Sample Preparation:

The important step in the total

process

Prepared by Lusi Mustika Sari 1

Sample Preparation
What is sample preparation?
Preparing the material of interest in such a
way that it can be measured in a
spectrometer or diffractometer

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Sample Preparation
Why is sample preparation required?
First and foremost to know what the
composition of the sample is.
Quality and quantity
Original material doesnt fit in a cup
E.g.rocks from a mine,
Solid material taken from an oven,
Sample is not homogeneous
E.g. powder with different particle sizes

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Sample Preparation
Accuracy is a key word in the analytical
world and it depends on:
Quality of the standards
Quality of the calibration
Reproducibility of the instrument
Sample preparation

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Sample Preparation
Type of samples:
Powders
Rock material
Solid material
Beads
Liquids
Chips

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Sample Preparation
Ways to prepare:
Grinding
Milling
Pressing
Fusion
Dissolving
Drying

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Sample Preparation
Presentation of the sample

Loose powder ( to be ground and pressed as it

contains various grain sizes )
Pressed powder
Solid material ( surface to be polished)
Bead ( can be measured directly)
Liquid

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Sample Preparation
Some theory:
Mineralogical effect
Particle size effect
Density of the material
Sample surface
Escape depth of the X-rays

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Sample Preparation
Mineralogical effect (also known as
metallurgical effect); One element present in
different phases giving different intensities for 1
element and therefore a wrong concentration.

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 Sample Preparation
Particle size effect

If e.g. the small particles contain much more Mg than the large
particles, and if there are more small particles on the analysis
surface, the measurement will show too much Mg.
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Sample preparation
Surface roughness:
A: represents the signal with infinite fine surface
B: represents the practical outcome
The longer the wavelength the more smooth the surface should
be
A surface roughness between 30 50 m is good enough for
the K-lines of elements below 13 (Al)

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Sample Preparation
Grinding and Pressing
Important parameters:
Quantity of the sample material
Grinding time
Type of additive used
Wet / Dry grinding
Pressure used
Time the pressure is on / Compacting time
( Dwelling time)

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Sample Preparation
Why grinding the material?
By using a grinder the particle size is reduced
in such a way that the particle size effect can
be neglected

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Sample Preparation
Influence of the particle size on the
intensity

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Sample Preparation
Grinding additives:
In general adding an additive will decrease
the grinding time and/or improve the
homogeneity of the final product.
The following additives are normally used:
Cellulose
Tetra Borate
Boric Acid

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Sample Preparation
Why pressing the material?
To make the sure the material is compact enough to get
good reliable results
To get rid of gas and air in the sample

Sample can either be pressed in an aluminium cup or in a

steel ring in case the sample has to be analysed in a
diffractometer / spectrometer combination

It is advised not to measure the

sample as loose powder as it will
negatively influence the analytical
result due to loss of intensity

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Sample Preparation
Additives for Pressing:
In general the binding aid will improve the
compactness of the sample
Example of materials used:
Wax
Strearate

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Sample Preparation
Effect of the binding aid on the intensity

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Sample Preparation
Sample presentation
Pressed powder; Cups and Rings

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Sample Preparation
Why fusion?
What is Fusion?
Fusion is in fact dissolving and oxidizing the sample in
borate at a temperature over 1000 C
Why making a bead?
A well established method for the majority of the
materials
A perfect bead will eliminate the mineralogical effect
A perfect bead will eliminate the particle size effect
A bead is less sensitive to moisture
A bead can be stored for a longer period without
much deterioration over time.

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Sample Preparation
Influences of additives on the fusion
temperature:
1000-1200 C (Tmp+2000C)
Li2B4O7 Tmp=9200C
LiBO2 Tmp=8450C
Na2B4O7 Tmp=7400C
The fusion temperature depends on:
Ratio Li/B
Ratio sample / additive
Grain size of sample and additive
Type of heater: Gas, Muffel oven, Induction

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Sample Preparation
Crucibles and casting dishes

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Sample Preparation
Important parameters in the fusion
process:
Fusion temperature
Cooling rate
Sample to Flux ratio
Condition of the crucible and casting dish
Type of oxidant ( some non oxidized elements
have to be oxidized prior to fusion)

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Sample Preparation
Perfect Crystallization

Stress
Insufficient material / too low temperature

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Sample Preparation
Overview of the possibilities to eliminate
the particle size and mineralogical
effect:
Particle size Mineralogical effect
reduction resolved? resolved?
Particle size reduction Yes No

Fusion Yes Yes

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Sample Preparation
Some examples:
Material Grinding Turning (lathe) Polishing
Iron, steel X X X
Copper, brass X X
Aluminium X X
Nickel alloys X X X
Zinc X X
Cobalt X X X
Titanium X X
Mg alloys X X
Tin X N.A.
Lead Pressing
Silicium X

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Sample Preparation

End of lesson

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