barite - density · 2019-07-29 · how do we determine density? mass per unit volume = density ......
TRANSCRIPT
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Barite - Density
Andrew Scogings
Principal Consultant
CSA Global, Perth, Australia
Houston, 8 May 2018 www.csaglobal.com
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Presentation outline
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• What is density?
• Why is density important?
• How does mineralogy relate to density?
• How do we measure density?
• Le Chatelier vs Gas Pycnometer test results
• Quality Control
• Conclusions and recommendations
Le Chatelier
Gas Pycnometer
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Excalibar Minerals LLC
CSA Global Pty Ltd
IMFORMED
Intertek Group plc
KlipStone Pty Ltdwww.csaglobal.com
Acknowledgements
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What is density?
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What is density?
Density vs SG
Term Units Definition
Density t/m3 Mass per unit volume
Specific Gravity Relative density: the ratio of the
density of the material to the density
of water at 4oC
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Why is density important?
Incorrect density measurements WILL have consequences!
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Mineralogy & Density
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Density – stoichiometric method
Relationship between mineralogy and density
Source: Lipton and Horton (2014) www.csaglobal.com
• Assays, or mineral contents, are expressed as weight %
• However, density is expressed in terms of volume
• Example: a quartz-copper rock has a grade of 50% copper
➢ Copper density = 8.9 g/mL; Quartz = 2.7 g/mL
➢ Mass weighted density = (8.9+2.7)/2 = 5.8 g/mL
➢ However copper is only 23% of the sample volume
➢ Volume based density = 4.14 g/mL
• Relationship between grade and density is curved
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Density – stoichiometric method
Example of lab-prepared Barite + Quartz (silicate) blends
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• Seven lab blends of barite and quartz
powders
• Ranging from 25% to 95% barite by mass
• Density measured using argon gas
pycnometer
• Density calculated based on mass
• Density calculated based on volume
BaSO4% (mass) SiO2 (Mass)
100% 0%
95% 5%
90% 10%
85% 15%
80% 20%
75% 25%
50% 50%
25% 75%
0% 100%
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Density – stoichiometric method
Example of lab-prepared Barite + Quartz (silicate) blends
BaSO4 SiO2 Barite (calc) Silicate (calc) Density (calc) Density (calc) Pycnometer
(% by mass) (% by mass) (% by volume) (% by volume) (g/mL by mass) (g/mL by volume) (g/mL lab blend)
100 0 100 0 4.5 4.5 4.5
95 5 92 8 4.4 4.4 4.4
90 10 84 16 4.3 4.2 4.2
85 15 77 23 4.2 4.1 4.0
80 20 71 29 4.1 4.0 4.050 50 38 63 3.6 3.4 3.5
25 75 17 83 3.2 3.0 3.0
0 100 0 100 2.7 2.7 2.7
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Density – stoichiometric method
Density calculated by volume or mass, compared with pycnometer
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Density – stoichiometric method
Conclusions
• Density is based on volume
• Thus relationship between grade and density is curved
• Curved line verified by pycnometer measurements
• The curved lines means that a quartz – barite rock will have a
higher volume of quartz than expected from SiO2 content
Calculated Quartz volumes
• Barite 4.2 - about 15% quartz by volume / 10% SiO2 by mass
• Barite 4.1 - about 25% quartz by volume / 15% SiO2 by mass
• Barite 3.9 - about 35% quartz by volume / 25% SiO2 by mass
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How do we measure density?
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How do we determine density?
Mass per unit volume = density
• We need to measure mass and
volume
• Measuring mass is the ‘easy bit’• However, the sample could be a:
• Competent solid (e.g. ‘fresh’ drill core, rock sample)
• Porous solid (e.g. weathered rock)
• Powder (e.g. milled barite)
• Therefore volume is typically the
‘difficult bit’ to measure
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Whole core tray method
Calliper method
Wax method
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There is a bewildering array of methods for measuring the
volume of samples (as core, rocks, stockpiles, powders, etc)
• Weight in water vs weight in air (Archimedes principle)
• Calliper – physical measurement
• Geophysical – down hole
• Core tray – weathered core
• Liquid displacement – Le Chatelier
• Gas displacement - pycnometer
How do we determine density?
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How do we determine density?
Competent solid – rock or drill core
• Immersion method (Archimedes)
• Volume determined by mass in air vs mass in water
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How do we determine density?
Stockpile loose density (10% moisture) using a cubic metre box
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Steel box 1m3
Clay stockpile
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How do we determine density?
Le Chatelier flask equipment for barite powder
Source: Excalibar Minerals LLC www.csaglobal.com
Heater & thermostat
Water tank
Weight Flask
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How do we determine density?
Le Chatelier flask equipment might look like this………….
Source: Andrew Scogings www.csaglobal.com
Crusher
Oven
Mill
Flasks
Balance
Flasks
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How do we determine density?
Gas pycnometers are an option for barite powder (API 13/I)
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API Specification 13A
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API Specification 13A
API Specification 13A – Sections 7 & 20
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Le Chatelier vs Pycnometer
Barite density test methods• The API specifies the Le Chatelier flask as the default method
• This utilises liquid displacement (kerosene or mineral spirits)
• API Recommended Practice 13I/ISO 10416 describes Air
Pycnometer and Stereopycnometer methods, but:
• “In case of dispute, the results from the Le Chatelier flask method prevail.”
• This study compares the results between Le Chatelier and gas
pycnometer methods
• Excalibar Minerals LLC supplied 30 milled barite samples of three
products PlusWate™, NewWate™ and NewBar™• Densities clustered in three groups between ~3.9 to ~4.3 g/mL
• Excalibar in-house results compared with commercial laboratory
results
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Quantachrome Stereopycnometer SPY2
Beckman Model 930 Air Comparison
API 13I pycnometers (outdated?)
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Le Chatelier method API 13A sections 7 & 20
Le Chatelier method – a slow process > 4 hours• Take approximately 100 g of barite that has been oven dried for at least two hours and cooled to room
• temperature in a desiccator.
• Fill a clean Le Chatelier flask to approximately 22 mm (0.8 in) below the zero mark with kerosene.
• Allow the flask and contents to equilibrate for a minimum of 1 h.
• Read the volume to the nearest 0,05 ml without removing the flask from the constant-temperature bath.
• If the kerosene level is outside the −0,2 ml to +1,2 ml volume range after equilibrating, use the 10 ml pipette to• add or remove kerosene in order to bring it within this range. Allow the flask to equilibrate for at least 1 h and
• record the initial volume.
• Remove the Le Chatelier flask from the bath, wipe dry and remove the stopper.
• Weigh 80 g ± 0,05 g of dried barite into the weighing dish and carefully transfer it to the Le Chatelier
• flask. Take care to avoid splashing the kerosene or plugging the flask with barite at the bulb. This is a slow
• process, requiring repeated transfers of small amounts of barite.
• 7.3.8 Gently roll the flask along a smooth surface at no more than 45° from vertical, or twirl the upright flask
• at the neck vigorously between the palms of both hands, to remove entrained air from the barite sample.
• Repeat this procedure until no more bubbles can be seen rising from the barite.
• Return the flask to the bath and let stand for at least 0.5 h.
• Remove the flask from the bath and repeat 7.3.8 to remove any remaining air from the barite sample.
• Immerse the flask in the bath again for at least 1 h.
• Record the final volume and record the volume as V2.
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Le Chatelier flask accuracy
mass volume density
g mL g/mL
80.00 20.50 3.90
80.00 20.00 4.00
80.00 19.50 4.10
80.00 19.05 4.20
80.00 18.60 4.30
How accurate is the flask?
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Barite density (g/mL)
Ba
rite
vo
lum
e(m
L)
mass volume density
g mL g/mL
80.00 19.50 4.10
80.00 19.45 4.11
80.00 19.40 4.12
80.00 19.35 4.13
80.00 19.30 4.15
80.00 19.25 4.16
80.00 19.20 4.17
80.00 19.15 4.18
80.00 19.10 4.19
80.00 19.05 4.20
80.00 19.00 4.21
80.00 18.95 4.22
80.00 18.90 4.23
80.00 18.85 4.24
80.00 18.80 4.26
~0.5 mL: 0.1 g/mL)
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How do we determine density?
Gas displacement pycnometry
• Inert gases, such as helium or nitrogen, are used as the displacement medium
• The sample is sealed in the instrument compartment of known volume
• Inert gas is admitted, then expanded into another precision internal volume
• The pressures observed upon filling the sample chamber and then discharging it into a second
empty chamber allow computation of the sample solid phase volume.
• Only the solid phase of the sample displaces the gas
• Dividing this volume into the sample weight gives the gas displacement density
Source: Micromeritics ACCUPYC II brochure www.micromeritics.com www.csaglobal.com
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N Pycnometer vs Le Chatelier
ID Excalibar Le Chatelier Excalibar Nitrogen
1 4.15 4.15
2 4.16 4.17
3 4.15 4.17
4 4.16 4.16
5 4.13 4.17
6 4.17 4.17
7 4.17 4.17
8 4.15 4.16
9 4.15 4.17
10 4.17 4.17
11 3.96 3.98
12 4.03 4.06
13 4.04 4.08
14 3.94 3.97
15 3.98 4.00
16 3.96 3.98
17 3.94 3.96
18 3.96 3.97
19 3.96 3.97
20 3.94 3.98
21 4.24 4.26
22 4.23 4.25
23 4.23 4.27
24 4.23 4.27
25 4.23 4.25
26 4.23 4.25
27 4.23 4.26
28 4.21 4.26
29 4.21 4.26
30 4.22 4.26
Positive bias to Nitrogen pycnometer
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Excalibar Le Chatelier (g/mL)
Exc
ali
ba
r N
itro
ge
n (
g/m
L)
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N Pycnometer vs Le Chatelier
Conclusions
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• Nitrogen pycnometer average is
0.5% higher than Le Chatelier
• Nitrogen pycnometer up to 1.2%
higher than Le Chatelier
• Gas penetrates deeper into pore
spaces, cracks or cavities than
kerosene – giving a lower volume
ID Le Chatelier Nitrogen Accupyc Diff % Diff
1 4.15 4.15 0.01 0.2%
2 4.16 4.17 0.02 0.4%
3 4.15 4.17 0.03 0.6%
4 4.16 4.16 0.00 0.1%
5 4.13 4.17 0.03 0.8%
6 4.17 4.17 0.00 0.0%
7 4.17 4.17 0.01 0.1%
8 4.15 4.16 0.02 0.5%
9 4.15 4.17 0.02 0.5%
10 4.17 4.17 0.00 0.0%
11 3.96 3.98 0.02 0.4%
12 4.03 4.06 0.02 0.6%
13 4.04 4.08 0.04 1.0%
14 3.94 3.97 0.03 0.6%
15 3.98 4.00 0.02 0.5%
16 3.96 3.98 0.02 0.4%
17 3.94 3.96 0.02 0.6%
18 3.96 3.97 0.01 0.4%
19 3.96 3.97 0.01 0.2%
20 3.94 3.98 0.04 1.0%
21 4.24 4.26 0.02 0.5%
22 4.23 4.25 0.02 0.4%
23 4.23 4.27 0.04 0.9%
24 4.23 4.27 0.04 0.9%
25 4.23 4.25 0.01 0.3%
26 4.23 4.25 0.02 0.4%
27 4.23 4.26 0.02 0.6%
28 4.21 4.26 0.05 1.2%
29 4.21 4.26 0.05 1.1%
30 4.22 4.26 0.04 0.9%
Global Average 4.12 4.14 0.02 0.5%
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Ar Pycnometer vs Le Chatelier
ID Excalibar Le Chatelier Intertek Argon
1 4.15 4.15
2 4.16 4.24
3 4.15 4.24
4 4.16 4.23
5 4.13 4.23
6 4.17 4.17
7 4.17 4.21
8 4.15 4.25
9 4.15 4.2
10 4.17 4.22
11 3.96 4.06
12 4.03 4.09
13 4.04 4.09
14 3.94 4.04
15 3.98 4.05
16 3.96 3.98
17 3.94 4
18 3.96 3.99
19 3.96 4.03
20 3.94 4.01
21 4.24 4.31
22 4.23 4.3
23 4.23 4.33
24 4.23 4.34
25 4.23 4.22
26 4.23 4.23
27 4.23 4.3
28 4.21 4.31
29 4.21 4.28
30 4.22 4.32
Positive bias to Argon* pycnometer
* Note Argon samples were not dried www.csaglobal.com
Excalibar Le Chatelier (g/mL)
Inte
rte
k A
rgo
n (
g/m
L)
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Ar Pycnometer vs Le Chatelier
Conclusions
* Note Argon samples were not dried www.csaglobal.com
• Argon* pycnometer global
average 1.5% higher than Le
Chatelier
• Ranges from -0.3% to 2.5%
difference
• The Argon samples were tested
‘as received’
ID Le Chatelier Intertek Argon Diff % Diff
1 4.15 4.15 0.01 0.1%
2 4.16 4.24 0.08 2.0%
3 4.15 4.24 0.10 2.3%
4 4.16 4.23 0.07 1.8%
5 4.13 4.23 0.10 2.3%
6 4.17 4.17 0.00 0.1%
7 4.17 4.21 0.04 1.0%
8 4.15 4.25 0.11 2.5%
9 4.15 4.20 0.06 1.3%
10 4.17 4.22 0.05 1.3%
Average 4.15 4.21 0.06 1.5%
11 3.96 4.06 0.10 2.5%
12 4.03 4.09 0.06 1.5%
13 4.04 4.09 0.05 1.2%
14 3.94 4.04 0.10 2.5%
15 3.98 4.05 0.07 1.8%
16 3.96 3.98 0.02 0.5%
17 3.94 4.00 0.06 1.5%
18 3.96 3.99 0.03 0.8%
19 3.96 4.03 0.07 1.8%
20 3.94 4.01 0.07 1.8%
Average 3.97 4.03 0.06 1.6%
21 4.24 4.31 0.07 1.6%
22 4.23 4.30 0.07 1.6%
23 4.23 4.33 0.10 2.3%
24 4.23 4.34 0.11 2.5%
25 4.23 4.22 -0.01 -0.3%
26 4.23 4.23 0.00 -0.1%
27 4.23 4.30 0.07 1.6%
28 4.21 4.31 0.10 2.4%
29 4.21 4.28 0.07 1.7%
30 4.22 4.32 0.10 2.3%
Average 4.23 4.29 0.07 1.6%
Global Average 4.12 4.18 0.06 1.5%
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Argon vs Nitrogen pycnometer
Positive bias to Argon pycnometer*
* Note Argon samples were not dried www.csaglobal.com
ID Excalibar Nitrogen Intertek Argon
1 4.15 4.15
2 4.17 4.24
3 4.17 4.24
4 4.16 4.23
5 4.17 4.23
6 4.17 4.17
7 4.17 4.21
8 4.16 4.25
9 4.17 4.20
10 4.17 4.22
11 3.98 4.06
12 4.06 4.09
13 4.08 4.09
14 3.97 4.04
15 4.00 4.05
16 3.98 3.98
17 3.96 4.00
18 3.97 3.99
19 3.97 4.03
20 3.98 4.01
21 4.26 4.31
22 4.25 4.30
23 4.27 4.33
24 4.27 4.34
25 4.25 4.22
26 4.25 4.23
27 4.26 4.30
28 4.26 4.31
29 4.26 4.28
30 4.26 4.32Excalibar Nitrogen (g/mL)
Inte
rte
k A
rgo
n (
g/m
L)
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Argon vs Nitrogen pycnometer
Conclusions
* Note Argon samples were not dried www.csaglobal.com
• Argon* pycnometer averages 1 %
higher than Nitrogen pycnometer
• Ranges from -0.6 % to 2.1 %
• The Argon samples were tested ‘as received’
ID Excalibar Nitrogen Intertek Argon Diff % Diff
1 4.15 4.15 0.00 0.0%
2 4.17 4.24 0.07 1.6%
3 4.17 4.24 0.07 1.7%
4 4.16 4.23 0.07 1.7%
5 4.17 4.23 0.06 1.5%
6 4.17 4.17 0.00 0.0%
7 4.17 4.21 0.04 0.9%
8 4.16 4.25 0.09 2.1%
9 4.17 4.20 0.03 0.8%
10 4.17 4.22 0.05 1.2%
Average 4.17 4.21 0.05 1.1%
11 3.98 4.06 0.08 2.1%
12 4.06 4.09 0.04 0.9%
13 4.08 4.09 0.01 0.2%
14 3.97 4.04 0.07 1.9%
15 4.00 4.05 0.05 1.3%
16 3.98 3.98 0.00 0.1%
17 3.96 4.00 0.04 0.9%
18 3.97 3.99 0.02 0.4%
19 3.97 4.03 0.06 1.6%
20 3.98 4.01 0.03 0.8%
Average 3.99 4.03 0.04 1.0%
21 4.26 4.31 0.05 1.1%
22 4.25 4.30 0.05 1.1%
23 4.27 4.33 0.06 1.4%
24 4.27 4.34 0.07 1.6%
25 4.25 4.22 -0.03 -0.6%
26 4.25 4.23 -0.02 -0.5%
27 4.26 4.30 0.04 1.0%
28 4.26 4.31 0.05 1.2%
29 4.26 4.28 0.02 0.5%
30 4.26 4.32 0.06 1.4%
Average 4.26 4.29 0.04 0.8%
Global Average 4.14 4.18 0.04 1.0%
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Argon (dry) vs Argon original pycnometer
Note that original Argon samples were not dried www.csaglobal.com
ID Argon pycnometer Argon pycnometer (dry)
1 4.15 4.18
2 4.24
3 4.24 4.08
4 4.23
5 4.23
6 4.17 4.21
7 4.21
8 4.25
9 4.20 4.15
10 4.22
11 4.06
12 4.09 4.09
13 4.09
14 4.04
15 4.05 4.03
16 3.98
17 4.00
18 3.99 3.93
19 4.03
20 4.01
21 4.31 4.25
22 4.30
23 4.33
24 4.34 4.31
25 4.22
26 4.23
27 4.30 4.18
28 4.31
29 4.28
30 4.32Intertek Argon original (g/mL)
Inte
rte
k A
rgo
n d
ry (
g/m
L)
Slight positive bias towards Argon original
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Argon (dry) vs Argon pycnometer
Conclusions
• Density is 1% lower on average after
2 hours drying
• Differences between -3.8% and +1%
• Drying seems to make a difference
www.csaglobal.com
ID
Ar pycnometer
(original)
Ar pycnometer
(dry) Diff % Diff
1 4.15 4.18 0.03 0.7%
3 4.24 4.08 -0.16 -3.8%
6 4.17 4.21 0.04 1.0%
9 4.20 4.15 -0.05 -1.2%
12 4.09 4.09 0.00 0.0%
15 4.05 4.03 -0.02 -0.5%
18 3.99 3.93 -0.06 -1.5%
21 4.31 4.25 -0.06 -1.4%
24 4.34 4.31 -0.03 -0.7%
27 4.30 4.18 -0.12 -2.8%
Average 4.18 4.14 -0.04 -1.0%
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Argon (dry) vs Nitrogen pycnometer
No bias to Argon (dry) pycnometer
Note that Argon samples were dried 2 hours www.csaglobal.com
Excalibar Nitrogen (g/mL)
Inte
rte
k A
rgo
n d
ry (
g/m
L)
ID Nitrogen pycnometer Argon pycnometer
1 4.15 4.18
3 4.17 4.08
6 4.17 4.21
9 4.17 4.15
12 4.06 4.09
15 4.00 4.03
18 3.97 3.93
21 4.26 4.25
24 4.27 4.31
27 4.26 4.18
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Argon (dry) vs Nitrogen pycnometer
Conclusions• Average density for Nitrogen
(4.15 g/mL) almost identical to
Argon dry (4.14 g/mL)
• Between -2.2% and +1%
difference
• Drying appears to be important
• However, the customer uses
barite ‘as received’ moisture• Preferable to test barite product
‘as received’ rather than after drying?
www.csaglobal.com
ID Nitrogen pycnometer Argon pycnometer Diff % Diff
1 4.15 4.18 0.03 0.7%
3 4.17 4.08 -0.09 -2.2%
6 4.17 4.21 0.04 1.0%
9 4.17 4.15 -0.02 -0.4%
12 4.06 4.09 0.04 0.9%
15 4.00 4.03 0.03 0.8%
18 3.97 3.93 -0.04 -1.1%
21 4.26 4.25 -0.01 -0.3%
24 4.27 4.31 0.04 0.9%
27 4.26 4.18 -0.08 -1.8%
Average 4.15 4.14 -0.01 -0.2%
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Helium pycnometer vs Le Chatelier
No obvious bias
Note that Argon samples were dried 2 hours www.csaglobal.com
Excalibar Le Chatelier (g/mL)
Inte
rte
k H
eli
um
(g
/mL)
ID
Excalibar Le
Chatelier
Excalibar
Nitrogen
Intertek
Helium
3 4.15 4.17 4.17
15 3.98 3.99 3.98
24 4.23 4.27 4.26
• Only three data points
• Helium pycnometer is
very close to Le Chatelier
Conclusions
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Quality Control
www.csaglobal.com
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Quality Control
Where do we want our analytical results to be?
Source: Scogings and Coombes (2014) www.csaglobal.com
• poor accuracy
• good precision
• high bias• good accuracy
• good precision
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Quality Control
What is QA / QC ?
Source: Scogings and Coombes (2014) www.csaglobal.com
• QA is planned actions to provide confidence in the data collection process
• QC is the use of statistical tools to ensure that the analytical systems are in
control
• QC samples are necessary to monitor contamination, precision, accuracy and
bias
• QC samples include standards, duplicates and external checks (umpire)
• Standards are samples of known or accepted value that are submitted to
assess the accuracy of a laboratory
• Duplicates are samples collected, prepared and assayed in an identical manner
to an original sample, to provide a measure of the total error of sampling
• External laboratory checks generally rely on pairs of pulverised exploration
samples (also known as umpire samples) to define inter-laboratory precision
and bias.
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Quality Control
Types of QC charts used in geological exploration
Source: Scogings and Coombes (2014) www.csaglobal.com
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Quality Control
Calibration – mass and volume
www.csaglobal.com
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Quality ControlORIGINAL (Le Chatelier) Original (Nitrogen) ORIGINAL (Argon) DUPLICATE (Argon) DUPLICATE (Argon dry) UMPIRE (Helium)
SAMPLE NUMBERS Density Density Density Density Density Density
1 4.15 4.15 4.15 4.18
2 4.16 4.17 4.24
3 4.15 4.17 4.24 4.08 4.17
4 4.16 4.16 4.23
5 4.13 4.17 4.23
6 4.17 4.17 4.17 4.21
7 4.17 4.17 4.21
8 4.15 4.16 4.25
9 4.15 4.17 4.20 4.15
10 4.17 4.17 4.22 4.18
11 3.96 3.98 4.06
12 4.03 4.06 4.09 4.09
13 4.04 4.08 4.09
14 3.94 3.97 4.04
15 3.98 4.00 4.05 4.03 3.98
16 3.96 3.98 3.98
17 3.94 3.96 4.00
18 3.96 3.97 3.99 3.93
19 3.96 3.97 4.03
20 3.94 3.98 4.01 4.07
21 4.24 4.26 4.31 4.25
22 4.23 4.25 4.30
23 4.23 4.27 4.33
24 4.23 4.27 4.34 4.31 4.26
25 4.23 4.25 4.22
26 4.23 4.25 4.23
27 4.23 4.26 4.30 4.18
28 4.21 4.26 4.31
29 4.21 4.26 4.28
30 4.22 4.26 4.32 4.33
BaSO4 Standard 4.43
Quartz-1 Standard 2.64
www.csaglobal.com
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Quality Assurance & Control
Conclusions – density QA / QC • Equipment should be regularly calibrated (QA)
• QC samples (each approximately 5% of originals):
➢ Standards
➢ Duplicates
➢ External checks (umpire)
➢ Alternative test methods
o e.g. if testing by Le Chatelier, use gas pycnometer as a check
o For incoming crudes, test using Le Chatelier for a milled
sample and also run some using whole rock by the
‘Archimedes’ method
www.csaglobal.com
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Conclusions
www.csaglobal.com
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Barite density
Conclusions – density methods• Le Chatelier
➢ Robust method
➢ However, very time consuming ~ 4 hours
➢ Cannot be automated or digitised – labour intensive
➢ Relatively inexpensive equipment (~$1K)
• Gas pycnometer
➢ Biased to higher densities (~ 1 % difference)
➢ Quick and easy to use ~ 5 minutes
➢ No chemicals to be disposed
➢ Can be automated and free up the operator
➢ Smaller footprint than Le Chatelier
➢ Relatively expensive equipment (~20K)www.csaglobal.com
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Barite density
General comments and questions
➢ If it is assumed that kerosene does not penetrate the barite in
the same way as a gas atom does, could a systematic
correction factor be applied to pycnometer data?
➢ Perhaps the API Le Chatelier method is more appropriate?
(even if more tedious to perform than pycnometry)
➢ Could the Le Chatelier method be improved by using two
separate funnels* to add liquid, or dry barite powder?
➢ Assuming that drilling muds are mainly water, perhaps water
should be used for Le Chatelier tests?
➢ Gas pycnometers are already accepted for refractory materials
density (ASTM C604). Why not for barite?
* e.g. Helsel et al., 2016 www.csaglobal.com
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Barite density
Conclusions – Mineralogy & QC
• Mineralogy
➢ Relationship between grade and density is curved
➢ A quartz – barite rock will have a higher volume of quartz
than expected from SiO2 content
➢ This may have implications for plant wear
• Quality Control
➢ Test equipment should be calibrated
➢ Insert QC samples (approximately 5% of originals):
➢ Standards, duplicates, external checks (umpire)
➢ Alternative test methods
www.csaglobal.com
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Recommendations
www.csaglobal.com
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Barite density
Recommendations• Evaluate alternate liquids for Le Chatelier e.g. Escaid 110,
isopropyl alcohol, ethyl alcohol (and water?)
• Try and improve the Le Chatelier method (e.g. adding barite via a
funnel)
• Assess the effect of temperature on Le Chatelier – does it have
to be at 32oC?
• Approach the API about updating the recommended
pycnometers to currently available models
• Collaboration between producers and commercial labs to
compare different methods and convince API to add gas
pycnometer as an alternative to Le Chatelier in Specification 13A
• Use QA and QC methods to ensure accurate and precise results
www.csaglobal.com
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Thank youAcknowledgments
• Excalibar Minerals LLC (David Henrick, Joe Gocke, Lori Garcia)
• CSA Global Pty Ltd
• Intertek Group plc
• IMFORMED Industrial Mineral Forums and Research
• KlipStone Pty Ltd
Houston, May 2018 www.csaglobal.com
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Bibliography
www.csaglobal.com
• Abzolov, M. Z., 2008. Quality Control of Assay Data: A Review of Procedures for Measuring and Monitoring Precision and
Accuracy. Exploration and Mining Geology, Vol. 17, 131–144. Canadian Institute of Mining, Metallurgy and Petroleum.
• Abzolov, M. Z., 2009. Use of Twinned Drillholes in Mineral Resource Estimation. Exploration and Mining Geology, Vol. 18,
13–23. Canadian Institute of Mining, Metallurgy and Petroleum.
• CIM, 2003. Estimation of Mineral Resources and Mineral Reserves Best Practice Guidelines. Available from:
http://web.cim.org/standards Canadian Institute of Mining, Metallurgy and Petroleum.
• Helsel, M., Ferraris, C. and Bentz, D. (2016). Comparative study of methods to measure the density of cementicous
powders. Journal of Test Evaluation, 44 (6).
• Lipton, I.T. and Horton, J.A. (2014). Measurement of bulk density for resource estimation - methods, guidelines and quality
control. Mineral resource and ore reserve estimation : the AusIMM guide to good practice. Monograph 30.
• Micromeritics (2014). Accupyc II gas pycnometry system. Information brochure
• Quantachrome (2017). Gas Pycnometers. True density analysis of powders, foams and bulk solids. ©Quantachrome
Corporation 07171 Rev B 0217
• Scogings, A.J. (2015). Drilling grade barite. Supply, Demand & Market. Industrial Minerals Research, January 2015. 226 pp.
• Scogings, A. J. (2015). Bulk Density: neglected but essential. Industrial Minerals Magazine, April 2015, 60-62.
• Scogings, A.J. (2015). Bulk density of industrial minerals: Reporting in accordance with the 2007 SME guide. SME Mining
Engineering, July 2015 Web Exclusive. Society for Mining, Metallurgy & Exploration.
• Scogings, A. J. and Coombes, J. (2014). Quality Control and Public Reporting in Industrial Minerals. Industrial Minerals
Magazine, September 2014, 50-54.
• Verly, G., 2012. Geostatistical Mineral Resource / Ore Reserve Estimation and Meeting JORC Requirements: Step by step
from sampling to grade control. Course Notes, October 15-19, 2012. Perth WA, Australia. 2012 Professional Development
Seminar Series; The Australasian Institute of Mining and Metallurgy.
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Andrew Scogings CV
www.csaglobal.com
Andrew Scogings
PhD (Geology), MAIG, MAusIMM, RPGeo (Industrial Minerals)
Dr Scogings is a geologist with more than 25 years’ experience in industrial minerals exploration, product
development and sales management. Andrew has published papers on reporting requirements of the JORC
Code 2012, with specific reference to Table 1 and Clauses 18 and 19 (industrial mineral Exploration Results)
and Clause 49 (industrial mineral specifications). He has published numerous articles on industrial minerals in
Industrial Minerals Magazine, SEG Mining News, AIG News and AIG Journal amongst others; addressing
aspects of QA/QC, bulk density methods and petrography for industrial minerals exploration. He was recently
senior author of two significant reviews: Natural Graphite Report – strategic outlook to 2020 and Drilling
grade barite - Supply, Demand & Markets published in 2015 by Industrial Minerals Research (UK). He has co-
authored several papers on lithium pegmatites including: Reporting Exploration Results and Mineral
Resources for lithium mineralised pegmatites published during 2016 in the AIG Journal. Andrew is a
Registered Professional Geoscientist (RP Geo. Industrial Minerals) with the Australian Institute of
Geoscientists.