Exploring Sampling and Assaying - Umicore Precious Metals Refining

Exploring
Sampling and Assaying

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1l Aerial view of the
sampling department
in Hoboken
Umicore Precious Metals Refining’s
Sampling and Assaying
An experienced key player in the
non-ferrous recycling business,
committed to a tradition of
quality, reliability and respect for
the environment
Recyclability is a key feature of non-ferrous
metals - in fact they can be used over and
over again! Umicore Precious Metals Refining,
a business unit of Umicore, is a world market
leader in recycling complex materials containing
precious metals. It provides refining services to
an international customer base.
The plant near Antwerp is the world’s largest,
cleanest and most advanced precious metals
recycling unit.
It is designed to recover precious and other
non-ferrous metals from a wide range of
complex raw materials in an efficient and
environmentally friendly manner.
These materials mainly consist of industrial
by-products and secondary precious metal
bearing raw materials from sectors such
as electronics, photography and catalysts
(oil refining, petrochemical and automotive).
The Sampling and Laboratory Department is
a cornerstone in this business.
The important sampling facilities are situated
in Hoboken and Hanau. While Hoboken is
focused on the whole range of recyclables,
Hanau is mainly oriented on automotive
catalysts (production scrap and end-of-life
convertors) and refractory material.
The acquisition of the precious metals division
of PMG by Umicore has increased our sampling
capabilities.

Sampling and Assaying 3
Total Quality is the driving force to
enhance the overall performance of
our organisation
Our mission statement
• To produce representative samples, from
complex precious metal bearing materials,
that are used to determine the real metal
content of the customers’ material.
• To assay the quality samples in an accurate
and efficient manner within the agreed time
frame.
• To use reliable, certified procedures and
methods, in accordance with the ISO 9001
quality system.
• To strive to be recognised by our customers
as a model in quality and service for the
sampling and assaying of complex precious
metal bearing materials.
Our results
• The wide variety and complexity of incoming
materials such as electronic scrap, catalysts,
electrolytic slimes, etc., mean that sampling
and assaying are a key success factor in
determining the exact metal content and our
customers’ financial yield.
• The sampling department is the largest and
best equipped in the world.
• The in-house analytical lab with its state-ofthe-art
equipment is unrivalled in the field of
non-ferrous and precious metals assaying.
Our resources
• A highly qualified and skilled team, managed
in a professional way, in line with our quality
objectives and values.
• An ongoing concern to meet all requirements
in respect of accurate, precise and economically
justified sampling and assaying procedures.
• The in-house development of the sampling
process technology and analytical methodology
ensures a high degree of automation and
validated, robust processes.
Our processes
• Well-managed and continuously optimized.
• Continuous investment in first-class, dedicated
sampling and assaying processes and
procedures.
• A permanent commitment to strive for more
efficient processes with a higher degree of
automation.
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1l Sampling installation
for automotive catalysts
2&3l Sampling lines for
electronic scrap
Umicore Precious Metals Refining
continuously invests in first-class
dedicated processes
Process innovation is the key of the Umicore
Precious Metals Refining approach.
Processes are designed and developed on the
basis of customer needs and expectations in
order to fully satisfy and generate increasing
value for customers.
Umicore Precious Metals Refining devotes more
than 15% of its operating budget to this unrivalled
service.
Investment programmes in sampling &
laboratory in the range of € 10 million have
been approved and implemented over the last
five years.
This budget is used to obtain a more in-depth
process-knowledge in order to offer improved
sampling and assaying services, in which the
environmental, safety and human impact is
taken into account.
Sampling
Key drivers are maximizing automation, so that
human intervention is minimized and sampling
capacities for growing markets such as electronic
scrap and catalysts are increased.
The aim is increased flexibility combined with
greater efficiency and shorter lead times.
This results in the correct metal content being
identified and optimum precious metal yields
being generated.
Recent major investments:
• enhancing the sampling capacity for e-scrap:
two separate lines for both shredded and
unshredded electronic scrap;
• sampling equipment for automotive catalysts;
• mixing and sampling devices for
heterogeneous and/or wet residues with a
high precious metal content.
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The modern organisation and dimensions of the
sampling, and the use of the most advanced
equipment and best available technology, make
our sampling reliable, competitive and safe.
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1l Ceramic converters
2l Decanning of the
converters
3l Metallic converters
4l Shredderline for
metallic catalysts
Due to the wide range of materials, the
Decanning the first step in sampling and recycling of autocatalysts.
In order to further support the growth of its precious metals recycling business Umicore Precious Metals Refining has build out a network of collection and
pre-processing (decanning, shredding) facilities located in Belgium, France, Germany, the USA and Brazil. We can handle entire convertors or broken monolith.
Recyclable products
automotive catalysts
Ceramic converters
The strategy of Umicore Precious
Metals Refining to offer a high
standard, closed-loop solution
for automotive catalysts to the
automobile industry, as well as to
catalyst producers and collectors.
Recyclable products
automotive catalysts
Metallic Converters
A unique patented shredding and
sampling line for metallic catalysts
(Alzenau, Germany).
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Final sample
preparation
Final sample
preparation

5l End-of-life automotive
catalysts
6&7l Sampling
installation for
automotive
catalysts
8l Electronic scrap 9l Loading of shredder 10l Conveyer belt to
sampler
sampling capabilities within Umicore are
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Recyclable products
automotive catalysts
Automotive catalysts
In the Hoboken sampling division
we recently installed a complete
integrated line:
after removal of the magnetic
fraction (magnetic separator) and
inert fraction (non magnetics/inerts
removed manually), the material is
crushed and sampled (rotary
samplers) in two steps.
The Hanau Sampling can rely on an
impact crusher, several rotary tube
dividers and ball mill to generate
quality samples.
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Recyclable products
electronic scrap
Electronic scrap
There are two separate lines for
unshredded and pre-shredded
electronic scrap. In front of the line
for unshredded e-scrap, a four-axis
slow rotating knife mill is installed.
A vibrating feeder transfers the
product to a conveyor belt. The
shredded scrap passes through the
crosscut-type sampling unit.
The particle size of the primary
sample is reduced in a small
(four-axis slow rotating) knife mill.
A rotary sampler takes a sample for
incineration, in two stages.
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Final sample
preparation
Final sample
preparation

11l Industrial catalysts
from oil refining industry
12&13l Biconical sweeps
blender
14l Bullions 15l Casting of ingots 16l Drilling of sample bar
highly diversified as regards techniques
Recyclable products
from industry
Fine free-flowing
material
Sampling is performed by means
of double blending in biconical
blenders, followed by sampling
with rotary samplers.
Recyclable products
from industry
Metallic material
Depending on the physical aspect,
lot size or precious metals content,
the material will be melted partially
or entirely, in an induction furnace.
Dip sampling is done in the liquid
bath, in three steps. The sample
bars are drilled to destruction, the
drillings are milled, screened and
reduced to final quality samples.
Highly magnetic material will be
matted in oil fired furnaces.
A mobile emission spectrometer is
used for a quality check.
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Final sample
preparation
Final sample
preparation

17l Tankhouse slimes 18l Spear sampling 19l Mixer for wet products 20l Slags 21l Pan mill 22l Rotary sampler
nd procedures
By-products
from non-ferrous industry
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Wet material
To ensure that the sampling of
heterogeneous precious metals
residues is as representative as
possible, homogenisation by
mixing is recommended. According
to the characteristics of the
material, the lot will be dispatched
to the automatic spear sampling
device or the mixer for integral
homogenisation. After homogenisation,
a number of increments have
to be drawn. The homogenisation
and sampling equipment is also
suitable for fine, free-flowing
material, e.g. concentrates.
By-products
from non-ferrous industry
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Lumpy material
After primary sampling, carried
out manually or by means of a
payloader, the material is crushed
by a hammer mill. The amount is
then automatically sampled,
whereupon it is subject to
milling in a pan mill (further size
reduction).
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Final sample
preparation
Final sample
preparation

23l Final samples 24&25l Tema mill 26l Rotary splitter
Final sample
preparation
Final sample preparation
The operations are:
• determination of the moisture or
loss on ignition by drying or
calcination
• preparation of the quality samples
for chemical analysis.
The samples are ground/screened
to a powder using Tema mills
(vibrating disc/ring mill).
After final blending, a rotary
splitter is used to fill the sample
bags.
The samples are packaged in
envelopes and sealed:
• a set of samples is sent to the
customer, together with the
certificate;
• a set of samples is forwarded to
our own laboratory;
• a set of samples is kept as a
reserve (umpire).
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Laboratory

A rarely found wealth of experience
in precious metals assaying
The precious metal bearing materials entering Umicore’s flow sheet vary widely in origin, lot size and specifications.
This diversity gives that extra dimension to Umicore Precious Metals Refining’s expertise in precious metals chemistry,
further enhanced by the use of state-of-the-art equipment and methods, combined with conventional fire assay and
chemical procedures to obtain the most accurate results.
Collection of precious
metals in Pb or NiS by
fire-assay fusion.
Separation of precious
metals from Pb by
cupellation.
Dissolution of the Au,
Pt, Pd, (Rh) residue by
aqua regia (HBr/Br 2 )
and conditioning of
the solution for final
measurement.
Measurement
of traces of
precious metals by
Zeeman Graphite
Furnace Atomic
Absorption
Spectrometry
(ZGFAAS).
Dissolution of the
Ag-button by HNO 3
for parting (gravimetric
determination of
Au/Pd).
Automatic titration of
Ag by potentiometry.

Sampling and Assaying 5
4&5l Spark source Optical
Emission
Spectrometer
6l Sequential X-Ray
Fluorescence
Spectrometer
7l Inductively Coupled
Plasma Optical Emission
Spectrometer
Sampling and assaying:
unrivalled in industry
Laboratory
A key factor for the optimal processing of the
incoming materials, via Umicore Precious Metals
Refining’ production flow sheet is the lab’s readiness
to continuously invest in analytical research
and method improvement in order to enhance
its overall performance.
Recent major investments:
• sequential and simultaneous X-Ray
Fluorescence Spectrometers;
• Inductively Coupled Plasma Optical Emission
Spectrometers;
• simultaneous Spark source Optical Emission
Spectrometer;
• Laboratory Information and Management
System;
• high-temperature melting furnaces for
fire-assay work.
The up-to-date analytical equipment combined
with an integrated quality assurance system give
precise and accurate results within optimal lead
times.
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Explore our Sampling Process
and Laboratory

Sampling and Assaying 13
Continuously pushing back
the limits of wet chemistry
The variety and complex structure of Umicore Precious Metals Refining’s feed supplies pose a constant challenge to the limits of wet chemistry technology.
Umicore Precious Metals Refining’ assayers draw fully on their extensive wet chemistry experience to extract the maximum obtainable elements from the
most complex raw materials.
Vessels used for
microwave dissolution.
Measurement
of anions by Ion
Chromatography.
Fast decomposition
of samples in a
microwave furnace.
Electrogravimetry
of Cu.
Determination of
N-compounds.
Automatic titration for
the accurate
determination of
elements in high
concentration such
as Pb.
Analysis of dioxins
Separation and
concentration of
dioxins prior to
measurement.
Determination of
dioxins by Gas
Chromatography-
Mass Spectrometry
(GC-MS).

A combination of the most recent equip
expertise in spectrometry
A key asset of Umicore Precious Metals Refining’s assayers, is the ability to increase their assaying potential in terms of: number of samples analysed,
number of elements analysed, range of elements analysed, range of detection limits. Umicore Precious Metals Refining has extensive experience and
an excellent reputation in X-Ray Fluorescence Spectrometry for non-ferrous metallurgy applications. Two new-generation simultaneous and sequential X-Ray
spectrometers are continuously in operation of the laboratory, 24 hours a day, seven days a week.
Pyrosulphate fusion
of samples for
simultaneous analysis
of 14 elements.
Borax fusion of
samples for
simultaneous analysis
of 25 metals and
refractory elements.
Pelletized sample.
Glass beads.
Accurate determination
of elements (Cu, Se, Ir,
Ru, etc.) via X-Ray
measurement in
solutions.
Measurement by
X-Ray Fluorescence
Spectrometry.

Sampling and Assaying 15
ment and over 40 years of hands-on
Atomic Absorption Spectrometry
Atomic Absorption Spectrometry is used for the
analysis of prepared solutions. Three instruments
are in daily operation for this purpose. One of
them is equipped with a hydride system, and the
other two with a graphite furnace coupled with
Zeeman background correction, allowing detection
limits at the ppb level.
Optical Emission Spectrometry
Optical Emission Spectrometry is widely applied
for the assaying of samples at all stages of the
production process and for the final quality control
of refined metals. It plays an important role in the
rapid preliminary assays of precious metals in all
incoming materials and in the exchange of silver
in some raw materials such as electronic scrap.
Inductively Coupled Plasma
Atomic Emission Spectrometry
Both simultaneous and sequential Inductively
Coupled Plasma Atomic Emission Spectrometers
are available to measure a series of elements in
sample solutions or in combination with fireassay
for final determination of precious metals
or after microwave dissolution for base elements.
ZGFAAS for the
determination of trace
elements.
Metal Hydride System
combined with
AA-Spectrometry
for ultra trace
determination of
hydride-forming
elements such as
Se, Te, As, etc.
Preparation of
(metal) samples for
measurement by
Emission Spectrometry.
Simultaneous determination
of impurities in
metals by Emission
Spectrometry for
production control (Pbrefinery)
and quality
control of end products
(Ag, Au, Pb, In, etc.).
ICP plasma for
Emission Spectrometry.
Measurement by
ICP-OES instruments.

www.preciousmetals.umicore.com
n.v. Umicore s.a.
Precious Metals Refining
A. Greinerstraat 14
B-2660 Hoboken, Belgium
www.preciousmetals.umicore.com
Tel +32 3 821 7480
Fax +32 3 821 7807
e-mail: preciousmetals@umicore.com
VAT BE 401 574 852
Bank 210-0052900-87 - TRB 85382
Registered Office Broekstraat 31 Rue du Marais, B-1000 Brussels, Belgium
01/2005 - ENG - Printed on recycled paper