED BY SHELL CANADA LIMITED ("SHELL")

MOTION TO THE JOINT REVIEW PANEL PURSUANT TO SECTION 27

OF THE ENERGY RESOURCES CONSERVATION BOARD RULES OF PRACTICE, AR 9812011

James Elford Department of Justice (Canada) 300 Epcor Tower 10423-101 Street Edmonton, Alberta T5H OE7 Telephone: (780) 442-1961 Facsimile: (780) 495-8491 E-Mail: james.elford@justice.gc.ca

Order Sought

1. The Attorney General of Canada, on behalf of Natural Resources Canada (NRCan), requests that the Joint Review Panel (JRP) make an order:

a. granting NRCan leave to file a document entitled "Fate of Naphtha Components in Oil Sands Tailings (the "Paper").

2. The grounds for this motion are:

a. the Paper is relevant to this public hearing and will assist the JRP in meeting its obligations under the Terms of Reference; and

b. no prejudice will result to the Proponent or other parties.

3. The affidavit of Ms. Kim Kasperski, Ph.D., sets out the facts to be relied upon for this motion, and includes a copy of the Paper.

Submissions

Background

4. Section 27 of the Energy Resources Conservation Board Rules of Practice, AR 98/2011 provides:

(1) A party who wishes to file a document, or a person who wishes to file a submission as an intervener, after the time limit set out in the notice of hearing has elapsed, may request of the Board leave to file the document or submission, as the case may be.

(2) The Board may grant a request under subsection (1) on any terms that the Board considers appropriate.

5. Pursuant to the Notice of Hearing, submissions were to have been filed by October 1, 2012.

6. NRCan has prepared the Paper which provides a summary of data from an ongoing experiment at NRCan to determine the thermodynamics and kinetics of volatile organic carbons (VOCs) from tailings ponds associated with oil sands development. Specifically, the Paper provides information on the quantity and speed of VOC release by tailings ponds.

7. The Paper was prepared by Dr. Kim Kasperski for a conference on oil sand tailings ponds to take place in December of 2012.

8. NRCan's submissions did not include the Paper as it was not completed in sufficient time to allow for it to be included.

The Paper will be of use to the JRP

9. NRCan submits that the Paper should be included in the evidence before the JRP. The Paper is relevant in that it will assist the JRP in meeting its obligations under the Agreement to Establish a Joint Review Panel for the Jackpine Mine Expansion Project, including specifically the associated Terms of Reference.

10. NRCan has already submitted evidence on the subject of VOC emissions from tailings at 2.4 of its submissions. It can be found under the heading VOC Emission Estimate From Tailings. The inclusion of this evidence will simply give the JRP more evidence with which to consider NRCan's position and the potential effect of this project.

11. NRCan submits that it is clear that the Paper will be of use to the JRP and leave should be granted to file it in evidence.

No Prejudice to the Proponent or Other Parties

12. NRCan submits that the late filing of the Paper as evidence will not be unfair to the Proponent or other parties. The Paper only reinforces and further substantiates NRCan's previously stated evidence regarding VOCs which is found in the submissions that were already filed.

13. Dr. Kasperski will testify before the Panel and will therefore be available to answer questions.

14. The foregoing is respectfully submitted in support of NRCan's request for leave to file the Paper.

TAKE NOTICE THAT the Affidavit of Ms. Kim Kasperski, Ph.D., Manager of the Oil Sands Water and Tailings Research Group is tendered in support of this Motion.

Joint Review anei/Shell Jackpine Mine Expansion Project nergy Resources Conservation Board

ERCB Law Branch Suite 1000, 250 5 Street SW Calgary, AB T2P OR4 Attention: Mr. Jim Dilay- Joint Review Panel Chairman- via email

AND TO: Martin K. Ignasiak- via email Stikeman Elliott, LLP 4300, 888-3 St SW Calgary, AB T2P 5C5

IN THE MATTER OF THE JOINT REVIEW PANEL ("JOINT PANEL") ESTABLISHED TO REVIEW THE JACKPINE MINE EXPANSION PROJECT

("PROJECT") PROPOSED BY SHELL CANADA LIMITED ("SHELL")

AFFIDAVIT OF KIM KASPERSKI

I, Kim Kasperski, Ph.D., of the City of Edmonton, Alberta, make oath and say:

1. I am the Manager of the Oil Sands Water and Tailings Research Group in Devon, Alberta, for Natural Resources Canada. My resume is attached to this my Affidavit as Exhibit "A".

2. The Oil Sands Water and Tailings Research Group, under my control and direction, have been conducting an experiment to determine the thermodynamics and kinetics of the release of volatile organic carbons from tailings ponds associated with oil sands development.

3. On September 26, 2012, I finalized a paper on the latest sample collected as part of this on-going experiment. The last sample relied upon in the paper was collected and the data referenced in the report was analyzed in early September. This paper is entitled "Fate of Naphtha Components in Oil Sand Tailings" and is attached to this my Affidavit as Exhibit "8".

4. The paper was prepared for the Third Annual International Oil Sands Tailings Conference which is scheduled for December 2 - 5, 2012. It is being hosted by the Oil Sands Tailings Research Facility and the International Canadian Oil Sands Network for Research and Development.

5. The paper forms the foundation of the presentation I will be giving at the Conference. I sent an abstract of the paper to conference organizers on March 2"d, 2012, and the abstract is attached to this my Affidavit as Exhibit "C".

6. Natural Resources Canada's internal deadlines for the finalization of written submissions for the Jackpine Oil Sands Mine Expansion Project hearing was prior to September 26, 2012.

7. I believe that the report is relevant to this hearing as it supplements the submissions already provided by NRCan at section 2.4 of its submissions, entitled VOC Emission Estimate From Tailings. Specifically, it provides evidence regarding the rate at which volatile organic carbon compounds leave oil sand tailings ponds.

8. I make this affidavit in support of a motion requesting that the Joint Review Panel allow the late filing of a document.

SWORN BEFORE ME at the City of Edmonton in the Province of Alberta the\~ dayof~012.

) ) ) )

~ A Commissioner of Oaths in and for the )

Province of Alberta )

ERIN ELIZABETH GALE MY COMMISSION §XPIRES

JULYS, 20.l:L

Kim Kasperski, Ph.D.

1 Oil Patch Drive Devon, Alberta T9G 1 A8 (780) 987-8665 Kim.kasperski@nrcan.gc.ca

EDUCATION

KIM L. KASPERSKI

SENIOR SCIENTIST I MANAGER NATURALRESOURCESCANADA

CanmetENERGY- Devon

UNIVERSITY OF ALBERTA- Edmonton, AB Doctor of Philosophy, Physical Chemistry (Thermodynamics)- 1988

McGILL UNIVERSITY- Montreal, PQ Master of Science, Biochemistry- 1983

UNIVERSITY OF LETHBRIDGE- Lethbridge, AB Bachelor of Science (with Honours), Chemistry -1977

EXPERIENCE

ERIN ELIZABETH GALE MY COMMISSION.e¥PIRES

JULY 8, 20-l.:S.

1) CanmetENERGY- Devon, NATURAL RESOURCES CANADA- DEVON, AB Manager, Oil Sands Water (since 2002) and Tailings (since 2011) Research Group

Team Projects: • Studies of the treatment of oil sand tailings • Study of partitioning of volatile hydrocarbons in oil sand tailings; • Determination of the persistence and fate of oil sand process chemicals; • Modeling and study of oil sand process water (inorganic) chemistry. Built computer

models or performed modelling for Suncor, Albian, True North, Imperial Oil, CNRL, Synenco, and Syncrude; (model work since 1998);

• Determination of factors affecting partitioning of naphthenic acids in oil sands tailings. • Study of high temperature and pressure chemistry of oil sand process water relevant to in

situ operations; • Produced an extensive review of emerging water treatment technologies and their

potential application to the oil sand industry.

Kim L. Kasperski - Resume Page 1 of2

EXPERIENCE (CONT'D)

2) CanmetENERGY- Devon, NATURAL RESOURCES CANADA- DEVON, AB Research Scientist, Emulsions and Tailings Group- I988 to 2002

Areas of work: • Water chemistry of oil sand tailings I process water systems; • Analysis of oil sand multiphase systems; • Hydrocarbon partitioning in oil sand process streams; • Thermodynamics of oil sand; • Thermal analysis of polymers; • Toxicity of oil sand process water;

PUBLICATIONS II papers in refereed journals or books. 3 7 papers presented at conferences or in conference proceedings (as author or co­

author). I43 divisional reports including confidential client reports.

The above include two major reviews, one on oil sands tailings (I988) and one on oil sand bitumen extraction fundamentals (200 I).

ADDITIONAL • Past-chair of the Canadian Oil Sand Network for Research and Development (CONRAD)

water focus group (2006 to 20IO); • Appeared before House of Commons Standing Committee on Natural Resources (2006)

and House of Commons Standing Committee on Environment and Sustainable Development (2009) as expert witness on oil sands water issues;

• Provide technical expertise on oil sand tailings and water issues to the executive branch of the federal department ofNatural Resources Canada.

Kim L. Kasperski - Resume Page 2 of2

Th1s is Exl'l\bl\" P-:> "rsferred to in the Affidavit of •

..... K\m .... ~{1.§.~.8 ......... . Affirmed before me this •• J~ ... day

of •••• acJ:Q ................ A.o..~~.~

ERIN ELIZABETH GALE MY COMMISSION ~RES

JULY 8, 20_u_

FATE OF NAPHTHA COMPONENTS IN OIL SAND TAILINGS Kim Kasperski, Xiaomeng Wang, Jiangying Wu, and Tadek Dabros

Natural Resources Canada, CanmetENERGY-Devon, Devon, Alberta, Canada

ABSTRACT The rate at which volatile organic carbon compounds (VOCs) leave oil sand tailings ponds has implications for operators and regulators concerned with air quality. The mobility of VOCs also has to be understood for reclamation when solvent-containing tailings may be moved about and re-handled. In addition, an understanding of the factors that affect VOC release from tailings ponds would help oil sand operators in designing tailings containment and handling of solvent-rich tailings such as froth treatment tailings.

In this report n-heptane and toluene, which are two components with usually the highest concentration in naphtha, were used to characterize the behaviour of volatile hydrocarbons in multiphase systems.

Impinging jet experiments showed that irrespective of any added mineral or mineral-bitumen, both heptane and toluene showed an initial rapid release from the water, which gradually decreased, with heptane being much more rapidly released than toluene.

When heptane and toluene were mixed with MFT and capped with water, their release from the MFT exhibited a lag period where there was not much change in MFT solvent concentration. However the concentration of heptane and toluene in the MFT eventually showed a linear decrease in concentration with about 80% of heptane being released within 9 months, and between 25% (frozen during winter) and 75% (never frozen) toluene being released.

INTRODUCTION Oil sand tailings contain volatile hydrocarbons from solvent that is not completely recovered from froth treatment tailings. Solvent sent to tailings ponds can end up in the pond water, adsorbed on mineral surfaces or dissolved in residual bitumen. Solvent which is not decomposed by bacteria can be released to the atmosphere through diffusion and convection. The objective of this research was to determine and model the factors that affect volatile hydrocarbon retention in tailings deposits.

The fate of VOCs in oil sands tailings is ultimately determined by the thermodynamics of partitioning

I

between gaseous, aqueous, solid and hydrocarbon phases, and the kinetics of these processes. In this study, a representative alkane hydrocarbon (n­heptane) and aromatic hydrocarbon (toluene) were used to characterize the behaviour of volatile hydrocarbons commonly found in naphtha. The evaporation of these VOCs from water phase was studied using an impinging jet apparatus and in addition, two mini-ponds were built to simulate solvent loss in a tailings pond. One of the pools was placed outdoor, to determine the impact of weather on the release of VOCs. The other pool was kept indoors to minimize weather effects.

EXPERIMENTAL Solvent release kinetics

Figure 1 shows the experimental setup used to study the kinetics of VOC release from water, and water with added solids (sand, clay, or bitumen­coated clay). It consists of a glass cylinder connected to a nitrogen source and a gas chromatograph (GC). Solvent-saturated water (or solids suspension) was added to the cylinder, keeping headspace to a minimum, and then left for 2 h to equilibrate with the headspace. A laminar flow of nitrogen was directed at right angles to the water surface, and the gas then exited to the side at the top and was carried to the GC. The total amount of solvent released during any time period was calculated from integration of the solvent peaks from the GC chromatogram. When solids were present, they were allowed to settle to the bottom of the cylinder after the set up.

Figure 1 - Apparatus used for solvent release experiments

VOC release from MFT pools

In order to approximate the VOC release from a tailings pond, an outdoor and an indoor pool were set up using mature fine tailing (MFT), solvent and tap water. The pools had a volume of 5 m3

, and were 2.4 m in diameter.

To fill the pools, MFT was homogenized in a tank and then pumped to a second tank. When the second tank was almost full, solvent was added and the MFT and solvent gently mixed for 30 minutes. After mixing, a thin layer of MFT was added on top to reduce solvent loss during a 2-day equilibration period. After 2 days, the MFT was mixed for 1 more hour before being pumped into the pool. Immediately after all the MFT had been added, tap water was carefully layered on top. The finished pool had a water layer about 33 em deep over an MFT deposit about 91 em deep. The outdoor pool was set up in November 2011 and the indoor pool was set up in January 2012. The pools were sampled at 4 or 5 depths (A to D or E) depending on the location (1 to 5) (Figure 2). A and B were in the water layer while C, D and E were (initially) in the MFT layer. After spring-thaw, the solid/water interface in the outdoor pool had dropped below the C-depth. The water level was kept constant during the course of the study by adding tap water to make up for evaporation losses.

cb ~

'

I A:

T :B s:

E :c 0 .... ;D "' E c.

l " c: a; D·

1 'E . E:

E:

Figure 2 - Sampling locations for pools

2

Figure 3 - Collecting samples from outdoor pool

Solvent content was determined in the MFT samples by analyzing a-xylene extracts on a GC­FID. An aliquot from the same extract was used to determined bitumen content by gravimetry. To measure the solvent concentration in the water the sample was injected directly into a GC-FID.

RESULTS AND DISCUSSION Solvent Release Kinetics

Assuming that transport of gas across the air/water interface is a steady-state process, it follows that:

F = kg(cg- csg) = k1(cs1 - c1)

where F is the flux of gas through the gas-liquid surface, cg is the VOC concentration in the gas

phase, csg is the VOC concentration in the gas

phase near the surface, cs1 is the VOC

concentration in the liquid phase near the gas­liquid surface and c1 is the VOC concentration in

the liquid phase. kg and k1 are the exchange

constants for the gas and liquid phases, respectively. If the exchange gas obeys Henry's

law, then csg = kHCsl, where kH is the Henry's

Law constant. A three-compartment model was built using Comsol software to simulate fluid dynamics in free and porous media. The modeling results can be used to compare with the experimentally obtained data. Based on modeling of other alkanes, the concentration of VOC in the water phase should decrease exponentially with time.

The initial concentrations of heptane and toluene in water were 8 ± 1 mg/L and 450 ± 25 mg/L

respectively. Figure 4 and Figure 5 show the release with time of heptane and toluene from water, water with sand, water with clay (kaolinite) and water with clay that has adsorbed bitumen (2.5 wt%) on its surface. The data are the concentrations of hydrocarbon in the purge gas from the heads pace of the impinging jet apparatus. The results show that heptane was rapidly released, and that there was essentially no heptane detected in the headspace after 10 minutes, for all systems. Toluene was released more slowly and was still evolving after 30 h. The presence of a mineral phase did affect the rate of release but not the ultimate concentration for heptane. For toluene the slowest release of was from the water-clay system but as these are preliminary data, this has to be checked before any conclusions can be drawn, especially as toluene release from the water-bitumen/clay system, was about the same as that from pure water.

e .s 10

20

0 H~ptane-;;.,ter- f

-----Heptane-bit-clay

--- Heptane-clay I - ; ·· ~- He_pta~e-s~n~--

11

0 _______ :~_.,,..., •.• _, __ .., __ , ___ ..,_,.._.__..,.,. .... """""~---·--_,_,_1 0.0 5.0 10.0 15.0 20.0 25.0 30.0 35.0

Time(mln)

Figure 4 -Graph of release of heptane from water saturated with heptane

8000

7000 ', --

.·. 6000 ~ --­

E a. ,!!, 5000 c 0 l! 4000 c g 3000

8 2000

1-• Toluene-bit-clay[ , _ _ 1····•-~- Toluene-water I -- -- ~

j -e- Toluene-clay

_:·t~_:_:_ T~!~en~s~~ J- -

0.00 50.00 100.00 150.00 200.00 250.00 300.00

Time (min)

Figure 5 - Graph of release of toluene from water saturated with toluene

VOC release from MFT pools

The amount of toluene and heptane that was added to the MFT was about 5-times what one

3

would calculate based on 4 vol. solvent per 1000 vol. bitumen production. The initial compositions of the MFT in the pools is given in Table 1.

Table 1 -Initial composition of MFT in pools

Concentration (wt%)

Indoor Pool Outdoor Pool

MFT bitumen 3.0 ± 0.3 2.5 ± 0.2

MFT solids 37.9 ± 0.9 37.1 ± 0.3

MFTwater 57.2 ± 0.7 57.8 ± 1.3

Heptane 0.074 0.089

Toluene 0.076 0.072

The outdoor pool froze shortly after being filled in November. Samples taken since spring-thaw showed a continuing evolution of toluene (Figure 6) from the MFT into the water1 and, what appeared to be, a trend of decreasing heptane (Figure 7) and toluene in the MFT (Figure 8). We roughly estimate that about 25% of the toluene had been released between November 2011 and August 2012 and about 75% of the heptane.

As one might expected the behaviour of the indoor pool was different than the outdoor. For a 3-month period, toluene in the surface water of the indoor pool was below the detection limit (0.1 ppm) (Figure 9). As the MFT showed no change in toluene concentration, no toluene (or heptane) was being released from the MFT. Since that period however, there was a steady release of toluene from the MFT to the water. As mentioned, the concentrations of heptane (Figure 1 0) and toluene (Figure 11) in the MFT showed little change for about 3 months, but since then have declined steadily. We estimate that about 80% of the heptane has been released and about 75% of the toluene.

1 Heptane in all water samples tested was below the detection limit of our method (1.0 ppm), but, as heptane was disappearing from the MFT we assume that the transport of heptane from the water phase to the air is much more rapid than from MFT to the water phase.

1.0

0.9

0.8

e c. 0.7 c. "; 0.6 0 :; 0.5

~ 0.4 u 5 0.3 u

0.2.

0.1

1A 1112A ["J3A ~4A

0.0 L.l.._B""""<Cl-,L.IIIIl.3---,J--"""'..L..

NV14 NV15 AP23 MA15 MA28 JN11

Figure 6- Toluene in water layer of outdoor pool

0.16

0.14

~ 0.12 ..,. ! 0.10 c 0 :; 0.08 ~ c 21 0.06 c 0 u 0.04

0.02

I

..

..

...... 1

l IQ 1EI I I1112Ei I f["J 3EIJ IBI4Ef, [m§EJ-j

-- - j I

- j

i ~· ~ ~I 0 00 \.L.IO!Io"""""""""'"'-'-r-----,.1-Jiiii.J!!--"-''"""'Y-"""'-'-,.ua.l!LJ,"-"'"'""'Y-"""'Ui

NV14 NV15 AP23 MA15 MA28 JN11 JN25 JL9 AU14

Figure 7- Heptane concentration in lowest MFT layer in outdoor pool

0.18

0.16

0.14 - .

:;: 0.12

! 5 0.10

i 0.08

~ s 0.06

0.04

0.02

NV14 NV15 AP23 MA15 MA28 JN11 JN25 JLS AU14

Figure 8- Toluene concentration in lowest MFT layer in outdoor pool

4

Figure 9 - Toluene concentration in water layer of indoor pool

Figure 1 0 - Heptane concentration in the lowest MFT-Iayer of the indoor pool

0.12

~ 0.10

"; 0.08 0 i 0.06

~ G1 0. 04 -1\lmll!liHII!IHIIIIHII!IHIUHI!IHI!JIH111H·IIliHI;-JIIIII u c 8 0.02 -lfiiiAIII':IIillllHil!UIMiilmlil!l!HI~fmll

0.00 lllllll

r- -

IHIIIJl

Figure 11 -Toluene concentration in the lowest MFT-Iayer of the indoor pool

Composition of Release Gases

A few months after setup, bubbles were observed rising to the surface of the indoor pool. Analysis of the gases showed mostly methane (Table 2), consistent with previous observations (1 ,2). A more detailed analysis showed that, aside from the expected methane, heptane, and toluene, there were also many branched linear and cyclic alkanes.

Table 2 -Composition of gases bubbling to surface of indoor pool

Compound Concentration (vol%)

June September

Methane 87 82

Carbon dioxide 7 3

Nitrogen 6 14

Hexanes 0.01 0.04

Heptanes 0.01 0.01

CONCLUSIONS When movement of molecules is relatively unconstrained, as in the impinging jet experiments, heptane and toluene show an initially rapid release from water, that slows exponentially. Heptane was released from solution faster than was toluene, as one might intuitively expect from their Henry's Law constants, ( k H ,heptane reported from 2272 to 833 bar

kg/mol; kH,toluene reported from 4.8 to 7.1 bar

kg/mol) (3), although kH is a thermodynamic

constant, not a kinetic constant. The presence of a mineral phase seemed to slow the initial release of heptane but seemed to have no impact on the initial rate of toluene release. However, the subsequent release of toluene seemed to be affected by the mineral present.

One sees the effect of constrained transport pathways when the data from the impinging-jet experiments is compared with the MFT-pools. There was a lag period observed in both indoor and outdoor ponds during which there was no apparent release of solvent. However, once started, there was a steady, linear decrease of solvent in the MFT. We speculate that during the lag period, drainage channels were established in the re-settling MFT solids by bacterial action, or some other mechanism, which allowed the physical release of the solvent.

ACKNOWLEDGEMENTS Many thanks to Craig McMullen, Amanda Neall, Lisa Robinson, Jordan Elias, Ken Dickson, and Pam Munoz for setting up the pools and subsequent analyses. A special thank you to Lisa Robinson for the report on the release gases.

Funding for this research was provided by Natural Resources Canada through the Clean Energy

5

Fund and the Panel for Research and Development.

REFERENCES 1. Penner, T.J. and Foght, J.M. Mature fine

tailings from oil sands processing harbour diverse methanogenic communities. Can. J. Microbial. 56, 459-470 (201 0).

2. Siddique, T., Gupta, R., Fedorak, P.M., MacKinnon, M.D. and Foght, J.M. A first approximation kinetic model to predict methane generation from an oil sands tailings settling basin. Chemosphere 72, 1573-1580 (2008).

3. Anon. NIST Chemistry WebBook. NIST Standard Reference Database Number 69. P. J. Linstrom and W. G. Mallard, editor(s). National Institute of Standards and Technology, Gaitherburg MD (2012).

ABSTRACT

OSTRF - International Oil Sands Tailings Conference 2012

Edmonton, Alberta

FATE OF RESIDUAL NAPHTHA COMPONENTS IN OIL SAND TAILINGS

K.L. Kasperski, J. Wu1, X. Wang, and T. Dabros

CanmetENERGY, Natural Resources Canada

Oil sand tailings contain volatile hydrocarbons from solvent that is not completely recovered from froth treatment tailings. Solvent sent to tailings ponds can end up in the pond water, adsorbed on mineral surfaces of the tailings solids, or dissolved in residual bitumen. Eventually, solvent which is not decomposed by bacteria is released to the atmosphere through diffusion and convection. The objective ofthis research was to determine and model the factors that affect volatile hydrocarbon retention in tailings deposits. We analyzed kinetics of solvent release from the solvent pool, water phase, and from subaqueous deposits of the tailings. Data obtained from these model studies were verified experimentally by analytical results obtained from small-scale (~5m3) ponds of oil sand mature fine tailings (MFT) dosed with known amounts of toluene and heptane.

This Is f.xtdbit" G "referred to in the Affidavit of

····~·~tf.Y.:l ... J$5?.~~8 ......... . Affirmed before me this ••• llo.:~ .... day

of •••• a:!P..~ .......... A.D., 2Q.l?

A NOtary Public, A CommissiOner· for Oaths In and for the Province of Alberta

ERIN ELIZABETH GALE MY COMMISSIONj:XPIRES

JULY 8, 20.l!;._

1 Currently on extended leave from Natural Resources Canada