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Abstract Flotation is a separation process based on the collection of particles on the surface of
bubbles. Flotation machines disperse air into bubbles using a variety of techniques. The characteristics of
the bubble population are strongly affected by the selection of frother type and concentration. As
metallurgical results depend on the properties of the bubble swarm, the measurement of frother
concentration is vital to understand and control performance. A previously developed colorimetric
technique was refined to increase analysis rate and reproducibility, particularly for low-solubility frothers.
The refinements include new procedures for preparation of standards and samples, for constructing
calibration curves and for establishing the reproducibility and accuracy of the technique. The refined
technique has been demonstrated to be robust, reliable and accurate. The refinements are briefly discussed
and documented. This paper focuses on applications of the technique in operations such as determination
of frother remnant levels in recycle water, reliability of frother delivery and frother dissolution and in
support of research interests related to gas dispersion and characterization of frother partitioning.
Rsum La flottation est un procd de sparation bas sur la collecte de particules la surface des bulles.
Les appareils de flottation dispersent de lair sous forme de bulles au moyen de techniques varies. Les
caractristiques de la population de bulles sont fortement affectes par la slection du type de moussant et sa
concentration. Comme les rsultats mtallurgiques dpendent des proprits de lessaim de bulles, la mesure
de la concentration du moussant est vitale la comprhension et au contrle du rendement. On a raffin une
technique colorimtrique, dveloppe auparavant, pour augmenter la vitesse danalyse et la reproductibilit,
particulirement pour les moussants faible solubilit. Les raffinements incluent de nouvelles procdures
pour prparer les talons et les chantillons, pour construire les courbes de calibration et pour tablir la
reproductibilit et la prcision de la technique. On a dmontr que la technique raffine tait robuste, fiable
et prcise. On discute brivement des raffinements et on les documente. Cet article se concentre sur les
applications de la technique dans les oprations comme les niveaux du reste de moussant dans leau de
recyclage, la fiabilit de la livraison du moussant et de sa dissolution et sur le soutien des intrts de recherche
relis la dispersion de gaz et la caractrisation du partitionnement du moussant.
Keywords: Colorimetry, Frothers, Flotation, Frother analysis, Frother partitioning
INTRODUCTION
Measurement of gas dispersion parameters (gas velocity, gas
holdup and bubble size) has become a tool to characterize
industrial flotation cells, for example, establishing the
operating range and the relationship to metallurgical
performance [1,2]. Gas dispersion properties are affected by
frother concentration. Calculating frother concentration
from dosage in an operating plant is difficult due to factors
such as incomplete dissolution and unknown distribution
between pulp and froth. Several commercial frothers are
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Sample Chloroform
Dehydration reactions:
H2SO4
H+ + HSO4
Sulfuric acid
Chloroform
RCHOH + H+
RCH+ + H2O
Discarded chloroform
Discarded water
Sulfuric acid + Colour indicator
Boiling water
(15 min)
Ice bath
UV absorbance measurement
Fig. 1. A schematic of the procedure for colorimetric analysis of frothers.
Wavelength, A
Fig. 2. Effect of water source on absorbance spectra of 10 ppm standard.
ANALYSIS REFINEMENTS
The application of the frother analysis technique in plant
demonstrated that improvements were required. Some
variability between operators was noted and reproducibility
was poor for low solubility frothers. A systematic tracking of
error sources produced new procedures in two areas,
preparation of samples and standards and construction of
calibration curves that significantly improved reliability.
Preparation of Samples and Standards
Stock Solution: The preparation of frother solutions with
concentrations in the ppm range involves the precise
weighing of a few mg of a viscous liquid. The original
procedure called for a stock solution, 1 L at 500 ppm, to be
used to prepare the standards by dilution. The preparation of
stock solution was changed from volume-based to massbased and to a larger and more dilute solution (2L, 25 ppm).
The lower concentration facilitated complete dissolution in
the case of low solubility frothers. The preparation considers
weighing drop by drop to have close to but less than the 50
mg of frother required and then adding the weight of water
calculated for a 25 ppm solution.
Choice of Water: Analysis of plant samples presents a
challenge in deciding what water to use in the preparations of
standards as water quality affects the colour (and absorbance).
In plants there are normally two sources of water: tap (potable)
and process waters. The first step in the analysis, extraction of
the frother into an organic layer of chloroform was expected to
be independent of inorganic contaminants. Experience
demonstrated, however, that components other than frother in
the process water are also apparently extracted and affect the
absorbance of the final solution. This is illustrated in Figure 2,
which compares UV absorbance spectra for a 10 ppm solution
of a frother prepared using tap and process waters.
Process water seems the better option but this water
often contains varying levels of remnant frother. The frother
residual concentration can be estimated by comparing
Absorbance
Process water
Tap water
Process water
Absorbance
Fig. 3. Calibration curves obtained in tap and process water
Concentration, ppm
Tap water
391
y = 93.2x + 0.4
y = 22.5x + 0.0
Frother
Collector
Absorbance
Fig. 4. Calibration curves in tap water for the combination frother/collector
in use at a concentrator.
392
y = 9.16x + 0.53
474 A
528 A
Absorbance
Fig. 5. Calibration curves obtained at different wavelength.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Average
95% C.I. range
Stock 1
Stock 2
Stock 3
Stock 4
Stock 5
Average
1.561
1.539
1.546
1.531
1.562
1.548
0.019
1.609
1.645
1.626
1.611
1.641
1.626
0.024
1.600
1.644
1.611
1.627
1.601
1.617
0.027
1.613
1.625
1.632
1.617
1.609
1.619
0.013
1.589
1.610
1.596
1.580
1.621
1.599
0.023
1.594
1.613
1.602
1.593
1.607
-
0.030
0.062
0.049
0.055
0.042
-
Frother Delivery
Gas Holdup, %
Day 1
Day 2
393
Day 1
Day 2
Day 3
Day 4
Time
Fig. 8: Frother concentration measured in a cell over time.
Canadian MetallurgiCal Quarterly, Vol 49, no 4
394
Tail samples
Concentration, ppm
Concentrate samples
Circuit
Cell
Fig. 9. Frother concentration profile measured in a nine-cell bank.
CONCLUSIONS
The colorimetric technique for frother analysis in industrial
streams was refined to increase analysis rate and
reproducibility, particularly for low solubility frothers. The
refinements include procedures for preparation of standards
and samples and constructing calibration curves. The refined
technique proved to be reproducible and accurate in both
laboratory and plant environments.
Examples from plant experiences illustrate uses in
tracking variations in frother feed between cells and circuits
and partitioning between pulp and froth. The technique is
becoming integrated into flotation characterization and
diagnostic work.
ACKNOWLEDGEMENTS
Tail samples
Concentration, ppm
Concentrate samples
Roughers
Cleaners
REFERENCES
Cleaner Scavengers
Circuit
Fig. 10. Frother partitioning in different circuits.
1.
2.
3.
4.
5.
6.
7.
8.
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