भारत सरकार /Government of India

परमाणु ऊर्जा विभाग /Department of Atomic Energy

परमाणु खनिज अन्वेषण एवं अनुसंधान निदे शालय
Atomic Minerals Directorate for Exploration and Research

है दराबाद/Hyderabad-500016
संख्या/No.AMD/MPU/gvsu/FS-19-20/AR दिनांक/ Date December 18, 2020

वार्षिक रिपोर्ट 2019-2020

Annual Report 2019-2020
महोदय
खनिज प्रक्रमण इकाई में किये गये कार्य में जुड़ा हुआ हूं एवं वार्षिक रिपोर्ट 2019-2020 प्रस्तुत

कर रहा हूँ।
Sir,
I have associated in Mineral Processing Unit, RMRE Group and the “Annual Report of 2019-
2020” (November 2019 to October 2020) is submitted herewith for your kind perusal
(Assignment Code 1319400)..

Yours faithfully,

(जी.वी.एस.उमामहे श्वर राव/G.V.S.Umamaheswara Rao)

वैज्ञानिक अधिकारी डी /Scientific Officer ‘E’
Submitted to:

निदे शक, प.ख.नि/प.ऊ.वि., है दराबाद/ Director, AMD/DAE, Hyderabad-500016.

प्रतिलिपि/Copy to:
1. अपर निदे शक (अ एवं वि), प.ख.नि., है दराबाद/ Additional Director (R&D), AMD, Hyderabad.

2. प्रधान, विरल धातु एवं विरल मद

ृ ा वर्ग, प.ख.नि., है दराबाद / Head, RMRE Group, AMD, Hyderabad.

3. प्रभारी, खनिज प्रक्रमण इकाई, प.ख.नि., है दराबाद/ Incharge, Mineral Processing Unit, AMD,
Hyderabad

(जी.वी.एस.उमामहे श्वर
राव/G.V.S.Umamaheswara Rao)
वैज्ञानिक अधिकारी डी /Scientific Officer ‘E’

1
 भारत सरकार /Government of India
परमाणु ऊर्जा विभाग /Department of Atomic Energy
परमाणु खनिज अन्वेषण एवं अनुसंधान निदे शालय
Atomic Minerals Directorate for Exploration and Research

वार्षिक रिपोर्ट 2019-20

ANNUAL REPORT 2019-20
(November 2019 to October 2020)
खनिज प्रसंस्करण इकाई
MINERAL PROCESSING UNIT
विरल धातु एवं विरल मद
ृ ा वर्ग
RARE METAL AND RARE EARTH GROUP

ASSIGNMENT Nos. 4.1 & 4.2 (Code 1319400)

Jaw Crusher Flotation Cell

Wet Low Hot acid agitation leaching

Intensity
Magnetic
Separator
G.V.S. UMAMAHESWARA RAO SO/E
P. SHIVARAM SO/G, I/C, Mineral Processing Unit

2
दिसंबर DECEMBER 2020 है दराबाद
HYDERABAD
असैन्में ट सं./Assignment No. 4.1:
Physical beneficiation and hydrometallurgical investigations of samples received from
Regions: (Target: 1 sample; Achievement: 1).
STUDIES ON SAMPLES RECEIVED FROM NORTHRN REGION (n=1).
1. Composite Core sample from BH No.NKT-2 to NKT-33 Naktu area, Sonbhadra dist.,
U.P. (n=1).

असैन्में ट सं./Assignment No. 4.2:

Laboratory investigations on samples received from RMRE and BSOI Groups:
(Target: 1 sample; Achievement: 10).
STUDIES ON SAMPLES RECEIVED FROM RMRE GROUP, WR (n=7) & SR (n=3).

1. Core samples- BH No.AMB-31, Ambadongar area, Chhota Udepur dt, Gujarat, WR (n=5).
2. Bulk composite core sample, Bhatikhera area, Barmer district, Rajasthan, WR (n=1).
3. Mine dump samples of Silicified Sovite Carbonatite, Ambadongar, Gujarat, WR (n=1).
4. Grab samples of Pegmatite, Amreshwar area, Raichur dist., Karnataka, SR (n=3).

R & D Assignment:
Assignment No. 22 (3319022) (Lithium extraction from Brines):
Brine samples from Pachpadra Salt Lake area, Barmer district, Rajasthan for beneficiation
studies for extraction of Lithium (n=4)
Assignment No. 24 (3319024) (Coal ash dump samples for uranium recovery)
Coal ash dumps samples from Thermal power plants- Kothagudem Thermal Power Plants and
Nava-Bharath Power Plants, Palvancha area, Bhadradri-Kothagudem district, Telangana (n=5).

3
 HIGHLIGHTS
1. NAKTU AREA, SONBHADRA Dt., UTTAR PRADESH
Composite Core sample from BH No.NKT-2 to NKT-33 (Feed Assay: 0.032% U3O8).
 The conventional hot acid agitation leaching on magnetic fraction (0.14% U3O8)
indicated 96.5% U3O8 leachability using 36 kg/t H2SO4 at 400C temperature in 6 hours
contact time. However, the composite core sample as a whole (ROM feed sample)
indicated 98.45% U3O8 leachability using 29 kg/t H2SO4.
 Leach liquor characterisation studies indicated low values of phosphate ion (0.02 g/L)
which do not affect uranium adsorption by ion-exchange resin (desirable phosphate
conc. is <0.1 g/L in leach liquor). Leach liquor also constitutes low values of transition
element ions i.e. V, Fe2+, Ni, Zn.
 Petrological studies indicated uraninite as the main uranium ore mineral.
2. AMBADONGAR AREA, CHHOTA UDEPUR Dt., GUJARAT
Bulk core sample BH No. AMB-31/2 (Feed assay: 3.70%TREE, 703 ppm Nb)
 Beneficiation studies to enrich REE & Nb by alkali scrubbing (NaOH agitation) & acid
treatment for separation of carbonate gangue and followed by magnetic separation of
the residue indicated marginal increase in grade to 5.13% TREE compared to
3.70%TREE in the feed sample, besides recovery of Nb values in 31%wt. magnetic
fraction with an increase in grade to 1437 ppm Nb compared to 703ppm in feed sample.
3. BHATIKHERA AREA, BARMER Dt., RAJASTHAN
Composite core sample-micro-granite-Feed Assay: 0.27% TREE, 0.08%Y, 0.037% Nb.
 Hot acid agitation leaching (-60#) indicated 47% TREE leachability at 700C
temperature, 24 hours contact time using 180 kg H2SO4/t.
 Wet high intensity magnetic separation indicated recovery of 72% TREE, 60%Y and
63% Nb values in magnetic fraction (40% weight) with marginal increase in grade to
0.45% TREE.
4. Mine dump, GMDC Mine, Ambadongar, Gujarat (Silicified Sovite Carbonatite).
 Feed assay: 0.53% TREE, 110 ppm Y & 470 ppm Nb. Static bed leaching on –60# feed
using 288 Kg H2SO4/t as leachant & 100 Kg K2S2O8/t as oxidant at ambient temperature
for 5 days indicated maximum leachability of 19.5% TREE.
5. PACHPADRA SALT LAKE AREA, BARMER Dt., RAJASTHAN:

4
  Evaporation-concentration experiments on brine samples from Pachpadra salt lake area
indicated 3.7 times enrichment of Li (from 25 ppm to 93 ppm).

असैन्में ट सं./Assignment No. 4.1:

भौतिक सज्जीकरण /जलधातुकार्य अभिलक्षण अध्ययन/ Physical beneficiation and

hydrometallurgical investigations of samples received from Regions:

STUDIES ON SAMPLES RECEIVED FROM NORTHERN REGION, (n=1)

Composite Borehole Core samples from Naktu area (NKT-2 to NKT-33), Sonbhadra dist.,
Uttar Pradesh, Northern Region.
A Composite core sample of boreholes NKT-2 to NKT-33 comprising of Migmatite Mobilizate
Complex and Pegmatoid Leucosome Mobilizate from Naktu area, Sonbhadra District, Uttar
Pradesh with average grade of 0.031% eU3O8 was received for leachability studies during the
year 2018-19. In continuation to the earlier studies, in which the composite core sample as a
whole assaying 0.032% U3O8 (ROM feed sample) indicated 98.45% U3O8 leachability using 29
kg/t H2SO4, the present study (2019-20) was carried out to find the leachability of uranium from
the beneficiated products.

i) Hot acid agitation leaching on Beneficiated products (Magnetic fraction):

In order to recover the trapped magnetic particles in the non-magnetic fraction and also to
obtain clean non-magnetic bearing product, wet high intensity magnetic separation (WHIMS) of
the feed sample (-60#) at 6 amperes followed by recycling of non-magnetic product
(scavenging/cleaning- two times) at 6 amperes was carried out. The products were chemically
analysed for U3O8, TREE & Y. The details are given in table-1.

Table 1 - Wet High Intensity Magnetic Separation (WHIMS)on -60#

S.No TREE %
Product %Wt. % U3O8 % Dist. Y ppm % Dist
. ppm Dist.
1 Mags at 6 A 23.02 0.145 86.29 1002 78.03 75 71.51
Non-mags at
2 76.98 0.0069 13.71 84.4 21.97 9 28.49
6A
Total 100.00 0.038 100.00 295 100 24 100.00

The test indicated 86% recovery of U3O8 values in 23%wt. magnetic fraction with an increase in
grade from 0.038 to 0.145% U3O8. The magnetic separation on the feed sample (-60#) has
shown preferential association and distribution of uranium values with magnetic fraction
indicating the feasibility of this method for enriching uranium values.

5
 Hot acid agitation leaching test on the above magnetic fraction having enriched grade (23% by
weight, 0.14% U3O8) was carried out. The test indicated 96.5% U3O8 leachability consuming
36 kg/t H2SO4 at 1.8 pH, 400C temperature, 18 kg MnO2/t as oxidant, 50% solids pulp density in
6 hours contact time. The details are given in Table-2.

Table – 2 Conventional hot acid agitation leaching of magnetic fraction

MOG- -60# 6A magnetic fraction , Agitation time: 6h, Pulp density: 50% solids, Temp: 400C
Product %Wt. U3O8 analysed H2SO4 consumed w.r.t % U3O8 leachability
in leach liquor magnetic fraction (23% wt.) w.r.t. mag. fraction
Mags at 6 A 23.00 690 mg/L 36 kg/t 96.5%

The above study shows that magnetic fraction has responded to conventional hot acid agitation
leaching with 96.5% uranium leachability.
ii) Heavy media separation of magnetic and non-magnetic fractions:
In order to know the association of uranium values with magnetic/ non-magnetic heavy and light
mineral, the representative -60# feed sample was subjected to wet high intensity magnetic
separation at 6A. The details are given in table-3.
Table 3 Summary of Wet High Intensity Magnetic Separation (WHIMS) -60#
S.No Product %Wt. % U3O8 % Dist. Y ppm % Dist.
.
1 Mags at 6 A 10.90 0.159 68.00 103 47.57
(including ferromags)
2 Non-mags at 6A 89.10 0.009 32.00 14 52.43
Total 100.00 0.025 100.00 24 100.00

The obtained magnetic fraction (10.90% wt.) and non-magnetic fraction (89.10%wt.) were
further subjected to heavy mineral separation using bromoform.
The test indicated 4.10% by weight of magnetic bromo heavy minerals and 6.80% by weight of
magnetic bromo lights. Traces of heavy minerals were obtained in the non-magnetic bromo
lights fraction (89.10% wt.). This shows that, in the case of non-magnetic products, the uranium
values (around 90 ppm reported) are associated with lighter fraction; hence, gravity separation
technique may not be useful to recover the associated values. The magnetic and non-magnetic
fractions were sent to Petrology laboratory for mineralogical studies to know the uranium
minerals associated with the magnetic and non-magnetic fractions. The Petrological studies
indicated the presence of:-
 Uraninite as the main radioactive mineral present in magnetic bromo-heavies and
magnetic bromo-lights fraction.

6
  Zircon is present in non-magnetic fraction.

 The other minerals present in magnetic bromo-lights and non-magnetic fraction are
quartz, plagioclase, microcline, biotite, chlorite, calcite and pyrite.

Photomicrographs showing different minerals associated with mag & non-mag fractions

AE RMRE 995 AE RMRE 996 AE RMRE 997

Bromo-heavies(mag.) Bromo-lights(mag.) Non-magnetic

Zircon
Uraninite with alpha tracks Uraninite with alpha tracks

Zircon chlorite
Biotite

orthoclase

Calcite

Allanite

iii) Leach liquor characterisation studies.

The leach liquor obtained by conventional hot acid agitation leaching carried out on -60# feed (>
90% uranium leachability) was chemically analysed for Ca, Mg, Na, K, SiO 2, P2O5, Pb, V, Zn,
Cu, Fe3+,Fe2+, SO4- and TDS. The details are given in Table 4.
Table - 4 Leach liquor analysis (values in ppm)
U3O SiO2 Fe2 Fe3 Ca Mg Na K Pb V Zn Cu Ni P2O %SO %TD

7
 8
+ +
5 4 S
157 51 12 25 <1 <1 <1 <1 <1 <1
200 <20 839 21 1.14 2.41
5 9 6 9 0 0 0 0 0 0

The chemical analysis indicates that the leach liquor constitutes low values of transition
element ions i.e. V, Fe2+, Ni, Zn. Further low values of phosphate ion (0.02 g/L) are also
observed which will not affect uranium adsorption by ion-exchange resin as the desirable
phosphate conc. is <0.1 g/L in leach liquor, thus beneficial in downstream operations.

iv) Process Flow-sheet:

The process flow-sheet for recovery of uranium from ROM feed and beneficiated magnetic
fraction are given below.

PROCESS FLOWSHEET FOR RECOVERY OF URANIUM

FROM URANIUM ORE (ROM) NAKTU AREA, SONBHADRA DIST., UTTAR PRADESH

ROM U3O8 - 320 PPM

(Migmatite Mobilizate Complex and Pegmatoid Leucosome Mobilizate)

CRUSHING (Rolls crusher)

GRINDING (Ball Mill)

-60 # (50% -200#)

HOT AGITATION LEACHING

28.8 KG H2SO4/T, 20 KG MnO2/T, 6 Hrs. CONTACT TIME,
500C TEMP., 50% P.D. (SOLIDS)

SOLID-LIQUID SEPARATION

RESIDUE LEACH LIQUOR

(<10 PPM U3O8) (147 -152 mg/l U3O8)
98% U3O8 LEACHABILITY

8
 PROCESS FLOWSHEET FOR RECOVERY OF URANIUM FROM
MAGNETIC FRACTION OF ORE, NAKTU AREA, SONBHADRA DIST., UTTAR PRADESH

ROM feed sample- U3O8 - 320 PPM

(Migmatite Mobilizate Complex and Pegmatoid Leucosome Mobilizate)

Crushing - Rolls crusher & grinding - Ball Mill up to -60# size

Wet High Intensity Magnetic Separation WHIMS (6 A)

(with scavenging/cleaning- two times)

Magnetic product at 6 Ampere Non-magnetic product at 6 Ampere

23% weight 77% weight
Assay: 0.145%U3O8, Distribution: 86% Assay: 0.007%U3O8, Distribution: 14%
(3.8 times enrichment)

HOT AGITATION LEACHING

36 Kg H2SO4/T, 18 Kg MnO2/T, 6 Hrs. Contact time,

400C Temp., 50% P.D.(Solids) w.r.t. magnetic product

SOLID-LIQUID SEPARATION

Residue
Leach Liquor (690 mg/l U3O8)
(<10 PPM U3O8)
96% U3O8 LEACHABILITY

9
असैन्में ट सं./Assignment No. 4.2:

भौतिक सज्जीकरण /जलधातकु ार्य अभिलक्षण अध्ययन/ Laboratory investigations on samples

received from RMRE and BSOI Groups:

STUDIES ON SAMPLES RECEIVED FROM RMRE GROUP WESTERN REGION, JAIPUR

1. Bulk core samples (BH No. AMB-31/1&2), Ambadongar, Chhota Udepur district,
Gujarat (Feed assay: (1) 2.45%TREE, 959 ppm Nb; (2) 3.70%TREE, 703 ppm Nb,).

The laboratory investigations on the core samples from Ambadongar area was partially carried
out during the year 2018-19 where-in a maximum leachability obtained was 30% of TREE & Nb,
with high acid consumption of 1260 kg/t H2SO4. During the present Annual Programme 2019-20
Beneficiation studies were continued to enrich the grade of REE & Nb values. The details of
studies carried out are given below.

I. PHYSICAL BENEFICIATION STUDIES:

A) Specific gravity determination
Specific gravity of the five bulk core samples (AMB-31/1 to 5) was determined on the
representative feed samples crushed to -100#. The Sp. Gravity ranges from 2.62 to 3.20.
Table 5- Sp. gr. of feed samples
Sample No./ Rock type Average Sp. gravity
AMB-31/1 Ankeritic carbonatite 3.10
AMB-31/2 Ankeritic carbonatite 3.20
AMB-31/3 Ankeritic carbonatite/Fractured fenite&Sovite 3.13
AMB-31/4 Ankeritic carbonatite/Fractured fenite&Sovite 2.85
AMB-31/5 Ankeritic carbonatite 2.62

B) Beneficiation studies to enrich REE & Nb

In order to separate carbonate gangue minerals and to enrich the grade of RMRE minerals, the
following experiments were carried out.
i) NaOH Agitation followed by magnetic separation of -100# feed, (AMB-31/1 Feed assay:
2.45%TREE, 959 ppm Nb)
Alkali agitation using NaOH for 6 hours (to solubilise carbonate minerals) followed by wet high
intensity magnetic separation (WHIMS) of residue (sand) at 6A was carried out on sample no
AMB-31/1 to enrich the grade of REE values. The test was carried out with 20% NaOH slurry

10
 at ambient temperature (26-280C) to solubilise carbonate matter. The details are given in Table
6 & 6A.

Table 6 - Wet high intensity magnetic separation of -100# feed (AMB-31/1)

Sl.No Product %Weight % TREE % Dist. %Y %Dist. %Nb %Dist.
1 Sand/6 A Mag. 1 40.00 2.05 36.31 0.017 33.17 0.105 55.82
2 Sand/6 A Mag. 2 10.50 2.35 10.90 0.018 9.00 0.074 10.29
3 Sand/6 A Mag. 3 6.10 2.42 6.52 0.020 5.89 0.063 5.13
4 Sand/6 A Non Mag 43.40 2.41 46.27 0.025 51.94 0.050 28.76
Total 100.00 2.26 100.00 0.021 100.00 0.075 100.00

Table 6 A - Summary of magnetic separation of -100# feed (AMB-31/1)

Sl.No Product %Weight % TREE % Dist. %Y %Dist. %Nb %Dist.
1 Sand/6 A Mag. 1 56.60 2.15 53.73 0.018 48.06 0.095 71.24
2 Sand/6 A Non Mag 43.40 2.41 46.27 0.0254 51.94 0.0501 28.76
Total 100.00 2.26 100.00 0.021 100.00 0.075 100.00

The above test indicates 56.6% magnetic minerals in the feed sample (AMB-31/1). However,
no preferential enrichment in REE in any product (magnetic or non-magnetic fractions) is
observed. Slight enrichment in Nb values (750 ppm in feed to 950 ppm in magnetic product
with 71% Nb distribution) is observed in magnetic fraction.

ii) NaOH agitation,acid treatment followed by magnetic separation of -100# feed ( AMB-
31/2 Feed assay: 3.70%TREE, 234 ppm Y, 703 ppm Nb )
The -100# feed sample(AMB-31/2) was subjected to agitation with NaOH (15% NaOH
concentration) at ambient temperature (26-280C) for 6 hours followed by acid treatment 360 kg
H2SO4/t to obtain soluble carbonate matter. The slurry is filtered. The filtrate and residue (sand)
are collected separately Further, the residue was subjected to wet high intensity magnetic
separation (WHIMS) at 6 amperes and the products were chemically analysed and the results
are given in Table 7.

Table-7 Magnetic separation -100# feed after NaOH treatment-(AMB-31/2)

Nb
S.No Product % TREE Y ppm
ppm
Mags at 6 A
1 5.78 234 1437
(31% wt.)
2 Non-mags at 6 A 4.83 254 505

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 Cal. assay 5.13 247 795
ROM feed as such 3.70 234 703

The test has indicated a magnetic product of 31% weight analyzing 5.78%TREE, 1437 ppm Nb
(1.5 & 2 times enrichment respectively).
II. LEACHABILITY STUDIES (AMB-31/1 and AMB-31/2)

Static leaching: Two stage static leaching tests were carried out on samples crushed to -100#.
In the first stage, water with 20%NaOH was used as leachant on the feed sample at ambient
temperature, 50% solids pulp density, 5 hours agitation. The residue and liquor were separated
by filtration. The liquor was analysed to estimate soluble TREE content.
In the second stage, the residues of first stage were re-leached at 2.0 pH with sulphuric acid
(360 kg H2SO4/t), at ambient temperature and 75% solids pulp density for 10 days. No oxidant
was used in the experiments. The tests indicated very low leachability (<5% TREE), which
infers that NaOH treatment followed by low dose of acid is not effective in separating the
carbonate gangue minerals.
2. Bulk composite core sample (BH No. BTK-6,7,9,11,12,17,23&27A), Bhatikhera area,
Barmer district, Rajasthan.
A bulk composite core sample (BH No. BTK-6,7,9,11,12,17,23&27A) comprising of micro-
granite, weighing about 34 kg from Bhatikhera area, Barmer dist, Rajasthan was sent to MinD,
BARC, Hyderabad by I/C, RMRE/WR. However, as per the suggestion of I/C, RMRE/WR, a part
of the sample was taken up for hydrometallurgical studies by MPU, AMD, Hyderabad, (sample
received on 22/11/2019 vide sample slip ID 1318201-29, sample ID- 13182011101 from Sanjay
Bagora, SO/F, WR). Details of studies carried out are given below.

I. PHYSICAL BENEFICIATION STUDIES

i) Size reduction: The bulk core feed sample was crushed and ground in Jaw crusher and roll
crusher to -60 & -100# sizes to carry out beneficiation studies.
ii) Chemical Analysis: The representative bulk core feed sample (-60#) was analysed for REE
& trace elements. The results are given in Table 8 & 8A.

Table 8- Rare Earth Element analysis (ppm)

La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y
50 949 12 566 13 10 126 23 12 25 86 11 73 12 798
9 1 4 9

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 Table 8A - Trace element analysis (ppm)
U3O8 Th Zr Nb Ta Cu Mo Pb Zn Ni Co V
34 85 5078 374 <20 <10 <10 110 666 15 105 <10
The chemical analysis shows that the sample contains 2772 ppm TREE, 798 ppm Y, 374 ppm
Nb. Anomalous concentration of Zr (5078ppm) & Zn (666ppm) is also observed.
iii) Size analysis: Size analysis on the bulk core feed sample was carried out on –6# to know
the preferential concentration/enrichment of rare earths, yttrium and niobium values in any
particular size (Table 9).

Table-9 Size Analysis (Bulk composite core sample Bhatikhera area)

% Cum. % Cum.
Mesh % U3 O 8
% wt. weight weight %D %Y %D %Nb %D %D
No. TREE ppm
retained passed
+10 50.94 50.94 49.06 0.266 46.34 0.072 46.32 0.036 48.14 17 45.74
+20 24.03 74.97 25.03 0.294 24.20 0.079 23.92 0.037 23.66 18 22.85
+40 6.86 81.83 18.17 0.299 7.04 0.082 7.10 0.037 6.74 20 7.25
+60 4.90 86.73 13.27 0.305 5.11 0.083 5.16 0.037 4.84 21 5.44
+80 2.29 89.02 10.98 0.304 2.38 0.082 2.37 0.038 2.32 23 2.78
+100 1.26 90.28 9.72 0.299 1.29 0.079 1.27 0.038 1.28 20 1.33
+150 2.33 92.61 7.39 0.302 2.41 0.080 2.36 0.039 2.39 22 2.71
+200 1.67 94.28 5.72 0.309 1.77 0.085 1.79 0.041 1.80 22 1.94
-200 5.72 100.00 -- 0.482 9.45 0.134 9.72 0.058 8.84 33 9.97
Total 100.00 0.291 100.0 0.079 100.0 0.037 100.0 19 100.0
The size analysis data indicated that total REE, Y and Nb values are marginally enriched in size
products finer than 150 # size.
iv) Heavy mineral separation (-60# feed)
The feed sample was ground to (-)60# size and subjected to gravity separation using wet
shaking table. The table concentrate was further subjected to heavy media separation using
bromoform and methylene iodide to know the heavy mineral concentration. Ferro-magnetics
were separated from the heavy media separation products using hand magnet. The details are
given in table no. 10.
Table 10 Heavy media separation of -60# feed
% Nb
S.No. Product % Wt. %D Y ppm %D %D
TREE ppm
1 T.conc/MI Heavies 2.60 0.63 5.59 1286 4.16 601 4.27
2 T. Conc/MI lights 1.27 0.62 2.69 1530 2.41 775 2.69
3 Bromo lights 96.13 0.28 91.72 782 93.43 354 93.04
4 Total 100.00 0.29 100.00 804 100.00 365 100.00

The heavy mineral separation test indicated that:-

13
  3.87% fraction of heavy minerals (Br. heavies) recovered analyzing 0.62% TREE with only
8% distribution.

 Majority of TREE & Nb values are associated with Bromo-light mineral fractions in -60#
feed sample due to non-liberation of REE values in this size fraction. Though the heavy
minerals assay more TREE, association of TREE with heavy mineral fraction is less.
v) Wet tabling and Wet High Intensity Magnetic Separation (WHIMS)
The feed sample ground to (-) 60# size was subjected to gravity separation using wet shaking
table. The table concentrate was subjected to heavy media separation using bromoform.
Further, the bromo heavies and bromo light fractions were subjected to wet high intensity
magnetic separation (WHIMS) to recover rare earths, Nb bearing minerals as heavy/magnetic
mineral concentrate. The details are presented in table no. 11.
Table 11
Sl.No Product %Wt. % % Y % Nb % Dist.
. TREE Dist. ppm Dist. ppm
1 Br. Heavies/Mags 26.90 0.591 62.81 1394 53.70 680 55.64
2 Br. Heavies/Non-mags Traces Not Analysed
3 Br. Lights/Mags 13.10 0.186 9.64 535 10.04 252 10.04
4 Br. Lights/Non-mags 60.00 0.116 27.55 422 36.26 188 34.32
Total 100.00 0.253 100.00 698 100.00 328 100.00

The chemical analysis of bromo heavies magnetic at 26.9% wt. analysed 0.59% TREE
and indicated a recovery of 63% of rare earths, 54% Y, and 56% Nb values. The Br. Lights
non-magnetic at 60 % wt. analyse 0.1%TREE with a recovery of 28% TREE, 36%Y and 34%
Nb values on - 60# size feed sample.
This test has indicated concentration of rare earths, yttrium & niobium values in the
heavy minerals magnetic concentrate, there by suggesting that gravity and magnetic methods of
concentration for rare earths from these samples is feasible.
vi) Wet high intensity magnetic separation (WHIMS) Studies:
Wet high intensity magnetic separation studies were carried out on -60# & -200# to know
the preferential enrichment/distribution of REE, Nb values in magnetic & non-magnetic products.
The details are given below.
a) WHIMS on -60# feed
WHIMS at 5,10 & 15 kilogauss magnetic intensity sequentially
The feed sample (-60#) was subjected to WHIMS at 5, 10 and 15 kilogauss magnetic intensity
to know the association and recovery/enrichment of TREE, Y & Nb values in magnetic and non-

14
 magnetic fractions. The products were chemically analysed and the details are given in tables
12 & 12A.

Table-12 Wet High Intensity Magnetic Separation (WHIMS) -60#

S.No. Product %Wt. % % Dist. Y % Dist. Nb %Dist.
TREE ppm ppm
1 Mags at 5 kilogauss 23.00 0.37 33.85 798 24.80 400 29.26
2 Mags at 10 kilogauss 7.00 0.74 20.60 1774 16.78 642 14.29
3 Mags at 15 kilogauss 2.00 0.83 6.57 2446 6.61 780 4.96
4 Non-mags
68.00 0.14 38.97 564 51.82 238 51.48
at 15 kilogauss
Total 100.00 0.25 100.00 740 100.00 314 100.00

Table 12A Summary of Wet High Intensity Magnetic Separation (WHIMS) -60#
S.No. Product %Wt. % TREE % Dist. Y ppm % Dist. Nb ppm %Dist.
1 Mags at 15 kilogauss 32.00 0.48 61.03 1114 48.18 476 48.52
2 Non-mags 68.00 0.14 38.97 564 51.82 238 51.48
at 15 kilogauss
Total 100.00 0.25 100.00 740 100.00 314 100.00

The test indicated 61% recovery of TREE values associated with magnetic fraction at
32%wt. with enriched grade of 0.48% TREE (about 2 times enrichment).

WHIMS at 15 kilogauss magnetic intensity

Wet high intensity magnetic separation (WHIMS) of the feed sample (-60#) was carried out
at 15 kilogauss to know the association and recovery/enrichment of REE, Y,Nb values in
magnetic and non-magnetic fractions. The chemical analysis results are given in Table 13.
Table 13 WHIMS at15 Kilogauss
S.No Product %Wt. % TREE %Dist. %Y % Dist. %Nb % Dist.
Mags at 15
1 40.0 0.45 72.13 0.10 60.60 0.05 63.23
kilogauss
Non-mags
2 60.0 0.12 17.87 0.04 39.40 0.02 36.77
At 15 kilogauss
Total 100 0.25 100.00 0.07 100.00 0.03 100.00

The above test indicated recovery of 72% TREE, 60%Y and 63% Nb values in magnetic fraction
(40% weight) suggesting that magnetic methods of concentration for rare earths from these
samples is feasible.
b) WHIMS on -200# feed (at 15 kilogauss magnetic intensity): The feed sample was crushed and
ground to -200# and subjected to WHIMS at 15 kilogauss magnetic intensity to know the

15
association and recovery/enrichment of TREE, Y & Nb values in magnetic and non-magnetic
fractions at finer sizes. The details are given in table 14.

Table 14 Wet High Intensity Magnetic Separation (WHIMS) -200#

S.No. Product %Wt. % % Dist. Y ppm % Dist. Nb ppm %Dist.
TREE
1 Mags at 6 A 30.00 0.59 63.30 1232 48.75 444 48.51
2 Non-mags at 6A 70.00 0.14 36.70 555 51.25 202 51.49
Total 100.00 0.28 100.00 758 100.00 274 100.00

The test indicated 63% recovery of TREE values associated with magnetic fraction at
30%wt. with enriched grade of 0.59% TREE (around 2.1 times enrichment). The maximum
recovery of rare earths did not improve with finer size fractions (-200#).
vii) Pre-concentration of REE by attrition scrubbing tests (-60#):
In order to enrich the grade of REE and other associated elements, the feed sample (-60#) was
subjected to attrition scrubbing in the ball mill for 10 minutes without ball at 100 rpm speed
with pulp density of 30% solids for liberation of cemented material or coatings on the surface.
Further, the pulp was de-slimed manually using a 200# sieve. The -200# (slime- 40%weight)
and +200# (sand- 60% by weight) were collected separately. The same study was carried out
using laboratory mechanical agitator (Remi make) with 50% solids pulp density at ambient
temperature. The chemical analysis data is given in table no. 15.

Table 15 Attrition scrubbing test (-60#)

S.No. Product %Wt. % TREE % Dist. Y ppm % Dist. Nb ppm %Dist.
1 +200# sand 60.00 0.25 47.00 631 44.50 264 48.40
2 -200# slime 40.00 0.42 53.00 1179 55.50 422 51.60
Total 100.00 0.32 100.00 850 100.00 327 100.00
The above test indicates marginal increase in TREE, Y & Nb values which are associated with
fine mineral fraction (i.e. -200# product).
II. HYDROMETALLURGICAL STUDIES
The following leaching tests were carried out to determine the rare earths leachability.
Conventional Hot agitation leaching (Feed Size variation)
Hot agitation leaching experiments were carried-out on samples ground to -60, -100# & -200#
using H2SO4 as leachant and 10 kg MnO2/t as oxidant in 6 hours contact time, pulp density at
50% solids & temp. 700C. Details are presented below in table-16
Table 16 Conventional hot acid agitation leaching
S.No. Size H2SO4 kg/t % REE Leachability
1. -60# 112 31.0

16
 2. -100# 180 33.0
3. -200# 180 33.2
These tests demonstrated that with decrease in size and increase in acid dosage, the
leachability has not increased significantly.

A. Conventional Hot agitation leaching at -60# feed sample

Conventional hot acid agitation leaching tests were carried out on the feed samples crushed to
minus 60# size for the extraction of rare earths under varying experimental conditions i.e.
Temperature- ambient (26-280C), 70 & 900C; Contact time - 6 & 8 hour; pH - 0.5, 1.0 &1.6;
Oxidants with varying dosages- MnO2, K2S2O8 (10-30 kg/t). pH (acid concentration), oxidant
dosage. The other parameters maintained were- 50% solids pulp density and 70 0C
temperature. The data is given below (Table 17, 17a, 17b & Fig. 1- 3)

Table 17 Conventional hot acid agitation leaching

MOG: -60#, Pulp density: 50% solids Temp: 700C
pH variation (1.0 & 1.8)
pH H2SO4 Kg/t MnO2 Agitation Time Leachability Leachability
Kg/t (hrs) %TREE %Y
1.8 29 15.0 6 28 32
1.0 72 20.0 6 32 34
1.0 83 20.0 8 33 36
Oxidant variation (MnO2 and K2S2O8, pH: 1.0, contact time: 6 hours)
Oxidant H2SO4 (kg/t) % leachability
(kg /t) % TREE % LREE %HREE %Y
fractional fractional
10 kg /t MnO2 72.0 28.64 28.87 27.19 30.08
20 kg /t MnO2 76.0 32.21 32.63 29.68 31.84
30 kg /t MnO2 108.0 30.11 30.48 27.85 31.00
20 kg/t K2S2O8 112.0 31.07 31.56 30.70 29.35
Contact time variation (pH: 1.0, 20 kg/t MnO2)
H2SO4 Contact time % Leachability
Kg/t (hrs.) TREE LREE HREE Y
83 8 33.44 33.32 34.37 36.12
126 16 (8+8) 39.68 40.83 33.72 37.30
180 24 (12+12) 47.24 48.92 36.95 40.92
Table 17a Effect of Oxidant on individual REE leachability
Oxidant H2SO4 %Fractional leachability
kg /t (kg/t)
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y
10
72 24.3 25.3 30.1 32.4 40.1 35.4 44.4 37.5 34.9 26.9 25.5 16.1 16.2 11.5 30.1
MnO2
20
76 27.7 28.9 33.8 36.8 43.8 39.3 47.7 40.3 38.2 30.2 26.5 26.5 17.3 12.4 31.8
MnO2
30
112 26.0 26.8 30.5 34.0 42.4 37.1 46.8 38.0 36.8 26.9 25.2 17.0 16.1 11.6 31.0
MnO2

17
 20
108 27.1 28.2 33.6 35.0 42.9 37.0 45.1 39.5 36.5 29.5 25.3 25.8 16.0 11.7 29.3
K2S2O8

60 10 kg/t MnO2 20 kg/t MnO2 30 kg/t MnO2 20 kg/t K2S2O8

50

40
% Leachability

30

20

10

0
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y

Fig. 1 Effect of oxidant on fractional individual REE leachability (-60# Feed)

%Leachability

TREE
%Leachability

60
60 LREE
50
50
40 40
30 30
20 20
10 10
0 0
6 8 10 12 14 16 18 20 22 24 26 6 8 10 12 14 16 18 20 22 24 26
Contact time in hours Contact time in hours
%Leachability

%Leachability

60 HREE 60 Y
50 50
40
40
30
30
20
20 10
10 0
0 6 8 10 12 14 16 18 20 22 24 26
5 10Contact15time in20
hours 25 30 Contact time in hours

Fig.2 Effect of contact time on REE,Y leachability( -60# feed)

18
 Table- 17b Hot agitation leaching - contact time (16 & 24 hr.) variation on -60# size feed
Temp.: 700C, Oxidant : 20Kg MnO2/t, Pulp density: 50% solids, H2SO4: 126 & 180 kg/t
%Leachability (fractional)
Contact
time
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y

16 hours 37.0 37.3 41.3 44.8 49.7 49.9 53.9 46.4 42.0 41.0 29.9 32.8 19.7 16.0
37.3
24 hours 45.5 46.2 48.1 53.0 55.2 54.9 58.5 47.2 45.8 42.8 32.1 35.0 20.9 17.3 40.9

16 hrs contact time 24 hrs contact time

60

50

40
%Leachability

30
B. Hot acid agitation
20
leaching on
10
Beneficiated
0
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y products (Magnetic
fraction):
Fig. 3 Effect of contact time on fractional individual REE leachability (-60# Feed)
Hot acid agitation leaching test on the magnetic separation products (6A magnetic and 6A non-
magnetic) was carried out. The details are given in Table no. 18.
Table – 18 Conventional hot acid agitation leaching (-60# feed)
6A magnetic & non magnetic fractions , Agitation time: 6h, Pulp density: 50% solids, Temp: 700C
Product %Wt. Cal. feed H2SO4 kg/t % TREE % Y leachability
%TREE leachability
Mags at 6 A 34.80 0.47 99 19.95 36.87
Non- Mags at 6 A 65.20 0.17 63 38.57 27.80
The above studies indicated that:
 Hot agitation on 6A magnetic and 6A non-magnetic fractions shows maximum
leachability of 19.9% and 38.57% of Total REE respectively in 6 hours contact time at
700C temperature
C. Pug cure leaching followed by agitation leaching at -100# size

Pug cure leaching tests (2 Nos.) with 2 hours pugging at 90 0C followed by 4 hours agitation at
700C were carried out on -100# feed . The acid used was 90 kg H 2SO4/t & 180 kg H2SO4/t with
20 kg MnO2/t as an oxidant in both tests. The details are given in table 19.
Table-19 Pug cure leaching (2+4 hours)
MOG: -100#, Pug cure time: 2hrs, Agitation time: 4 hrs,
Pulp density: 90% and 50%solids, Temp: 900 and 700C , Oxidant: 20kg MnO2 /t
Product H2SO4 kg/t Leachability %TREE Leachability %Y
-100# feed 90 29 31
-100# feed 180 36 32

19
 The above tests indicated maximum TREE leachability of 36% by pug cure leaching method (2
hours pugging + 4 hours agitation). However, the conventional hot acid agitation leaching of -
60# feed sample has indicated 33% TREE leachability with low dosage of acid up to 83 kg
H2SO4/t at 700C for 8 hours contact time. The individual REE leachability data is presented in
table 20 and fig. 4.
Table 20 - Effect of hot agitation & pug cure leaching on individual REE leachability
@ Temp :70oC, Time:6 hours, Pulp density:50%Solids
Leaching H2SO %Fractional leachability
method 4
(kg/t) La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y

HAL 83 36.0
27.6 30.0 33.7 36.9 45.7 63.7 51.6 45.7 43.2 53.2 31.7 18.5 19.7 9.8
@60#
PCL 180 32.0
34.6 34.7 37.8 38.9 42.2 40.7 42.2 48.0 35.3 31.6 27.3 14.0 18.3 15.0
@-100#
HAL= Hot Agitation Leaching; PCL= Pug Cure Leaching

70

60

50
%Leachability

40
HAL
30 PCL

20

10

0
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y

Fig. 4- Effect of leaching method on individual REE leachability.

D. Cold Static Bed Leaching

Static bed leaching experiments (2 nos.) were carried out on the –100# feed samples at
75% solids pulp density using 180 Kg H2SO4/t as leachant at ambient temperature, 7 days
contact time by varying oxidants (NaClO3: 20 kg/t, K2S2O8: 50 kg/t). These experiments were

20
carried out to study the dissolution of REEs at higher oxidation potentials even without agitation
method. The derails are given in Table 21.

Table-21 Static leaching - oxidant variation on -100# size feed

MOG: -100#, Temp.: Ambient, contact time: 7 days, Pulp density: 75% solids, H2SO4: 180 kg/t
Oxidant % Leachability
Kg/t % TREE % LREE % HREE %Y
fractional fractional
20 kg NaClO3/t 27.42 26.75 30.44 31.02
50 kg K2S2O8/t 35.51 35.75 34.41 33.20

The above studies on -100# ROM feed samples indicated

 Maximum leachability of 35.51% Total REE, 35.75% LREE (fractional), 34.41% HREE
(fractional) and 33% Y in 7days of contact time.
 Fractional LREE, HREE and Y have shown almost similar leachability.

The comparison of hot agitation and static bed methods and conditions determined to obtain
maximum %REE leachability is given in table 22.

Table 22 Comparison of Hot agitation and Static bed leachability studies

Parameter Hot agitation Leaching Cold Static bed leaching

Size of ore 250 micron (60#) 150 micron (100#)
Pulp density 50% solids 75% solids
H2SO4 consumed 180 kg/t 180 kg/t
Oxidant 20 kg MnO2/t 50 kg K2S2O5/t
Contact time 24 hours 7 days
Temperature 700C Ambient (25- 270C)
Recovery (% Leachability) 47.24% TREE, 40.92%Y 35.51% TREE, 33.2%Y

The process flow-sheet studied for extraction of rare earths from ROM feed is given below.

Flowchart for extraction of rare earth elements from Bhatikhera area, Rajasthan .

Micro-granite rock (core sample-ROM)

21
(Feed Assay: 0.27% TREE, 0.08%Y, 0.037% Nb)
 Manual crushing (3 – 4 inch size)

Crushing in Jaw crusher (1/4 in. size)

Crushing and grinding in Rolls crusher and Ball Mill (-60 and -100# sizes)

Powdered Ore Water

Leaching Sulphuric Acid
Oxidant

Filtration
(Solid – liquid separation)

Leach liquor 47% TREE Leachability

INFERENCE

 The feed sample chemically analysed 2772 ppm TREE, 798 ppm Y, 374 ppm Nb
5078ppm Zr & 666ppm Zn
 The size analysis test on -6# feed indicated that total REE, Y and Nb values are
marginally enriched in size products finer than 150 # size.
 The heavy mineral separation test on -60# feed indicated 3.87% fraction of heavy
minerals (Br. heavies) analyzing 0.62% TREE with only 8% distribution. Majority of
TREE & Nb values are associated with Bromo-light mineral fractions in -60# feed sample
due to non-liberation of REE values in this size fraction. Though the heavy minerals
assay more TREE, however, association of TREE with heavy mineral fraction is less.
 Wet high intensity magnetic separation (-60#) indicated recovery of 72% TREE, 60%Y
and 63% Nb values in magnetic fraction (40% weight) with marginal increase in grade
from 0.27% to 0.45% TREE.

22
  The magnetic separation test has shown preferential association and distribution of rare
earth values with magnetic fraction indicating the feasibility of this method for enriching
rare earth values.
 Leachability studies by hot agitation on -60# ROM feed samples indicated maximum
leachability of 47.24% Total REE, 48.92% LREE (fractional), 36.95% HREE (fractional)
and 40.9% Y in 24 hours contact time , using 180 H2SO4/ ton as leachant and 20 kg
MnO2/t as oxidant
 Among the LREEs (i.e., La to Gd), maximum leachability of Sm:55%, Gd: 58.5% are
obtained. Among the HREEs (i.e., Tb- Lu), maximum leachability of Tb: 47.2%, Dy:
45.8% are obtained.

3. Mine dump sample of Silicified Sovite Carbonatite, GMDC Mine, Ambadongar, Gujarat.
A bulk mined ore dump sample comprising of silicified sovite carbonatite weighing about 10 kg
from GMDC mine, Ambadongar area, Chotta Udepur district, Gujarat was taken up for physical
beneficiation and REE leachability studies. (Samples received on 16/12/2019 vide Sample ID
131920388, Sample No. - ODS/AMBA-19-20/2, from Shri P.S.C. Pandit, SO/E, WR).
I. PHYSICAL BENEFICIATION STUDIES:
i) Size reduction of feed samples: The rock sample was crushed to -60# & -100# sizes for
carrying out beneficiation studies.
ii) Chemical Analysis: The representative feed sample was chemically analysed for REE & U.
The analytical result is given in table- 23

Table 23- Rare Earth Element analysis (ppm)

La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Y Sc Nb U3O8
1323 2437 262 101 140 28 64 4 30 5 10 <3 5 1 110 <1 470 <10
1 0

Chemical analysis indicated 0.53% TREE, 110 ppm Y and 470 ppm Nb in the feed sample.

iii) Heavy media separation on -60# feed sample:

The feed sample (-60#) was subjected to heavy media separation at sp.gr. 2.8 using
bromoform. The details are given in Table 24.
Table 24 Heavy media separation of -60# feed

23
 % Y
S.No. Product % Wt. %D %D Nb ppm %D
TREE ppm
1 Heavies at Sp.gr. 2.8 2.2 0.679 2.91 177 3.49 1596 7.60
2 Lights at Sp.gr. 2.8 97.8 0.509 97.09 110 96.51 436 92.40
4 Total 100.0 0.513 100.00 111 100.0 461 100.0

This test has not indicated any significant concentration of TREE values in the heavy minerals
concentrate, there by suggesting that gravity methods for concentration of REE from these
samples is not feasible. Marginal enrichment in Nb (3 times) was noticed. However, majority of
TREE, Y, Nb values are associated with light mineral fraction due to non-liberation of REE
values in this size(-60#) fraction.

iv) Wet high intensity magnetic separation (WHIMS) on -60# feed:

WHIMS of the feed sample (-60#) at 2,4,6 amperes was carried out to know the recovery of
REE, Y, Nb values with magnetic and non-magnetic fractions with their enrichment. The test
details are given in Table 25 & 25A.

Table-25 Wet High Intensity Magnetic Separation (WHIMS) -60#

% Nb
S.No. Product %Wt. % Dist. Y ppm % Dist. %Dist.
TREE ppm
1 Mags at 2 A 4.10 0.613 4.85 102 3.67 1170 10.75
2 Mags at 4 A 3.84 0.735 5.44 119 4.01 1212 10.43
3 Mags at 6 A 4.02 0.758 5.87 119 4.20 1080 9.73
4 Non-mags at 6 A 88.04 0.494 83.84 114 88.12 350 69.08
Total 100.00 0.518 100.00 114 100.00 446 100.00

Table 25A Summary of Wet High Intensity Magnetic Separation (WHIMS) -60#
%
S.No. Product %Wt. % Dist. Y ppm % Dist. Nb ppm %Dist.
TREE
1 Mags at 6 A 11.96 0.70 16.16 113 11.88 1153 48.52
2 Non-mags at 6A 88.04 0.494 83.84 114 88.12 350 69.08
Total 100.00 0.518 100.00 114 100.00 446 100.00
These tests indicated that majority of TREE, Y values are associated with non-magnetic
minerals which are present in major amounts.

v) Pre-concentration of REE by attrition scrubbing test (-60#):

Attrition scrubbing was carried out on -60# feed sample in the work index ball mill for 10 minutes
without ball at a pulp density of 30% solids, 100 rpm speed. Further, the pulp was de-slimed
manually using a 200# sieve. The -200# (slime 40% by weight) and +200# (sand 60% by

24
weight) were collected separately and chemically analysed for REE content. The details are
given in table 26.

Table 26 Attrition scrubbing test (-60#)

S.No. Product %Wt. % TREE % Dist. Y ppm % Dist.
1 +200# scrub sand 60.00 0.45 56.56 91 56.00
2 -200# scrub slime 40.00 0.52 43.44 107 44.00
Total 100.00 0.48 100.00 97 100.00
(Cal. feed assay)

The above test did not show any preferential concentration of TREE, Y values in any of
scrubbed sand/slime products.
vi) Sedimentation-Decantation studies
Gravity concentration by Sedimentation-Decantation was carried out to enrich the heavy
minerals and flotation was carried out to separate carbonates from silicates and oxides etc.
The representative feed sample crushed and ground to -60# size was subjected to
sedimentation process (allowed to settle in water medium for complete dispersion) about ½
minute and 1 minute time duration. Particles having higher settling velocities (sedimentation)
and lower settling velocities (decantation) are separated. The details with chemical analysis are
given in Table 27.

Table 27 Sedimentation-Decantation of -60# feed sample

S. No. Product % Wt. %TREEY %Dist.
1. Decantation fraction at ½ minute 6.5 0.58 7.86
2. Decantation fraction at 1 minute 18.0 0.53 19.81
3. Sedimentation fraction after 1 minute 75.5 0.46 72.32
Total 100 0.48 100.00

The test indicated:-

i) Sedimentation product (high settling minerals) of 75.5% by weight is associated with
72% REE values.
ii) No preferential enrichment of REEY in any fraction, thus indicating that the gravity
separation method is not feasible for this sample.

vii) Flotation studies

Flotation was carried out on -60# feed sample to float carbonate minerals using oleic acid as
collector, sodium silicate as depressant for silicate minerals and pine oil as frother. The float
product was subjected to heavy media separation using bromoform. All the separated products

25
were chemically analysed for rare earths content. Only about 8% rare earths values are
associated with float bromo- heavies fraction. The details are given in table 28

Table 28- Flotation of -60# feed sample

Size: -60#, pH modifier: 10 kg Na2CO3/t, Collector: 2 ml for 100 grams feed,
Depressant: 10 kg sodium silicate/t, Frother: pine oil
S.No Product %Wt. %TREEY %Dist.
1 Float Br. heavies 6.0 0.60 7.95
2 Float Br. Lights 62.0 0.48 65.51
3 sink 32.0 0.38 26.54
Total 100 0.46 100.00

Flotation of the feed sample did not show any enrichment of rare earth values indicating the
non-feasibility of this method.

II. HYDROMETALLURGICAL STUDIES

Cold Static Bed Leaching

Two static bed leaching experiments on –60# sample at 75% solids pulp density using
288 Kg H2SO4/t as leachant were carried out by varying oxidants 100 Kg K2S2O8/t & NaClO3/t at
ambient temperature (27-300C) keeping the slurry for 5 days. The chemical analysis results
indicated maximum leachability of 19.5% TREE with K2S2O8 as oxidant. The experiment with
NaClO3 as oxidant indicated very low TREE leachability (<5%). The details are given in table 29
& Fig.1.

Table 29 Static leaching on -60# size feed

MOG: -60#, Temp.: Ambient, Oxidant : 100Kg K2S2O8/t, Pulp density: 75% solids, H2SO4: 288 kg/t
Contact time %LREE, Y Leachability (fractional)
La Ce Pr Nd Sm Eu Gd Y
5 days 16.8 18.8 16.5 18.0 24.0 29.9 38.9 49.1

26
 50
45
40
35
% Leachability

30
25
20
15
10
5
0
La Ce Pr Nd Sm Eu Gd Y

Fig. 5 Cold static bed leaching on -60# feed samples (fractional LREEY leachability)

4. Grab samples of Pegmatite from Amreshwar area, Raichur dist., Karnataka

A total of 19 pegmatite samples from Amreshwar area, Raichur district, Karnataka were sent by
Shri K. Thillairaj, SO/D, RMRE/SR for Petro-mineralogical studies. As per the discussions with
AD (R&D) and Head, RMRE Group it was advised to select initially, three samples with
anomalous Li content for separation of Spodumene rich concentrate in MPU Lab, Hyderabad.
Accordingly following three samples were selected for isolation of spodumene mineral
concentrate.

Table 30 Sp.gravity of feed samples

S. No. Sample No. Li content in ppm Sp. gravity

1 AMR/PEG/7/2 6647 2.37
2 AMR/PEG/4/4 2295 2.75
3 AMR/PEG/4/7 4600 2.33

The samples were processed by gravity concentration (heavy media separation) and low
intensity magnetic separation. The data on all the three samples is given below.

i) Specific gravity determination

Specific gravity of the pegmatite feed samples crushed to -40# were determined and the
obtained specific gravity is given in table 30 above.

27
ii) Isolation of heavy minerals

The samples were crushed to -40 mesh size by hand pounding and sizing was carried out using
100 mesh sieve. In general, the specific gravity of spodumene mineral varies from 3.03 to 3.23.
Accordingly, the sized products were subjected to heavy media separation using bromoform
and methylene iodide at specific gravities of 2.89 and 3.3 to recover spodumene mineral fraction
(MI light product Sp. gr. >2.89 but <3.3). The details are given in table 31

Table 31 Mineral isolation of sized products

Product -40+100# -100# Total
Sample No.
Wt. %wt. Wt. %wt. Wt. %wt.
(Li content)
grams grams grams
MI Heavies 0.30 0.06 Nil --- 0.30 0.06
AMR/PEG/4/4
MI Lights 8.40 1.68 Nil --- 8.40 1.68
(2295ppm)
Bromo Lights 226.30 45.26 265.00 53.00 491.30 98.26
Total 235.00 47.00 265.00 53.00 500.00 100.00
MI Heavies 0.10 0.029 Nil --- 0.10 0.029
AMR/PEG/7/2 MI Lights 41.60 12.23 Traces --- 41.60 12.23
(6647ppm) Bromo Lights 113.30 33.32 185.00 54.41 298.30 87.73
Total 155.00 45.58 185.00 54.41 340.00 100.00
MI Heavies 0.60 0.18 Nil --- 0.60 0.18
AMR/PEG/4/7 MI Lights 0.12 0.03 Nil --- 0.12 0.03
(4600ppm) Bromo Lights 164.28 50.55 160.00 49.24 324.28 99.79
Total 165.00 50.76 160.00 49.24 325.00 100.00

The above tests indicated 0.03% to 12.2% by weight of MI lights (spodumene rich conc.)
These sample fractions were also subjected to low intensity magnetic separation using hand
magnet. No ferro-magnetic minerals were found.
Further, specific gravity of the spodumene rich concentrate fraction (MI light of 12.2% by weight,
sample No. AMR/PEG/7/2) were determined and obtained specific gravity is 3.1 (approx.). The
specific gravity of this product can be correlated to the specific gravity of spodumene mineral
(3.03-3.23). The obtained sp. gravity of the MI light fraction falls within the range of spodumene
mineral.

28
R&D Assignment No. 22 (3319022) (Lithium extraction from Brines):
The assignment is in continuation of the previous year R&D work. In continuation to the studies
carried out on Li enrichment/precipitation from brine samples (2 nos.), another set of four brine
water samples (about 20 liters each) which includes two duplicate of previous samples
(PPR/W/468 & 489) and two new samples (PPR/W/454 & 493) collected from Pachpadra Salt
Lake area, Barmer district, Rajasthan were taken up for beneficiation studies for extraction of
Lithium from brine samples.
Specific gravity & pH determination:
Specific gravity and pH of the four brine samples was determined. The specific gravity of these
samples vary from is 1.04 to 1.28 and pH range from 6.75 to 7.85 (table 32).
Table 32 Specific gravity & pH of brine samples
Sample number Sp.gr. pH
PPR/W/454 1.24 6.81
PPR/W/468/A* 1.12 7.70
PPR/W/489/A* 1.28 6.75
PPR/W/493 1.04 7.85
A* Refers to duplicate samples collected during 2019-20

Chemical Analysis
The representative brine samples were chemically analysed for Li and associated elements,
which indicated <1 to 15 ppm of Li with high content of Na (23.8 – 81.3 g/l) and Mg (1.1 – 46.4
g/l). The results are given in the table 33
Table 33 Chemical analysis of brine samples
g/l mg/l ppb
Sample No. Na K Mg SO4 2-
Ca Cl- Fe PO 4
3-
Li B U
PPR/W/454 81.3 8.8 32.8 254.2 0.2 218.0 <1 <1 14 95 30
PPR/W/468 50.0 1.3 3.1 29.5 2.5 93.9 <1 <1 3 33 105
PPR/W/489 68.1 11.1 46.4 548.7 0.1 180.8 <1 <1 15 300 840
PPR/W/493 23.8 0.9 1.1 14.4 1.8 53.2 <1 <1 <1 <10 5
Note: As the sample No. PPR/W/493 analysed <1 ppm Li, hence not taken up for further
beneficiation studies.
Recovery of Li by Evaporation- Concentration process:
Earlier experiments of evaporation-precipitation conducted for 3 days indicated Li enrichment
from 25 ppm to 93 ppm i.e. Li enrichment up to 3.7 times, with Na concentration reduced to 90
- 93% while Mg concentration increased. In continuation to these studies, evaporation-
precipitation experiments with longer duration (>3 days) and tests to precipitate Magnesium and
to enrich lithium were carried out.
29
Experiment no. 1: The brine samples (500ml each) were heated to 40 0 – 450C for 6 hours and
allowed to cool for over-night (18 hours) for precipitation to take place. The process continued
for 6 days (3 + 3 days sequentially). The details are given in table 34.
Table 34 - Chemical analysis of evaporated brine samples
Sample No. Product Li ppm Na % Mg %
PPR/W/468 Crystals stage 1 (after 3 days) 2 30 0.7
Crystals stage 2 (after 6 days) 18 4.3 4.9
PPR/W/489 Crystals stage 1 (after 3 days) 4 9 4.7
Crystals stage 2 (after 6 days) 11 0.4 7.3
PPR/W/468 Filtrate after stage 2 (after 6 days) 66 mg/L 2.9 g/L 71 g/L
PPR/W/489 Filtrate after stage 2 (after 6 days) 78 mg/L 2.4 g/L 72 g/L
 The above study indicates 66 to 78 ppm Li values in 6 days of evaporation-concentration
process in the filtrate compared to the feed brine sample of 25-26 ppm Li.
 The filtrate analysed high Mg values of 72g/L.

Experiment no. 2: Evaporation concentration experiments were conducted on 500ml volume

of the brine samples. The samples were heated to 400 – 450C for 6 hours and allowed to cool for
over-night (18 hours) for precipitation to take place. The process was continued for 3 days.
Chemical analysis results indicated 72% to 99% evaporation. The details of are presented in
Table 35.

Table 35 Chemical analysis of brine evaporation- concentration

Sample No. Product Li Na K Ca Mg Cl- SO42-
mg/L ---------------g/L-------------------------
PPR/W/454 Filtrate after evaporation 35 6.8 12.0 0.1 84.8 273.0 82.6
Crystals after evaporation 3 30.3% 0.35% 0.09% 1.98% 60.6% 6.1%

PPR/W/468 Filtrate after evaporation 23 62.5 7.5 2.0 26.5 216.2 9.1
Crystals after evaporation 1 32.5% 0.23% 1.55% 0.23% 70.9% 4.2%
PPR/W/489 Filtrate after evaporation 44 12.5 18.0 0.1 84.7 265.9 78.0
Crystals after evaporation 5 24.3% 0.93% 0.06% 3.55% 45.2% 21.5%
The above process indicated

i) Li enrichment from 15ppm (in feed) to 44 ppm in filtrate (about 3 time’s enrichment).
ii) Separation of appreciable amounts of impurities i.e. Na, K, Ca, Cl - & SO42- away from Li
bearing filtrate which are concentrated/separated as evaporated crystals. However, Mg is
also being concentrated along with Li.
Experiment no. 3: Evaporation concentration experiments were conducted on 500ml volume of
the brine samples. The samples were heated to 400 – 450C for 6 hours and allowed to cool for
over-night (18 hours) for precipitation to take place. The process was continued for 3 days.
Further, the evaporated brine was subjected to Na2CO3 treatment at 900temperature. The details
are given in table 36

30
 Table-36 Chemical analysis of evaporated brine samples
Treatment of evaporated brine with Na2CO3 at 900 temperature.
Sample No. Product Li Na Mg SO4-2
mg/l g/l g/l g/l

Brine before evaporation 26 30 50 71

Filtrate after Na2CO3 treatment 78 26.3 60.1 96.5
PPR/W/489 & evaporation (3 times enrichment)
Crystals after evaporation 5 to 7 24.5 to 0.9 to 1.4 to
28% 1.0% 4.8%
Precipitate (Mg cake- dry) 20 7.1% 8.9% 4.0%
Brine before evaporation 15 68.1 46.4 548.7
Filtrate after Na2CO3 treatment 37 99.8 0.1 38.0
PPR/W/489/A
(duplicate of above & evaporation
sample) Crystals after evaporation 2 30.0% 0.20% 15.7%
Precipitate (Mg cake- dry) 21 12.9% 12.2% 6.8%
Brine before evaporation 3 50 3.1 29.5
Filtrate after Na2CO3 treatment 10 133.8 0.1 11.1
PPR/W/468/A & evaporation (3 times enrichment)
Crystals after evaporation 0.9 30.7% 0.1% 0.3%
Precipitate (Mg cake- dry) 5 16.7% 7.4% 0.6%

The above studies indicated Li enrichment from 26 ppm in feed to 78 ppm in filtrate in sample
no. PPR/W/489. However, the impurities like Mg, SO4-2 were not removed.
In sample no. PPR/W/489/A, Li content increased from 15 in the feed to 37 in filtrate with
appreciable removal of Mg & SO4-2 content from 46 g/l in feed to 0.1 g/l (Mg) and 548 to 38 g/l
(SO4-2) in the filtrate. Further, the test shows that magnesium and sulphate values are intimately
associated and can be separated together.
Experiment no. 4: Recovery of Li by Evaporation followed by treatment of filtrate with
Ca(OH)2 and Na2CO3 : Evaporation at 400- 450C, 6 hours, filtration, treatment with Ca(OH) 2 to
remove magnesium as Mg(OH)2. Further, Na2CO3 is added to the filtrate to separate calcium as
CaCO3. The details are given in table 37.

Table 37 Chemical analysis of evaporated brine samples

Sample No. Product Li Ca Na Mg
mg/l mg/l g/l g/l
PPR/W/468 Liquor after evaporation 70 22 4.5 72
Evaporated brine treated with 38 <10 88 0.002
Ca(OH)2 and Na2CO3 filtrate

The experimental parameters optimized are:

31
 Brine samples heated to 400 – 450C for 6 hours and allowed to cool for over-night (18 hours) for
precipitation to take place (to crystallize the major salts like sodium, potassium and magnesium)
and continuing the process for 6 days.
With above process, the impurities like Na, K, SO 4-2 were removed from the evaporated brine,
however, Mg concentration was increased.

concentration

R&D Assignment No. 24 (3319024) (Coal ash dump samples for uranium recovery)

The assignment is in continuation of the previous year R&D work. Five samples of coal ash
dumps each weighing about 1-1.5 kg from Kothagudem Thermal Power Plant (1 No.), and Nava
Bharath Power Plants (4 Nos.), Palvancha area, Bhadradri-Kothagudem district, Telangana
were received for Beneficiation & Hydro-metallurgical studies from Shri B. Vijayanand, SO/F. In
continuation to the earlier studies in which the representative feed samples analysed 13-16 ppm
U3O8, 296-439ppm TREE, 24-48ppm Y & 34-42ppm Th, further beneficiation studies were taken
up during the current Annual Programme. The details are given below.
i) Mineral isolation studies: The feed samples were subjected to heavy media
separation using bromoform as the media with varying specific gravity of 2.89, 2.2, &
1.8 (Table 38).
Table 38- Mineral separation at different specific gravities (with chemical analysis)

32
Sample NBVL 114 NBVL coarse
KTPS ( I & II) NBVL 150 MWPP NBVL Granules
No. Silo III Silo IV
% TREE U3O8 TREE U3O8 TREE U3O8 TREE U3O8 TREE U3O8
Product %wt. %wt. %wt. %wt.
wt. ppm ppm ppm ppm ppm ppm ppm ppm ppm ppm
Heavies
0.60 435 57 0.49 1660 22 0.40 622 <10 0.89 120 <10 2.06 180 <10
@ 2.8
Lights @
4.00 303 <10 19.89 416 <10 65.60 405 <10 95.23 322 <10 95.70 286 <10
2.8
Lights @
72.80 390 <10 78.01 371 <10 30.00 402 <10 3.16 249 <10 1.98 238 <10
2.2
Lights @
22.60 424 <10 1.61 235 <10 4.00 179 <10 0.72 173 <10 0.26 150 <10
1.80
Total 100.00 394 <10 100.00 384 <10 100.00 395 <10 100.00 316 <10 100.00 282 <10
The above test indicated:-
i) 0.40- 2.06% heavy mineral and 0.26 to 22.60% carbonaceous matter (lights).
ii) Two samples analysed 22 to 57 ppm U3O8 values in bromo-heavies while the remaining
samples analysed low U3O8 values (<10 ppm).
iii) The bromo-heavies of first three samples viz. KTPS (I & II), NVBL 150, NVBL 114 analysed
higher concentration of REE values (435 – 1660 ppm).
ii) Wet high intensity magnetic separation (WHIMS): Wet high intensity magnetic separation
(WHIMS) of the feed samples (-60#) at 6 amperes was carried out to know the feasibility of
enrichment of U, REE by magnetic method. The test indicated 30 to 70% wt. magnetic fraction.
The details are given in table 39.
Table 39 Wet high intensity magnetic separation of -60# feed samples
Smpl.No
KTPS ( I & II) NBVL 150 MWPP NBVL 114Silo III
.

% TREE U3 O 8 TREE U3 O 8 TREE U3 O 8

Product %D %D %wt. %D %D %wt. %D %D
wt. ppm ppm ppm ppm ppm ppm

Mags 6A 33 446 38 10 29 30 383 31 <10 -- 65 375 66 47 88

Non-
67 354 62 12 71 70 368 69 <10 -- 35 356 34 12 12
mags 6A
10
Total 100 385 100 11 100 100 372 <10 -- 100 368 100 34 100
0

Table 39 (cont.) Wet high intensity magnetic separation of -60# feed samples
Smpl.No. NBVL coarse Silo IV NBVL Granules
% TREE U3 O 8 % TREE U3 O 8
Product %D %D %D %D
wt. ppm ppm wt. ppm ppm
Mags at 6A 70 320 70 <10 -- 60 292 62 <10 --
Non-mags at 6A 30 322 30 10 -- 40 269 38 <10 --
Total 100 321 <10 -- 100 283 100 <10 --
The chemical analysis of the magnetic separation fractions indicated that there is no preferential
enrichment of uranium/rare earth values with the magnetic and non-magnetic fraction. Only one
sample i.e. NVBL 114 Silo III analysed 47ppm U 3O8 values with 88% distribution.
NOTE: In the review meeting of R&D assignments during March 2020 it was advised to close

33
the studies on the Coal ash samples, as the feed samples analysed 13-16 ppm U 3O8 and the
bromo heavies analysed upto 57 ppm U3O8.
Miscellaneous:
i) Associated in the preparation and submission of following reports
a. Annual Report of Mineral Processing Unit for the year 2018-19 submitted in December
2019.
b. Granite rock samples for REE beneficiation, Sheetalamata area, Siwana Ring
Complex, Barmer dist., Rajasthan.
c. Micro-granite rock (grab) samples for REE beneficiation, Bhatikhera area, Siwana Ring
Complex, Barmer dist., Rajasthan.
d. Bulk composite core sample (BH No. BTK-6,7,9,11,12,17,23 & 27A), Bhatikhera area,
Barmer district, Rajasthan for REE beneficiation, Bhatikhera area, Siwana Ring
Complex, Barmer dist., Rajasthan.
e. Bulk Core samples of BH AMB-17, Ambadongar area, Chhota Udepur dist, Gujarat.
f. Composite Borehole core sample from Naktu area, Sonbhadra dist., U.P (final report)
g. Coal ash dump samples from thermal power plants, Palvancha area, Bhadrai-Kothagudem
dist., Telangana
ii) Associated in the Presentation of following R&D assignments
“Review and progress of Assignment No. 20 (3319020) (Ambadongar- mineralogical,
size liberation studies ),
Assignment No. 22 (3319022) (Lithium extraction from Brines) and
Assignment No. 24 (3319024) (Coal ash dump samples for uranium recovery)” which
were presented on 20-03-2020.
iii) Presentation and Publication of scientific papers: Co-authored in the following paper
preparation/publication:
Abstract of paper titled “A study on the recovery of xenotime mineral concentrate
from the pre-concentrates of Siri River, Kunkuri, Jashpur district, Chhattisgarh,
India “ co-authored with K.L.Mundra, K.K.Pandey for presentation in the 36 th
International Geological Congress, Delhi, India – 2-8 March, 2020”. The conference was
postponed due to COVID-19.
iv) Associated and participated in National Science day exhibition held in AMD complex,
Hyderabad on 28-02-2020, in which a stall exhibiting various activities of MPU and
RMRE was setup for the benefit of invited school students.
v) Technical Committee for Scrutinising Mining Plans (TCSM):

34
 As a member of Technical Committee for Scrutinising Mining Plans scrutinized nine (9)
Mining Plans and progressive mine closure plans (review mining plans) in reference to
Mineral processing aspects, pertaining to M/s Uranium Corporation of India Ltd. (UCIL).,
M/s Indian Rare Earths Ltd. (IREL) & M/s Kerala Minerals and Metals Ltd (KMML).
a) M/s Uranium Corporation of India Ltd. (UCIL) – 6 Nos.
i)Bhagjata Uranium Mines over an extent of 122.73 Ha ii)Tummalapalle 813.41 Ha
iii) Mohuldih Mine 288.20 Acres iv) Jaduguda 959.34 Acres v) Turamdi Mine 557.18
Acres vi) Mohuldih Mine – 288.20Acres
b) M/s Indian Rare Earths Ltd. (IREL) - 2 Nos
i) NK Block II EE Ilmenite Mine 67 Ha, Chavara, Kerala
ii) Manavalakuruchi (7.06.0 Ha), Ilmenite Mine, Kanyakumari dist., Tamil Nadu.
c) M/s Kerala Minerals and Metals Ltd (KMML): - 1 No. Chavara, Kerala over an extent of
203.802 Ha (review mining plan)
d) Attended meetings on “Draft Format of Prospecting (Scheme, Year & Final Report) along
with other members on during August,2020
e) Attended meetings for discussions & scrutiny of mining plans in r/o geological reports of
Kakinada, Mining plan of Manavalakuruchi (7.06 Ha), GSI reports on REE exploration in r/o
Mincheri Block, Raichur dist, Karnataka and Ambadongar-Gujarat along with other
members.
vi) Associated in the monthly monitoring of pH on the toxic waste water samples generated
from Tanks-1 and 4 received from Engineering Services Group. The effluent samples
recorded 6.4 – 8.0 pH value which is within the prescribed limit.
vii) Attended “Vishwa Hindi divas” lecture on 13th Jan & Vigilance awareness lecture on 14th
Jan.2020.
viii) Attended 71st Annual Day Celebrations of AMD at HQ, Hyderabad.
ix) Work from Home on lockdown period due to COVID- 19: During the lockdown
period (23/03/20 to 14/04/20, 16/04/20 to 19/04/20 & 21/04/20 to 07/05/20) as part of
work from home, preparation of Laboratory sample investigation reports and Literature
consultation/ research papers/ scientific literature pertaining to beneficiation of RMRE
minerals and extraction of Lithium from brine were referred through internet websites.
x) Associated with Incharge, MPU, RMRE and attended EGDMS review meetings,
uploaded Monthly Reports of MPU in the updated EGDMS portal.

35
xi) Associated with Incharge, MPU on the discussions of Achievements of the Mineral
Processing Unit 2019-2020 with Director, Additional Directors & other members on 27-
10-2020.

xii) Associated in the updating of purchase folders for procurement of Laboratory items –
Jaw crusher, Wet Low Intensity Drum Magnetic Separator, Desk top computer etc for
Mineral Processing Unit.
xiii) Pre-dispatch inspection of equipment for MPU lab.: Attended Pre-dispatch
inspection along with Incharge, MPU, RMRE on 1 0th September 2020 for supply of :- i)
Wet low intensity drum magnetic separator, ii) Ro-tap sieve shaker, iii) Flotation cell at
the premises of Insmart Systems, Moosapet, Hyderabad. The items were supplied and
installed in MPU Lab., Hyderabad on 22nd September, 2020.

(जी.वी.एस.उमामहे श्वर
राव/G.V.S.Umamaheswara Rao)
वैज्ञानिक अधिकारी डी /Scientific Officer ‘E’
EC No. 6066.

36