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Sampling Issues: Getting the right sample Dr. Rob Bowell SRK Consulting (UK)

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Page 1: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Sampling Issues:

Getting the right sample

Dr. Rob Bowell – SRK Consulting (UK)

Page 2: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Introduction

Geochemical and mineralogical

testwork requires validated, well

located samples that are

representative

Essential components in

characterization of mine waste

Starts with getting a good

sample!

What is a good sample?

Page 3: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

What to sample?

Depends on focus:

• Source

Waste rock, core, tailings, heap leach, pit walls, pit lake, tailings pond

• Pathway

Groundwater, surface water

• Receptor

Soil, sediment, water, plants, animal tissue/fluid

5/19/2014 3

Page 4: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Gaps in Predictive Knowledge

Sampling approach • Representation

• Heterogeneity

• Number of samples

Verification of data

Assessment of non-standard protocols

Application of field tests

Kinetic tests

Assessment of ecotoxicology

Page 5: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Approaches to Sampling

Spatial • Visual assessment

Numerical • Samples collected randomly

proportional to predicted waste production

Geological • Determine rock and alteration

types to determine

Statistical • Account for heterogeneity in

sampling set by determining number of samples required

• Apply Gy theorem to variation in sample parameters

Page 6: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Sampling: Two key issues for ARDML

0

10

20

30

40

50

60

70

80

90

100

0.010.1110100

Sieve Size (mm)

Pe

rce

nt

Fin

er

0-10 10-20 20-30 30-40 40-50

Representation

• Provide representative sampling

of system being assessed

• Complicated by heterogeneity

Heterogeneity approach

• Accept heterogeneity and complicate

QA-QC programs & sampling

• Eliminate through homogenization

Size fraction

• Silt fraction controls majority

of water movement

in most waste types.

Important to ensure

sample represents size fractions

Page 7: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Material Type Delineation

and Sample Selection

• Review of drill core logs and delineation of primary material types.

• Material defined by:

o Lithology e.g. quartz monzonite, breccia, andesite, limestone

o Alteration e.g. argillic, potassic, silica

o Oxidation - oxide, transitional (minor limited mainly to ore),

sulfide

o Metal grade – ore, marginal or low grade, mineralized waste,

non-mineralized waste, overburden

Page 8: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Use of Mine Site Information

Site knowledge

Geological – mining model of

site

Incorporate –

• Spatial distribution

• Material characteristics

• Geology

• Relationship to phases of

mining

Page 9: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Core Sample Collection

• Leapfrog 3D geological modeling software used to query mine model.

• Sample intervals representative of waste within pit shell.

• Includes samples within shell drawn 200 feet outside the proposed pit.

Page 10: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Example of Sample Matrix –

by material type Material Type Number of Samples

Andesite 4

Diabase 2

Sulfide waste 72

Transitional waste 13

Sulfide ore 26

Transitional ore 14

Oxide ore 1

Tailings 12

Historic tailings 2

TOTAL 146

Page 11: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Example using site specific

rock classification

Page 12: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Important: rock type and spatial

representativity

Page 13: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Compare samples to rock

geochemistry from exploration

Page 14: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Best Approach – a combination

Avg sulfur grade % % of deposit

Albite 0.02 0.14%

Actinolite Skarn 0.37 0.55%

Amphibolite 1.06 1.02%

Banded Iron Formation 5.17 0.05%

Biotite phlogopite 0.14 0.46%

CPX Actinolite Skarn 0.95 7.36%

CPX-skarn 1.19 16.66%

Diorite 3.52 0.13%

Dyke 0.43 0.15%

Granite 0.24 3.84%

Greenstone 0.16 0.22%

Marble 0.85 2.53%

Magnetite-skarn 0.55 16.48%

Quartz Phyllite 0.93 0.13%

Quartz 2.32 0.16%

Skarn 0.45 31.91%

Serpentinite skarn 0.65 8.29%

Tremolite skarn 0.22 1.53%

AVERAGE 0.62%

Page 15: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Field Assessment

Field mapping

Mineralogy

• Estimate sulfide/carbonate

minerals present

Field tests- the paste method

• Assessment of reactivity

• Useful screening method

Field analysis

Use data for screening & direct

laboratory work

Page 16: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Benefit of Field Assessment

• Rapid results

• Material characteristics to

explain chemical

heterogeneity in similar

materials

• Expand to undertake field

trails on “pilot scale waste

dumps”

• Test historic waste materials

versus freshly mined

materials

Page 17: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Analysis in the field

• No delay due to laboratory analysis

• Rapid turnaround of results to aid sampling

• Cost effective

• Measure parameters of environmental

concern

• Sulfur – indication of acid generation

• Ca+Mg – indication of acid buffering

(calcite-dolomite and Mg-rich silicates)

• Metals (Cu, Cr, Fe, Mn, Pb, Zn, Cd, Hg….)

• Metalloids (As, Sb, Mo, Se……..)

Portable XRF in Environmental

Geochemistry

Page 18: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Relate geochemistry to site conditions

• Use lithology but often lithologies can have

large differences due to alteration

• Obtain geochemical indices of high/low S

or metals – distinguish end points

for each lithology

Take Away Statement

Sample Selection

Page 19: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Environmental risk – liability due to

unprocessed ore or reactive waste

• But can we relate potential for metal

release or acid generation to total metal

content?

Rapid Risk

Assessment

Page 20: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Environmental risk – assess toxicity in terms of total metals such as in EU

contaminated land guidelines

• Assess metals in terms of Geochemical Abundance ie GAI >3 anomaly

• Total metal chemistry as an initial guide to metal toxicity

Toxicity evaluation

Ag Bi Cu Hg Mo Pb S Sb Se Zn

ppm ppm ppm ppm ppm ppm % ppm ppm ppm

AECA 0.07 0.2 60 0.085 1.2 14 0.04 0.2 0.1 70

GAI=0 0.105 0.3 90 0.1275 1.8 21 0.0525 0.3 0.075 105

GAI=1 0.21 0.6 180 0.255 3.6 42 0.105 0.6 0.15 210

GAI=2 0.42 1.2 360 0.51 7.2 84 0.21 1.2 0.3 420

GAI=3 0.84 2.4 720 1.02 14.4 168 0.42 2.4 0.6 840

GAI=4 1.68 4.8 1440 2.04 28.8 336 0.84 4.8 1.2 1680

GAI=5 3.36 9.6 2880 4.08 57.6 672 1.68 9.6 2.4 3360

Lithology GAI=6 6.72 19.2 5760 8.16 115.2 1344 3.36 19.2 4.8 6720

QMBS Avg 5.26 9.16 1101.15 3.10 20.00 2963.13 2.47 7.86 1.12 2697

SDev 4.06 7.66 1398.35 7.70 17.63 3787.40 1.55 13.25 0.94 2913

MV Avg 0.92 1.09 178.46 0.12 4.67 203.86 0.55 1.25 0.50 888

SDev 1.35 1.24 202.24 0.27 5.26 410.97 1.01 2.19 0.00 1313

QMS_Sul (Sil/Cly/Chl/Ser) 2.39 7.09 1110.00 0.24 29.60 187.00 5.00 6.70 2.00 4120

MBS_Sul (Sil/Chl(Ser)) 1.83 6.56 1110.00 0.21 34.40 179.00 5.00 6.67 2.00 3540

Overburden Avg 2.94 2.69 414.00 0.62 6.39 909.00 0.43 5.18 0.50 1360

SDev 3.27 2.24 408.71 0.66 5.96 963.08 0.11 4.94 0.00 495

Page 21: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Metal distribution across site:

Tsumeb, Namibia

Page 22: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Copper distribution

across Tsumeb district

TSF

Smelter

Tschudi

Tsumeb West

Page 23: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Representative sample

• Representative analysis

• Issues with penetration into the sample?

• Surface analysis- representative analysis?

• Mineralogy effects?

Major Issues

Page 24: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Cwmstywth mine,

mined from 1845 to 1928

• More than 4 Mt of mine waste

and tailings deposited

adjacent to Yswth river

• High levels of acid generation on site

from weathering of pyrite

and marcasite

• Some buffering from calcite

and dolomite

• Reported impacts of zinc, cadmium

and acidic pH in receiving water

Case Study: Cwmstywth mine,

Central Wales

Page 25: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Base metal mineralization associated with faults in Ordovician rocks

• 400 to 350 Ma, Caledonian orogeny

• Mineralogy is galena, sphalerite, chalcopyrite, arsenopyrite, with some pyrite

and marcasite within a quartz, barite and carbonate

• Geological oxidation in Tertiary to Recent, over 40 secondary minerals

Central Wales Orefield

Page 26: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Mined between 1600 and 1955 for Ag, Pb and Cu

• Predominantly underground

• Liability due to unprocessed ore, discharged

tailings or reactive mine waste, groundwater

rebound in underground mines

History of Central Wales Orefield

Page 27: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Hydrogeochemistry

Page 28: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Measures of potential

reactivity is paste pH

and paste EC

• Correlation in acidic pH

to leachable solids (EC)

• Potential to correlate

to XRF would allow

easier definition

of reactive mine waste

and define metals

of concern

and magnitude

Material Reactivity Geochemistry

Page 29: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Calibration of XRF instruments

Sample CY1-5

Sample CY1-7

Sample CY1-10

Sample CY1-11

Page 30: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

XRF Results Comparison

to Acid Generation Assessment

Page 31: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Comparison to leaching tests, Zinc

Page 32: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Risk Assessment Maps

Leachable Zinc from mine waste,

Contact test/ICP

Total Zinc in mine waste, XRF

Page 33: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Risk Assessment Maps

Total Arsenic in mine waste, XRF

Page 34: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

Abuse of portable XRF

in Environmental Studies

26.2% Pb

32% Pb

2.6% Pb

56% Pb

1.9% Pb

1 m

Abuse comes from:

• Utilising the internal calibration of the XRF unit and assuming these recorded

values as reportable – overcome by external calibration

• Matrix effects – overcome by destructive method to homogenize sample

• Bias in In-Situ analysis due to matrix effects- overcome by preparation of

samples

Page 35: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Mine Waste Studies

o Characterize mine waste geochemistry

o Define impacts to the environment

o Seek to define risk of impacts

o Define toxicity

• Conventional studies require careful selection

of representative samples for laboratory testing

• Portable XRF has potential to be integral

in achieving these goals BUT:

• Require good control over calibration

• Require good mineralogical understanding of material

• Avoid spurious results as a consequence

of selective analysis of In-situ material –

homogenize samples better than many in-situ results

Recommendations

Page 36: Sampling Issues: Getting the right sample · • Receptor Soil, sediment, water, plants, animal tissue/fluid 5/19/2014 3 . Gaps in Predictive Knowledge Sampling approach • Representation

• Good sampling is essential

in an ARDML study

• Requires knowledge of geology

and history of the site, mineralogy

and mining methods

• Needs to be representative

• Different sample medium to collect –

depends on focus of study

• Environmental Geochemistry Studies

benefit from Portable XRF

Summary