Trans Indian Inst Met (2016) 69(1):125–133
DOI 10.1007/s12666-015-0721-7
TECHNICAL PAPER
Quantitative Estimation of Mineral Phases from Chemical Assays
and Powder X-Ray Diffraction Rietveld Analysis: A Case Study
on Selective Flocculation of Iron Ore Slimes
Venugopal Tammishetti1 • Beena Rai1 • B. Ravikumar2 • Rakesh Kumar2
Pradip1
Received: 9 June 2015 / Accepted: 7 October 2015 / Published online: 23 November 2015
Ó The Indian Institute of Metals - IIM 2015
Abstract A generic method for quantitative estimation of
mineral phases in ores and process streams has been illus-
trated in this paper with the help of an example taken from
our own work on the selective flocculation of alumina rich
iron ore slimes. The method used conventional bulk
chemical assay data and information on phases present, as
determined by powder X-ray diffraction (XRD) pattern
analysis. Iron ore slime samples were subjected to selective
dispersion–flocculation experiments and the feed, concen-
trate and tails were analyzed using this method. Chemical
assays (iron, alumina, silica and loss on ignition) were
determined by wet chemical analysis and mineral phases
(hematite, goethite, gibbsite, kaolinite and quartz) were
quantified by Rietveld analysis of XRD patterns. Consid-
ering the proportion of various elements present in the
constituent minerals, the chemical assay data and the rec-
onciliation of assays (as well as the mineral compositions
determined by Rietveld analysis, if available), one could
estimate the proportion of various minerals present in dif-
ferent process streams. The mineral compositions estimated
based on this method matched reasonably well with those
obtained by quantitative phase analysis by the Rietveld
analysis. In case the Rietveld analysis results were also
reconciled with the elemental assays, one could arrive at
even a better estimate of the proportion of various minerals
in the different process streams. The estimated mineral
& Venugopal Tammishetti
venugopaltammishetti@gmail.com;
venugopal.tammishetti@tcs.com
1
Tata Research Development and Design Centre, Tata
Consultancy Services, Pune 411013, India
2
CSIR-National Metallurgical Laboratory, Jamshedpur
831007, India
•
compositions in feed, concentrate and tails were also used to
compute mineral wise recoveries. The approach presented
in this paper would provide mineral engineers a simple and
relatively easy method to convert elemental assays into
mineralogical compositions and thus compute extremely
useful and reliable estimates of the mineral-wise recoveries,
grades and distributions in the various plant streams, which
are necessary for plant optimization and control purposes.
Keywords Iron ore slimes  Mineral composition 
Powder X-ray diffraction  Rietveld analysis 
Data reconciliation
1 Introduction
Mineral processing plants are designed to separate minerals
but the optimization and control in the operating plants are
currently based on chemical assays. It is a well acknowl-
edged fact that different mineral phases comprising of the
same element may behave differently under similar process
conditions. Iron ore slimes for example, typically consist of
a variety of iron minerals such as hematite (Fe2O3), mag-
netite (Fe3O4) and goethite (FeOOH). As illustrated in this
paper, it is of great value to establish the conditions under
which each one of these minerals are separated. It is thus
important in general to track the partitioning of the con-
stituent minerals across various streams in order to optimize
the plant operations. In operating plants, while it is common
to measure elemental assays across various streams, it is
rare to measure and track flow of mineral constituents, since
petro-mineralogical analysis typically requires high level of
expertise and infrastructure. With the advent of automated
mineral analyzers (QEMSCAN, MLA, Clemex, TESCAN),
it has now become possible to determine mineralogical
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126
composition of various plant streams [1]. However, these
techniques are relatively expensive and time consuming,
thereby limiting their widespread application. Further lim-
itations are imposed when the particles are too fine to pre-
pare polished section and, mineral grains have similar
compositions (e.g. Fe2O3 and Fe3O4).
Banerjee and Mukherjee [2] have studied the liberation
characteristics of iron ore slime samples via automated
mineral analysis QEMSCAN and also attempted to gen-
erate grade-yield curve. Thella et al. [3] have used back
scattered electron image technique for identifying mineral
phases. These researchers have used energy dispersive
spectroscopy (EDS)–scanning electron microscopy (SEM)
for microanalysis and found that the characterization
becomes extremely complex with the poor liberation of the
minerals in the samples. SEM–EDS of iron ore samples by
Raghukumar et al. [4] shows observed coating of gibbsite
particles on iron bearing minerals in finer fractions thus
complicating the estimation of mineral compositions. Rao
et al. [5] have done qualitative mapping and quantitative
Electron Probe-Micro Analysis (EPMA) of iron ore sam-
ples. Their observation shows the presence of gibbsite
grains intimately and intricately along with iron oxides in
fine particle size range.
Another approach for quantitative estimation of mineral
phases present in a sample is based on the quantitative
X-ray diffraction analysis where mineral proportions can
be estimated using Rietveld refinement. The procedure
involves identification of mineral phases present in the
system followed by refinement of the recorded XRD pat-
tern against the calculated XRD patterns of the constituent
minerals. Once, the simulated XRD pattern matches with
the recorded pattern, then corresponding mineral propor-
tions are computed. However, whenever there are amor-
phous phases present in the samples, the procedure
becomes complex. Further, elemental substitutions in the
crystal lattice, crystallite size and their preferred orienta-
tion make the procedure increasingly more complex and
the quality of results is affected. There are reports in the
literature on the quantitative phase estimation in bauxite
[6–9], iron ore [10–13], clay minerals [14, 15], clinker and
cement additives such as slag and fly ash [16–18].
Ideally, there has to be a methodology by which one can
estimate mineral assays from elemental assays. Attempts
have been made in the past to estimate the mineral compo-
sition of a sample from chemical assay data. Whiten [19] has
recommended a procedure for calculating the mineral
composition from a given chemical assay based on the sin-
gular value decomposition (SVD) technique. Lund et al. [20]
have developed a tool to convert elemental assays to mineral
assays based on the solution of a set of linear algebraic
equations relating elemental assays to mineral compositions
and treating it as a constrained optimization problem.
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Trans Indian Inst Met (2016) 69(1):125–133
The conversion of elemental assays to mineral assays
based on stoichiometric formulae of each mineral (provided
one has identified all the minerals present in an ore) is in
principle a data reconciliation problem. It involves reconcil-
ing all the elemental assays as well as all the computed min-
eral assays across a node and/or across all nodes in a plant.
There are several algorithms available in literature to
carry out data reconciliation of plant data [21–27]. More
recently, Subramanian et al. [28] have proposed a concurrent
reconciliation methodology for estimation of mineral com-
position from chemical assay data for a single stream/sample
as well as for mineral processing circuits. In this paper, we
have used a methodology proposed by Subramanian et al.
[28] for reconciling simultaneously both elemental assay
and mineral assays for a given beneficiation circuit.
As part of an ongoing ambitious program to develop a
selective flocculation–flotation process for the beneficiation
of alumina-rich Indian iron ore slimes, attempts are being
made to establish the response of individual constituent
minerals to the different reagents being developed for
selective separation. Indian iron ore slimes typically con-
tain two iron minerals (hematite and goethite) and two
alumina minerals (gibbsite and kaolinite). The separation
efficiency is conventionally quantified based on chemical
assays such as %Fe, %Al2O3, %silica and loss on ignition
(LOI) present in the concentrates and tailings.
We have attempted a direct estimation of mineral assays
using Rietveld refinement of XRD patterns of various
products generated during the test work. The quantification
of phases by Rietveld refinement is complemented by
thermal analysis (TG/DTA). Thermal anslysis albeit limi-
tations arising due to overlapping peaks (e.g. gibbsite and
goethite DTA peaks appearing *300 °C [29, 30]), yields
weight loss data in specific temperature ranges for indirect
estimation of phase(s). A comparison of results on the
mineral assays estimated by different techniques are
reported in this paper. The results indicate that these esti-
mates are comparable and one can estimate the mineral
compositions from elemental assays only.
2 Materials and Methods
2.1 Iron Ore Slime Samples
The iron ore slime samples used in the study were obtained
from two different iron ore mines of India. The slime sam-
ples were of -400 mesh (-37 microns) size. Particle size
distributions of both these slime samples were similar
(Fig. 1). However, their chemical composition differed
significantly (Fe 42–59 %, Al2O3 7–16 %, SiO2 4–11 %,
LOI 5–9 %) indicating wide variation in mineralogical
makeup.
Trans Indian Inst Met (2016) 69(1):125–133
100
Size (µm)
Cumulative Weight%
80
D10
60
D50
D90
40
20
0 0
0 10 20 30
Diameter (µm)
Slime 1 Cumulative Weight%
Slime 1 Weight%
Fig. 1 Particle size analysis of slime samples
2.2 Dispersion–Flocculation Experiments
Iron ore slime slurry of desired pulp density was prepared
by dispersion of dry slime sample in 800 ml of distilled
water. The pH of the solution was adjusted to the desired
value (alkaline) while stirring it at 159 rpm using DBK
flocculator. The slurry was dispersed further by ultra-son-
ication for 5 min at 30 % amplitude using Branson Sonifier
(Model: 102C). The pH was re-adjusted, if there was any
change observed after ultra-sonication, and stirring was
continued at 100 rpm for 15 min. The slurry was floccu-
lated by addition of desired amount of flocculant (starch or
guar gum) and stirred at low speed (3 min at 40 rpm). The
stirring was stopped and the slurry was allowed to settle for
the required amount of time. At the end of the experiment,
the suspended portion was decanted from the flocculated
(settled) portion. Both suspended and settled portions were
dried in the oven and analyzed by wet chemical analysis.
The settled portions (concentrates) were labelled as C1–C5
and corresponding suspended fractions were designated as
tails. Figure 2 represents in a typical batch experiment a
node where feed is separated into concentrate and tails.
2.3 Phase Identification and Quantitative X-Ray
Diffraction Analysis
X-ray powder diffraction patterns were recorded on a
Bruker D8 Discover diffractometer under following
experimental conditions: diffractometer geometry—
Bragg–Brentano, radiation—CuKa, tube voltage/current—
40 kV/40 mA, detector—Lynx solid state, scan range
(2h)—10°–100°, step size—0.02°, counting time 3 s/point.
The powder iron ore samples after different processing
were mounted in a rectangular Perspex sample holder and
examined. Phase identification was carried out using
search–match technique. The major phases identified in the
slime sample included: hematite (Fe2O3), goethite
127
8 Feed Dispersion- flocculation Concentrate
7 experiment
Slime 1 Slime 2
6
1.7 1.3
5
Weight%
5.8 8.1
4 Tails
24.1 23.3
3
Fig. 2 Separation experiment (single node with concentrate and tails)
2
1
([FeO(OH)] or [Fe2O3H2O]), gibbsite ([Al(OH)3] or
40 50
[Al2O33H2O]), kaolinite (Al2O32SiO22H2O) and Quartz
(SiO2). TOPAZ, the software available with the diffrac-
Slime 2 Cumulative Weight%
Slime 2 Weight%
tometer was used for the quantification of phases based on
Rietveld analysis. The scheme of the quantitative estima-
tion of phases is shown in Fig. 3. The crystal information
files (cif files) for the identified phases were obtained from
COD open database [31]. The cif data used was for pure
phases under ambient conditions. The unit cell dimension
‘b’ obtained after Rietveld analysis was used for the esti-
mation of Al-substitution in goethite (i.e. (Fe1-xAlx)OOH)
[32].
2.4 Thermal Analysis
Thermogravimetric (TG) weight loss and differential
thermal analysis (DTA) plots were recorded from ambient
temperature to 1100 °C using a TA Instruments thermal
analyzer (Model SDT Q600). Approximately 25 mg sam-
ple was taken in all the cases. Samples were heated at
10 °C/min.
2.5 Chemical Analysis of Separated Fractions
The chemical analysis of separated fractions were carried
out by conventional chemical analysis methods [33]. Iron
and aluminum contents were determined in digested sam-
ples using atomic absorption spectroscopy (AAS). Silica
was estimated by standard acid insoluble method. The loss
on ignition (LOI) was determined by heating the sample at
850 °C for 1 h in muffle furnace. The results were
expressed in weight % of dried solid.
2.6 Estimation of Mineral Phases Using Chemical
Assay and Reconciliation
The computational method of mineral phase estimation
used in this paper is based on the method proposed by
Subramanian et al. [28]. The technique is based on the
premise that all the minerals present in the sample are
identified, minerals have a well-defined chemical formula
and the extents of elemental substitution, if any, are known.
This means that elemental and mass balance prevails at any
processing step (node). Schematic of the method of
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128
Fig. 3 Quantitative estimation
of phases using Rietveld 1 2
Data
analysis of powder diffraction
patterns
X-ray diffraction
pattern
cif File for identified
minerals
Fig. 4 Scheme for estimating
mineral proportions from Input
chemical assay using our
computational tool
• Flow Split (Optional)
• Chemical Assays
(Feed, Concentrate
and Tails)
• Minerals in the sample
• Substitutions (if any)
estimating mineral composition from chemical assay is
shown in Fig. 4. The input data include mass flow split,
chemical assays, mineral phases present in the sample and
substitutions present, if any. The mass flow split data is
optional however; wherever the stream flow data is avail-
able, those can be used as the inputs in order to get the
reconciled flows. The optimization algorithm developed by
Subramanian et al. [28] performs computations for error
minimization, reconciliation and mineral estimation.
3 Results and Discussions
3.1 Nature of Slime Sample
Figure 5 shows typical SEM micrographs of the slime
sample used in this study. Figure 5a is a general view
which gives an idea of the shape of particles and size
distribution. The X-ray micro-analysis using EDS detector
was carried out to understand the nature of liberation and
heterogeneity present. The points marked in Fig. 5b–d
were analyzed by X-ray micro-analysis and the results are
summarized in Table 1. The compositional variation is
observed across points which are only a few microns apart.
The analysis at different spots show the presence of all the
major elements (Fe, Al, Si, O) in all cases, thus, indicating
an intimate association of mineral grains and/or coating of
particles by finer particles and, possible inter-elemental
substitutions. Majority of the particles/spots analyzed are
iron rich as is expected, given that the hematite and goe-
thite are the major minerals present. In general, an inverse
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Trans Indian Inst Met (2016) 69(1):125–133
3 Analysis
Entry
Input raw data file Preliminary analysis
Evaluation checking Rietveld Refinements
and entry and final results
Computations Results
• Error Minimization • Reconciled Flow Splits
• Reconciliation • Reconciled Chemical assays
• Mineral Estimation • Mineral Composition
correlation between the amount of oxygen and iron is
observed. This may be the results of the presence of iron as
hematite (Fe2O3) and goethite (FeOOH); higher oxygen
possibly indicates the presence of greater amount of goe-
thite. Iron deficient Al–Si-rich particles are indicative of
the presence of kaolinite which is identified by powder
X-ray diffraction of the sample. Pure mineral grains of
quartz (SiO2) and gibbsite (Al(OH)3) are not found. This
may be due to small amounts of these phases vis-à-vis iron
minerals. The X-ray microanalysis results also highlights
the fact that image analysis based quantification of phases
using QEMSCAN or similar techniques may not be feasi-
ble for these kinds of slime samples.
3.2 Quantitative Estimation of Phases
Quantitative X-ray diffraction (QXRD) analysis involving
Rietveld refinement has been performed for a large number
of slime samples and the efficacy of the method has been
assessed. Typical phase analysis results for a slime sample
and corresponding concentrates generated after various
experiments are presented in Table 2. The Rietveld
refinement has assumed texture effect (in \00l[ direction)
for gibbsite. Strong effect of crystallite size is observed for
kaolinite and it has also been considered in the analysis.
Values of x [in goethite—(Fe1-xAlx)OOH] has been cal-
culated from lattice parameter bgoethite estimated during the
refinement. Table 3 shows the comparison of the results of
the chemical analysis of the samples calculated using
QXRD with wet chemical analysis of the samples. Con-
sidering the fact that minerals are assumed to be pure
Trans Indian Inst Met (2016) 69(1):125–133
Fig. 5 SEM micrographs showing typical morphology and size distribution (a) and distinct particles marked with spots subjected to X-ray
microanalysis (b–d)
(except goethite where Al substitution is considered), the
match is reasonable for Fe, Al and LOI. Discrepancy is
observed for silica, which may be due to the presence of
small amount, elemental substitutions in kaolinite and
possible omission of other silicate minerals which were not
identified by XRD. A number of minerals in iron ore are
characterized by the presence of chemically combined
water. Typically, goethite and gibbsite lose this water in
200–400 °C temperature range. Table 4 shows the total
weight loss up to 1000 °C and in the temperature range of
200–400 °C which has been estimated by thermogravi-
metric analysis and has been calculated based on QXRD
results. The match that is observed between experimentally
determined values and calculated values is in good agree-
ment which and further confirms reasonableness of quan-
titative estimation of phases by QXRD.
A number of minerals in iron ore contain chemically
combined water and exhibit characteristic thermal analysis
response [34]. Figure 6a, b show thermo-gravimetric (TG)
and differential thermal analysis (DTA) plots for the sam-
ples for which QXRD results are given in Table 2. Initial
small weight loss that is observed below 200 °C (*0.6 %
129
for Slime 1 and \0.3 % for the concentrate samples
(C1–C5)) essentially corresponds to adsorbed/physical
moisture. The DTA peaks at *275 and 310 °C are typical
of goethite and gibbsite, respectively and weight loss
between 200 and 400 °C is predominantly due to dehy-
droxylation of these minerals to hematite and boehmite [34,
35]. The weight loss above 600 °C accounts for\0.1 % and
the one observed between 400 and 600 °C may be assigned
to secondary dehydroxylation of boehmite [35] and
kaolinite [34]. Total weight loss up to 1000 °C and in the
temperature range of 200–400 °C has been estimated by
thermogravimetric analysis and is compared with weight
loss calculated on the basis of QXRD results (Table 4). As
evident from Table 4, the match observed between exper-
imentally determined values and calculated values is in
good agreement and confirms reasonableness of quantita-
tive estimation of phases by QXRD. It can also be observed
that the weight losses in the concentrate samples (C1–C5)
are lower as compared to the original slime (Slime 1); this
indicates removal of hydrous minerals from the Slime 1 and
their enrichment in tailing samples. QXRD results in
Table 2 also support this observation and amounts of
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130 Trans Indian Inst Met (2016) 69(1):125–133

Table 1 Summary spots X-micronalysis for typical slime particles F ¼CþT ð1Þ
Particles image Spots X-ray microanalysis (wt%) where, F, C and T are the flowrate/weight of the feed,
Fe O Al Si concentrate and tails, respectively.
The chemical assay balance for each of the stream can
Figure 5b 1 71.92 26.24 1.84 –
be written as below:
2 61.02 33.47 2.90 2.61
3 60.72 34.90 2.55 1.82 %Fe measured ¼ Fe contribution from
ð2aÞ
4 57.02 34.03 2.65 6.31 ðHematite þ GoethiteÞ
5 79.54a 18.25 1.24 0.97
%Al measured ¼ Al contribution from
6 66.06 31.80 2.14 – ð2bÞ
Average 66.05 29.78 2.22 2.93
ðGibbsite þ KaoliniteÞ
Figure 5c 1 64.68 29.17 4.55 1.59 %LOI measured ¼ LOI contribution from
2 77.86 22.14 – –
ðGoethite þ Gibbsite þ KaoliniteÞ
3 10.63 50.57 18.37 20.44
4 80.95 18.14 0.91
ð2cÞ
5 74.04 19.91 3.19 2.86 %Silica measured ¼ Silica contribution from
6 89.78 8.38 1.02 0.81
ð2dÞ
ðKaolinite þ QuartzÞ
Average 66.32 24.72 5.61 6.43
Figure 5d 1 8.02 53.15 18.49 20.33 The equations can be suitably modified to take into
2 74.97 15.61 5.32 4.10 consideration, elemental substitutions e.g. aluminium in
3 35.47 40.08 11.99 12.47 goethite. %Al is calculated from %Al2O3.
4 70.06 25.51 2.57 1.85 By solving the objective function to minimize the total
Average 47.13 33.59 9.59 9.69 error with constraints (all assays, mineral compositions are
a
positive and \100), a tool to obtain reconciled flows,
High value of Fe over stoichiometric iron content in Fe2O3 ([70 %)
assays and mineral compositions was developed by
may result during X-ray microanalysis since hydrous nature of min-
erals can not be taken into account Subramanian et al. [28]. We have employed this method to
estimate the mineral compositions in two sets of experi-
mental data (Tables 5a, 6a) obtained from laboratory scale
goethite, gibbsite and kaolinites are higher in the concen- selective dispersion–flocculation batch experiments on iron
trate samples as compared to the feed slime. The sample C4 ore slime sample. Using the information of weights and
shows weight losses which is next to Slime 1. This is not chemical assays, mineral phase compositions are predicted.
unexpected since amount of gibbsite in C4 is higher as It is important to note that our computations have assumed
compared to other concentrate samples. 11 % Al substitution in goethite, as observed by XRD
analysis. The predicted mineral phase compositions are
3.3 Reconciliation of Assay Data compared with those estimated using quantitative XRD
techniques in Tables 5b and 6b. It is evident from the
When a separation experiment is performed, the feed splits results that the estimation of quantitative mineral compo-
into two streams: concentrate and tails (Fig. 2). The overall sitions, based on chemical assay alone, match reasonably
mass/flow balance can be written as: well with the quantitative XRD results. It is also important

Table 2 QXRD results based on Rietveld refinement for a slime and corresponding concentrates generated after different treatments
Sample Phase (%) x
Hematite (Fe2O3) Goethite (Fe1-xAlx)OOH) Gibbsite (Al(OH)3) Kaolinite (Al2O32SiO22H2O) Quartz (SiO2)

Slime 1 64.7 28.9 3.0 3.3 0.0 0.117

C1 77.7 18.6 1.4 1.9 0.3 0.116
C2 75.0 18.0 2.2 2.1 2.8 0.113
C3 79.9 17.2 1.1 1.3 0.6 0.104
C4 73.5 18.5 3.2 1.9 2.9 0.105
C5 75.0 19.2 2.3 1.6 1.8 0.069
x—substitution of Al in goethite

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Trans Indian Inst Met (2016) 69(1):125–133 131

Table 3 Comparison of chemical assay results of standard method observed that quartz (undesired mineral) is also being
with calculated analysis based on QXRD recovered in the concentrate along with hematite (desired
Sample wt% mineral). We can observe that rejection of gibbsite and
kaolinite is better in the experiment 1 as compared to
%Fe %Al %LOI %Silica
experiment 2. It is interesting to note that goethite (desired
Slime 1 58.5 (61.3) 3.8 (3.3) 4.9 (4.6) 4.1 (1.5) mineral) is being rejected to tails in experiment 1, whereas,
C1 66.9 (64.7) 2.1 (1.9) 3.2 (2.8) 1.4 (1.3) no separation of goethite is observed in experiment 2. Thus
C2 65.6 (62.6) 1.4 (2.1) 3.5 (3.0) 0.9 (3.7) these results do point out that there is a need to further
C3 64.2 (65.6) 1.5 (1.4) 3.0 (2.4) 1.0 (1.2) improve the process conditions so as to recover goethite and
C4 66.5 (61.9) 2.4 (2.4) 3.8 (3.3) 1.4 (3.8) reject quartz in the beneficiation of these samples, in order
C5 67.4 (63.8) 1.3 (1.7) 3.1 (3.0) 0.8 (2.5) to improve recoveries. Goethite recovery will of course
result in the decrease in the grade of the final concentrate.
Numbers in brackets are calculated from the QXRD data

Table 4 Total weight loss and weight loss attributed to the thermal 4 Concluding Remarks
transformation of goethite and gibbsite as estimated by thermo-
gravimetric analysis and calculated based on QXRD analysis
Mineralogical assay provides useful information for
Sample Total weight loss Weight loss % (Goethite ? Gibbsite) assessing the efficiency of the mineral separation processes
(%) but we normally measure elemental assays of the various
QXRD TG 200–400 °C XRD phase streams. A number of techniques (QEMSCAN, Rietveld
analysisa (TG) analysis analysis etc.) are available currently for estimation of
Slime 4.6 5.1 3.0 4.1 mineralogical assays directly but not so easily accessible to
1 the plant operators. We have demonstrated in this paper
C1 2.8 3.3 2.2 2.5 that one can estimate the mineral composition of various
C2 3.0 3.3 2.3 2.7 streams in the plant from chemical elemental assays which
C3 2.4 3.1 2.1 2.2 are routinely measured in the plants. The proposed
C4 3.3 3.9 2.6 3.2 methodology of estimating mineral assays from elemental
C5 3.0 3.1 2.3 2.8 assays is generic even though it has been used in this paper
a
to estimate the composition of concentrate, tails and feed
Weight loss up to 850 °C
produced during the beneficiation of iron ore slimes. It is
also shown that in case one is using more than one tech-
to note that estimation of mineral phases in various process nique for measuring mineral compositions—for example
streams provide valuable insight about the efficiency of the (elemental assays and Rietveld analysis) or (elemental
process. For example, in both these experiments, it is assays and QEMSCAN) or all three, there is a need to

100
(a) (b)
Goehtite -> Hematite
Gibbsite -> Boehmite

1.2
dehydroxylaion
Kaolinite and

98
secondary

1.0
96
DTA, V/mg
TG (%)

94 0.8

Slime 1
92
Slime 1 C1 Slime 1
Slime 1 C2 0.6 Slime 1 C1
Slime 1 C3 Slime 1 C2
90 Slime 1 C4 Slime 1 C3
Slime 1 C5 Slime 1 C4
0.4
Slime 1 C5
88
0 200 400 600 800 1000 0 200 400 600 800 1000
o
Temperature, C
o Temperature, C

Fig. 6 a TG and b DTA plots for a slime and corresponding concentrates generated after different treatments

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132 Trans Indian Inst Met (2016) 69(1):125–133

Table 5 Results of separation experiment 1 (experimental conditions: pH 11.5, pulp density 1 %, sodium hexa-meta phosphate 30 ppm, poly
glutamic acid 1 ppm, settling time 5 min)
(a) Chemical assay
Sample Split Chemical assay (wt%)
Fe Al2O3 LOI Silica

Feed (Slime 1) 100.0 58.5 (61.3) 7.2 (6.2) 4.9 (4.6) 4.1 (1.6)
Concentrate 32.1 67.4 (63.8) 2.4 (3.2) 3.1 (3.0) 0.8 (2.5)
Tails 67.9 56.0 (58.3) 8.9 (7.0) 6.94 (5.3) 4.5 (4.5)
Recovery (%) 37.0 10.9 20.2 6.0
(b) A comparison of mineral compostions obtained using our method and QXRD
Mineral (wt%) Feed Concentrate Tails
Estimateda QXRD Estimated QXRD Recoveryb Estimated QXRD

Hematite 62.2 64.7 72.2 75 37.2 46.8 56.9

Goethite 30.2 29 25.7 19.2 27.3 37.3 31.8
Gibbsite 2.6 3.1 1.3 2.3 16.1 4.7 1.6
Kaolinite 4.4 3.3 0 1.6 0.1 11.2 9.6
Quartz 0.5 0 0.8 1.8 52.4 0 0

Numbers in the brackets are assays back calculated from the QXRD data
a
Estimated-mineral composition computed from elemental assays only [28]
b
Recoveries are calculated from the mineral proportions estimated using our method

Table 6 Results of separation experiment 2 (experimental conditions: pH 11.5, pulp density 11 %, no dispersant, corn starch 60 ppm, settling
time 5 min)
(a) Chemical assay
Sample Split Chemical assay (wt%)
Fe Al2O3 LOI Silica

Feed (Slime 2) 100.0 42 (44.7) 15.8 (15.5) 9.3 (7.9) 10.9 (12.9)
Concentrate 56.3 50.5 (51.9) 11.4 (10.6) 7.53 (6.5) 5.4 (8.8)
Tails 43.7 30.3 (43.3) 23.7 (15.9) 12.2 (8.1) 17.3 (14.2)
Recovery (%) 67.6 40.6 45.7 28.1
(b) A comparison of mineral compositions obtained using our method and QXRD
Mineral (wt%) Feed Concentrate Tails
Estimateda QXRD Estimated QXRD Recoveryb Estimated QXRD

Hematite 37.9 39 48.1 50 71.4 18.4 35.9

Goethite 32.4 32.8 32.7 30.3 56.8 31.9 34.2
Gibbsite 8.3 3.6 7.4 4.9 50.2 10 3.4
Kaolinite 21.1 21.8 11.5 11.2 30.7 39.6 23.1
Quartz 0.2 2.8 0.3 3.6 82.4 0 3.5

Numbers in the brackets are assays back calculated from the QXRD data
a
Estimated-mineral composition computed from elemental assays only [28]
b
Recoveries are calculated from the mineral proportions estimated by using our method

reconcile all these measurements. It is not recommended to only estimates the mineral compositions from elemental
use the data without reconciliation since it can lead to assays but also provides the reconciled data for further
misleading results. Methodology used in this paper not reliable diagnostics and process optimization.

123
Trans Indian Inst Met (2016) 69(1):125–133
Acknowledgments Authors would like to thank Dr. Subramanian
Subramanian, Principal Scientist, Tata Consultancy Services Ltd. for
his help in developing the data reconciliation program and Dr. Ansu J.
Kailath, CSIR-National Metallurgical Laboratory for helping in
thermal analysis. Authors also express their sincere gratitude to Mr.
K. Ananth Krishnan, CTO, Tata Consultancy Services Ltd., and Dr.
S. Srikanth, Director, CSIR-National Metallurgical Laboratory for
their support and encouragement during the course of this work.
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