Kwame Nkrumah University of

Science & Technology, Kumasi, Ghana

MSE 256 Assaying

2 Credit Hours

Anthony Andrews (PhD)

Associate Professor
Department of Materials Engineering
Faculty of Mechanical and Chemical Engineering
College of Engineering
Website: www.anthonydrews.wordpress.com
Online Lectures: classroom.knust.edu.gh

Teaching Assistants: Ms Freda Quaye / Ms Mabel Agyare

 Course Objectives

• Understanding the methodology of proper metallurgical sampling

• Understanding fire assaying procedure

• Identification of ores types and selection of suitable reagents to

determine grade of ores using different assay methods

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 Learning Outcomes

• Conduct proper metallurgical sampling

• Select suitable reagents for fire assaying procedure

• Determine the grade of ores using different methods of assaying

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 Course Content
Week Topic
1 Introduction
2-4 Sampling
5-6 Fire assay, instrumental method analysis
7 Mid-semester exams
8 Analysis of gold ores
9-10 Wet Chemical Analysis - Bottle role test
11 Diagnostic leaching

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 Recommended Textbooks
• Bugbee, E. E. (1991) A textbook of fire assay, Legend Inc.,
USA

• Cochrane, G.W. (1977) Sampling Techniques, 3rd Edition,

Wiley Inc., USA

• Marsden, J. and House, I. (2006) The chemistry of gold

extraction, SME, Littleton

• Mendham, J. Denney, R. C. Barnes, J.D. and Thomas, M.J.K.

(2000) Vogel’s quantitative chemical analysis, 6th Edition,
Prentice Hall, USA

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 Forms of Assessment

Quizzes 15
Mid-Sem Exam 15
End of Semester Exam 70
Total 100

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 Definition of Assaying
• Assaying is defined as the quantitative estimation of metals in
ores and metallurgical products.

• Fire assaying is a quantitative determination of metals in ores and

metallurgical products by addition of dry reagents and application
of heat

• An ore is a mineral-bearing substance from which a metal, alloy

or metallic compound can be extracted at a profit
– Metalliferrous (valuable portion)
– Gangue (valueless portion)

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 Classification of Assaying
Assaying can be classified into three methods

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 Classification of Assaying
• Some assay methods are suitable for raw materials; others are
more appropriate for finished goods

• Silver is assayed by titration, gold by cupellation and platinum

by inductively coupled plasma optical emission spectroscopy
(ICP OES)

• The assay method under discussion is aimed only at measuring

gold

• Variations of fire assay can be used for other metals, however, in

most instances other analytical methods are preferred
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 Fire Assaying
• Fire Assay is essentially used as a technique for extracting gold from geological
sample.

• In this method, a pulverized mineral sample is dissolved using heat and fluxing
agents in a process called “crucible fusion”.

• Gold is extracted from the melted material using molten lead (Pb).

• Gold is then separated from lead in a secondary process called “cupellation”.

• The gold content of the precious metals collected is then determined, using a
variety of analytical techniques.

• The amount of gold in the solution is then back-calculated, to indicate the

amount present in the original sample
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 Assaying – Applications
• Soil samples Gold bars
• Grade control
• Ore beneficiation

Gold nugget

Exploration drill samples

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Tailings
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 Steps in Fire Assaying
1. Sub-sampling & Catch-weigh

2. Fluxing

3. Firing

4. Cooling & Separation

5. Cupellation

6. Parting & Dissolution

7. Analysis

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 Sampling
• Sampling is a procedure by
which some members of a
population are selected as
representative of the entire
population

• Sampling is a process of taking

a portion from a bulk of
material and using that portion
to represent the bulk of material

• The sub-group thus selected to

represent the whole population
is known as sample

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 Why Sampling?

• Convenience in size for

transportation and testing

100% examination of
• Obtain the desired information at
the smallest cost the total material is
not possible!!!
• Entire bulk may be inaccessible,
too massive or too dangerous to
deal with.

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Importance of Sampling in Mineral
Processing
• Assay analysis
• Moisture analysis – e.g. coal
• Size analysis
• Flow rates
• Characterization - density, mineralogical associations, etc
• Process control

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Fundamental Statistical Terminologies
Accuracy: - the correctness of measurement or closeness of a result
to its true or accepted value

Precision: - the closeness of data to other data that have been

obtained in exactly the same way

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Fundamental Statistical Terminologies
• Bias is the difference between the true value and the average of a
number of experimental values and hence is the same as the
systematic error

• The variance between repeated samples is a measure of precision

or reproducibility

Minimizing or
eliminating biases is
more important than
improving precision for
metallurgical accounting
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 Fundamental Statistical Terminologies
• Replicates: - samples of the same size that are carried through an
analysis in exactly the same way.

• Outlier: - an occasional result in replicate measurements that

obviously differs significantly from the rest of the results.

• Error: a measure of deviation of the observed or calculated value

from the true value

• Types of error – Random, Systematic and Gross

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 Random Error
• Caused by unknown and unpredictable changes in the experiment

• Examples: measuring instruments and environmental conditions

– electronic noise in the circuit of an electrical instrument
– irregular changes in the heat loss rate from a solar collector due to changes in
the wind.

• Precision is limited by random errors.

• Random error may be reduced by repeating the measurements.

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 Systematic Error
• Occur with measuring instruments
when the calibration of the instrument
is not known correctly.
– Instrument has linear response

• Two types of systematic errors

– Offset or zero setting error
– Multiplier or scale factor error

The accuracy of
measurements is often
reduced by systematic
errors
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 Gross Error
• Gross errors occur occasionally, are often large, and may cause a
result to be either high or low.

• Gross errors lead to outliers

• Generally the fault of the person using the instruments

• Gross errors can be avoided by using two suitable measures

1. Proper care should be taken in reading, recording and calculating data.
2. By increasing the number of experimenters

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