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Optimizing XRF calibration protocols for elemental quantification of mineral solids from Athabasca oil sands

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Optimizing XRF calibration protocols for elemental quantification of

mineral solids from Athabasca oil sands

Patarachao, B.; Mercier, P. H. J.; Kung, J.; Woods, J. R.; Kotlyar, L. S.;

Sparks, B. D.; McCracken, T.

(2)

Optimizing XRF Calibration Protocols for Elemental

Quantification of Mineral Solids from Athabasca Oil Sands

B.Patarachao*, P.H.J Mercier*, J. Kung*, J.R. Woods*, L.S Kotlyar*, B.D. Sparks**, T. McCracken*

*Institute for Chemical Process and Environmental Technology, National Research Council Canada

1200 Montreal Road, Ottawa, ON, Canada K1A0R6

(3)

Athabasca Oil Sands

Oil sands being composed of coarse

sand, silt and clay solids (80

–85%),

bitumen (5

–15%) and water (1–5%)

Photographs taken from the National Geographic, March 2009

Oil sands mine

• an open-pit north of Fort McMurray

• produced ~ ¾ of a million barrels a day

(4)

Organic Rich Solid (ORS)

Oil sands

+

Toluene

+

Water

ORS

Agitate

Centrifuge

Low Temperature

Agglomerates

A

B

C

I = Illite

K = Kaolinite

Q = Quartz

A = Anatase

R = Rutile

P = Pyrite

D = Dolomite

S = Siderite

Z = Zircon

Plasma Oxidation

ORS sample

Solid particles

6 8 10 12 14 16 18 20 22 24 26 28 30 32 34

2-theta

I

K

I

K Q

K

A

Q

R

P

I

D

S

P

Z

~ 0.1-0.3g

(5)

United States Geological Survey (USGS)

– 8 standards

BCR-2, BHVO-2, BIR-1, DNC-1,GSP-2, QLO-1, SDC-1, W2-a

National Institute of Standards and Technology (NIST)

– 15 standards

Cement Standards:

SRM1880a, SRM1881a, SRM1882a,

SRM1883a, SRM1884a, SRM1885a,

SRM1886a,SRM1887a, SRM1888a,

Soil Standards:

SRM2586, SRM2857, SRM2709,

SRM2710, SRM2711, SRM2782

Centre de la Recherche Scientifique (CNRS)

– 16 standards

AC-E, AL-I, AN-G, BE-N, DR-N, DT-N, FK-N, GA, GH,

GL-O, GS-N, Mica-Fe, Mica-Mg, PM-S, UB-N, WS-E

Certified Reference Materials

(6)

TiO

2

- 99.999%purity, rutile

Fe

2

O

3

- 99.999%purity, metal basis

ZrO

2

- 99.99%purity

Concentration Range

0

10

20

30

40

50

60

70

80

N

a2

O

M

gO

K

2O

C

aO

A

l2

O

3

Si

O

2

P2

O

5

SO

3

Ti

O

2

Fe

2O

3

M

nO

Major Oxides

C

o

n

ce

n

tr

a

ti

o

n

(

w

t%)

0

20000

40000

60000

80000

100000

120000

140000

160000

Cr

Ni

Pb

Sr

Zn

Zr

Trace Elements

C

on

c

e

n

tr

ati

on

(p

p

m)

Certified Reference Materials

ORS samples

(7)

Claisse 66.67%Li

2

B

4

O

7

-32.83%LiBO

2

-0.5%LiBr

0.1g Sample + 7.0g Flux

Sample preparation

(8)

Challenges

1. Lack of certified reference materials to cover

important elements e.g. Fe, Ti and Zr

concentration in ORS

2. Small amount of samples available (100-300mg)

3. High carbon content (LOI ~ 25-30%)

(9)

• Vacuum mode

• 28mm mask

• 0.23dg collimator

Bruker AXS S4 Pioneer

Instrumentation

Crystals

Elements

PET

Si, Al

LiF200

Ca, Cr, Fe, K, Ni, Pb

Sr, Ti, Zn, Zr

LiF220

Mn

XS-55

Mg, Na

Ge

P, S

Measurement Conditions

4 kW sequential WDXRF with end window and

Rh-target X-ray tube

(10)

Calibration Curves for ORS

0

5

10

15

20

25

30

0 5 10 15 20 25 30 35

N

e

t

In

te

n

si

ty

TiO

2

(wt%)

0

10

20

30

40

50

60

70

80

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8

N

e

t

In

te

n

sit

y

Al2O3 (wt%)

0

10

20

30

40

50

60

0

20

40

60

80

100

N

e

t

In

te

n

si

ty

Fe

2

O

3

(wt%)

0

40000

80000

120000

160000

0 20 40 60 80 100 120 140

N

e

t

In

te

n

si

ty

Zr (ppm)

0

10

20

30

40

50

60

70

80

0 2 4 6 8 10 12 14 16 18 20 22

N

e

t

In

te

n

si

ty

SiO

2

(wt%)

±1.70wt%

±0.91wt%

±0.054wt%

±0.79wt%

±1138ppm

n=53

n=53

n=53

n=53

n=36

±0.040wt%

±0.30wt%

±239ppm

Un-Extended

(11)

Accuracy

10 Certified reference materials that

were not participated in the calibration

(12)

Accuracy

10 Certified reference materials that

were not participated in the calibration

(13)

Bitumen-Free Solids (BFS)

Fraction 1

>212um

Fraction 2

150-212um

Fraction 3

75-150um

Fraction 4

45-75um

Fraction 5

<44um

Oil sands

Soxhlet

– Dean and Stark extraction

with toluene

Extracted Bitumen

5-15%

Bitumen-Free solids

80-85%

Disperse in 0.1%w/w of Na

4

P

2

O

7

Screen through standard sieve

Water

1-5%

• Processability of oil sands

• Recovery of heavy metals

• Recycle of oil sands tailing

(14)

5

10

15

20

25

30

35

0 200000 400000 600000 800000 1000000 1200000 1400000

C

o

u

n

ts

2-theta

Calibration for BFS

Major Oxides

Min (wt%)

Max (wt%)

SiO

2

90

100

Al

2

O

3

0

5

Minor Elements

Min (ppm)

Max (ppm)

Mg

0

10000

Ca

0

10000

Ti

0

10000

Cr

0

10000

Mn

0

10000

Fe

0

10000

Ni

0

10000

Zr

0

10000

Zn

0

10000

K

0

10000

Calibration Range

5 10 15 20 25 30 35 0 5000 10000 15000 20000

C

ou

n

ts

2-theta

Q

Q

I

K

I

K

A

S

P

Q = Quartz

I = Illite

K = Kaolinite

A = Anatase

S = Siderite

P = Pyrite

(15)

Oxides

Purity

SiO

2

99.995% metals basis

Al

2

O

3

99.998% metals basis

MgO

99.999%

CaO

99.995%

TiO

2

99.999%, rutile

Cr

2

O

3

99.9%

MnO

99.99+% metals basis

Fe

2

O

3

99.999% metals basis

NiO

99.999% metals basis

ZrO

2

99.99%

ZnO

99.999% metals basis

K

2

CO

3

99.995%

Sample preparation

McCrone Micronizing Mill

Claisse 49.25%Li

2

B

4

O

7

-49.25%LiBO

2

-0.5%LiBr

 Perfect beads

10g of oxide mixtures

+

25 mL of isopropanol

Weigh and mix different

oxides concentrations

Air dry for 24 hrs

Wet grinding

– 5 min

Fusion

1.0g Sample + 7.0g Flux

Claisse 66.67%Li

2

B

4

O

7

-32.83%LiBO

2

-0.5%LiBr  Un-dissolved particles

Claisse 34.83%Li

2

B

4

O

7

-64.67%LiBO

2

-0.5%LiBr  Crystallization

(16)

0

2000

4000

6000

8000

10000

0 100 200 300 400

N

e

t

In

te

n

s

it

y

Zr (ppm)

N=48

±153ppm

0

2000

4000

6000

8000

10000

0 10 20 30 40

N

e

t

In

te

n

si

ty

Zr (ppm)

0

2000

4000

6000

8000

10000

0 5 10 15 20 25 30

N

e

t

In

te

n

si

ty

Fe (ppm)

±318ppm

N=24

Why Micronizing?

±655ppm

N=27

Un-Micronized

Un-Micronized

0

2000

4000

6000

8000

10000

0 10 20 30 40 50

N

e

t

In

te

n

si

ty

Fe (ppm)

N=66

±115ppm

Micronized

Micronized

(17)

90

92

94

96

98

100

185 190 195 200 205 210 215 220

N

e

t

In

te

n

si

ty

SiO

2

(wt%)

N=69

±0.27 wt%

0

1

2

3

4

5

0.0 0.2 0.4 0.6 0.8 1.0

N

e

t

In

te

n

si

ty

Al

2

O

3

(wt%)

N=51

±0.06 wt%

0 2000 4000 6000 8000 10000 0 10 20 30 40 50 N e t In te n si ty

Fe (ppm)

N=66

±115ppm

0

2000 4000 6000 8000 10000

0 2 4 6 8 10 N e t In te n si ty

Ti (ppm)

N=54

±80ppm

0 2000 4000 6000 8000 10000 0 100 200 300 400 N e t In te n s it y

Zr (ppm)

N=48

±153ppm

Calibration Curves for BFS

(18)

-1

0

1

2

3

4

5

6

7

8

0

100

200

300

400

500

600

700

800

B

F

S

_

Z

r

(p

p

m

)

ORS_Zr(wt%)

0

2

4

6

8

10

12

0

1000

2000

3000

4000

T

S

_

T

i(

p

p

m

)

ORS_Ti(wt%)

Results Correlation

• Zr and Ti content in BFS and ORS samples compared

• More data is required to determine the relationship

B

F

S_

T

i(

ppm

)

(19)

Conclusion

 Optimized the calibrations for two types of mineral

solids in oil sands

 Able to achieve good precision and accuracy in the

calibrations without matrix correction

 Discover some correlation that could be a possible

marker for oil sands recovery

 Potential applications in mineral recycling and heavy

metal recovery from oil sands tailings

 Future work: quantification of heavy metal in oil sands

bitumen (Ni, V, Fe)

(20)

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