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Minerals Engineering, Vol. 14, No. 1, pp.

1-12, 2001

Pergamon

2000 Published by Elsevier Science Ltd


All fights reserved
0892-6875/01/$ - see front matter

0892-6875(00)00156-4

EVALUATION OF A DIAGNOSTIC LEACHING TECHNIQUE FOR GOLD IN


NATIVE GOLD AND GOLD _+SILVER TELLURIDES*
K. J. HENLEY ~, N.C. CLARKE I and P. SAUTER*
~mdel Limited, Osman Place, Thebarton, South Australia 5031, Australia
E-mail: khenley@amdel.com
q[ Imtech Pty Ltd, 2 Lindeith Court, Sandy Bay, Hobart, Tasmania 7005, Australia
-~Homestake Gold of Australia Limited, 2 Mill Street, Perth, Western Australia 6000, Australia
(Received 16 May 2000; accepted 17 October 2000)

ABSTRACT
A detailed investigation of the stability in cyanide solutions of native gold and gold ~ silver
teUurides in a flotation concentrate from the Golden Mile, Kalgoorlie, has been undertaken to
assess whether leaching under different conditions can be used to quantify the distribution of Au
between native gold and gold i- silver tellurides, as suggested by, for example, Chryssoulis and
Cabri (1990).
The leaching was carried out on +20 Inn native gold and gold ~ silver tellurides separated from a
high-grade flotation concentrate and then diluted with barren quartz. The material leached assayed
270 ppm Au and 118 ppm Te. About 77% of the Au was present as native gold (largely liberated)
and about 23% was in gold i- silver tellurides (predominantly calaverite with trace petzite and Aubearing hessite, also largely liberated). The grainsize of the gold-bearing minerals was mainly in
the range 20/~n to lOOpm. The leach conditions used were:Stage 1:
Stage 2:

Leaching in dilute cyanide (0.1%) at pH 9.5for 24 hours to dissolve native gold but
not gold :~silver tellurides.
Leaching the residue from Stage 1 in strong cyanide (2%) at pH 12.5for 96 hours to
dissolve gold ~ silver tellurides.

Extractions of native gold and gold i-silver tellurides in the two stages of leaching were found to be
as follows:
Mineral

Native gold
Calaverite
Au-bearing
hessite
(and petzite)

% Extracted
in
Stage I

% Extracted in
Stage 2

94
6
53

5
11
40

* Presented at Hydromet 2000, Adelaide, Australia, April 2000

Total %
extracted
in Stages 1
and 2
99
17
93

K.J. Henleyet al.


The results showed that the bulk of the native gold dissolved in the Stage 1 leach (weak cyanide,
moderate pH), along with about half the hessite and petzite but hardly any of the calaverite. The
estimate of Au in native gold from the Stage 1 leach corresponded fairly closely to the native gold
content as the hessite/petzite concentrations were low. However, although the Stage 2 leach (strong
cyanide, high pH) dissolved almost all the remaining hessite/petzite, only a small proportion o f the
calaverite dissolved.
The main conclusions of the investigation are that calaverite is very refractory to cyanidation, much
more so than hessite/petzite, and that the diagnostic leaching procedure studied did not provide a
good estimate of Au in gold 4-silver tellurides. For the diagnostic leach procedure to be effective, a
treatment, such as chlorination, which breaks down calaverite prior to the Stage 2 cyanidation is
required. 2000 Published by Elsevier Science Ltd. All rights reserved.

Keywords
Gold ores; cyanidation; hydrometallurgy; leaching; ore mineralogy
INTRODUCTION
The solubility of gold + silver tellurides in cyanide solution has been debated for many years but there is
relatively little definitive experimental work in the technical literature on the subject. It is generally agreed
that gold + silver tellurides dissolve at a slower rate than native gold and electrum (Marsden and House,
1992; Cornwall and Hisshion, 1976; Cathro and Walkley, 1961) and leaching tests on synthetic sylvanite
(AuAgTe4) and calaverite (AuTe2) have shown low gold extractions (Lu and Lawson, 1994; Padmanaban
and Lawson, 1991). However, leaching rates can be increased by ultrafine grinding (Liddell and Dunne,
1988,1989), increasing the pH to 12.0 to 12.5 (Jayasekera et al., 1988, 1991) and use of oxygen rather than
air as oxidant (Jackman and Sarbutt, 1990). Chryssoulis and Cabri (1990) use the difference in Au
extraction at pH 10.5-11.0 and 12.0-12.5 as a measure of the Au attributable to gold + silver tellurides and
this method can be considered to be an example of diagnostic leaching.
Diagnostic leaching involves a series of leaches, each designed to destroy specific minerals (preferably
only one), followed by cyanidation of the residue from each stage to measure the amount of gold released
from the mineral,s) at each stage (Bruce, 1976; Tumilty et al., 1987; Lorentzen and Van Deventer, 1992;
Lorentzen, 1995). Table 1 from Lorentzen (1995) summarises various pre-treatment leach stages and the
minerals destroyed. The sequence of leaches used is designed on the basis of knowledge of the mineralogy
of the sample.

TABLE 1 Selective pre-treatment leach stages and the minerals destroyed


(from Lorentzen, 1995)
Pre-treatment stage
1
NaCN washes
2
NaCN
3
Na2CO3
4
HC1
5
HC1/SnCI2
6
H2SO4
7

FeC13

8
9
10
11

HNO3
Oxalic acid washes
HF
Acetonitrile elution

Minerals likely to be destroyed


Precipitated gold
Gold
Gypsum and arsenates
Pyrrhotite, calcite, dolomite, 8alena, goethite, calcium carbonate
Calcine, hematite, ferrites
Uraninite, sphalerite, labile copper sulphides, labile base metal
sulphides, labile pyrite
Sphalerite, galena, labile sulphides, tetrahedrite,
sulphide
concentrates
Pyrite, arsenopyrite, marcasite
Oxide coatings
Silicates
Gold adsorbed on carbon, kerogen, coal

Evaluationof diagnosticleachingtechniquefor gold

A disadvantage of diagnostic leaching is that the pre-treatment leach stages are generally not specific to a
single mineral and may dissolve several minerals, or partially dissolve several minerals to different extents.
This complicates the interpretation of the leaching/cyanidation data but can be overcome to a certain extent
by analysing the leach liquors for elements characteristic of the minerals being leached (e.g., Pb for galena,
Zn for sphalerite) and using simultaneous equations and a knowledge of the mineralogy to calculate the
gold distribution ;among the minerals (Tumilty and Schmidt, 1986). However, although the leach sequence
selected is based on the mineralogy of the sample, there is little in the published literature on diagnostic
leaching to indicate that the mineralogy of the residue from each leaching stage has been studied to confirm
the assumptions as to which minerals have been leached. In our investigation of diagnostic leaching to
quantify the Au distribution among native gold and gold + silver tellurides, we have addressed this problem
by quantifying gold mineral proportions before and after each stage of leaching, so that we have a direct
measure of the extent of dissolution of individual gold minerals.
Our investigation, which was carried out for Kalgoorlie Consolidated Gold Mines Pty Ltd (KCGM), was to
test the validity of a diagnostic leach procedure for quantifying the Au attributable to native gold and gold
+ silver tellurides in ores and mill products from the Golden Mile, Kalgoorlie. The basis of this procedure,
which is similar to that used by Chryssoulis and Cabri (1990), is to leach in dilute cyanide (0.1%) at pH 9.5
for 24 hoursto dissolve native gold but not gold + silver tellurides (Stage 1), followed by a strong cyanide
(2%) leach at pH 12.5 for 96 hours to dissolve gold + silver teUurides (Stage 2). A summary of the results
of this investigati,an was given in Henley et al. (1995) and this paper gives the detailed results.

EXPERIMENTAL PROCEDURE

The starting material for the investigation was a re-cleaner concentrate obtained by laboratory flotation of
over 60 kg of KCGM plant flotation concentrate with a head grade of approximately 37 ppm Au and 47
ppm Te. The re-cleaner concentrate assayed 1466 ppm Au and 677 ppm Te and contained 53% of the Au
and 19% of the T,~ in the plant flotation concentrate.
The re-cleaner concentrate was screened at 20 Ixm and from the +20 ~tm fraction a small amount of very
high grade telluride/gold concentrate containing predominantly liberated native gold and gold + silver
tellurides was prepared using a combination of heavy liquid, magnetic and magnetohydrostatic separation
methods. This telluride/gold concentrate represented the non-magnetic fraction with a specific gravity
greater than 6.5 and assayed 43.5% Au and 19.03% Te.
The subsequent investigation carried out on the telluride/gold concentrate is summarised in Figure 1.
A polished section was prepared of the telluride/gold concentrate and selected mineral grains were circled
and analysed quantitatively by electron microprobe. Some of these analysed grains were then used by
CSIRO to calibrate QEM*SEM (now known as QEMSCAN) to identify and quantify the proportions of the
various gold + silver tellurides present. A full QEM*SEM analysis was then carried out on the
telluride/gold concentrate to quantify the proportions of all minerals present.
Because of the very small weight (<1 g) of telluride/gold concentrate available, cyanide leach tests were
carried out on telluride/gold concentrate diluted with +20 ~tm ground quartz. The dilution factor was
1:1613. Riffled portions of the diluted telluride/gold concentrate were analysed for mercury-soluble Au,
mercury-insoluble Au, total Au and a wide range of elements by ICP-OES.
A riffled portion of the diluted telluride/gold concentrate was subjected to 24 hours cyanide bottle-roll
leaching nominally to extract native gold (termed the Stage 1 leach). Leaching was carried out as specified
by KCGM at 40% solids in distilled water, pH 9.5 and 0.1% NaCN initial concentration. Cyanide
concentration decreased to 0.048% NaCN after 24 hours, at which point the recorded pH was 9.67,
Sulphuric acid was added during this stage to maintain pH control.

K.J. Henleyet al.

Chemical

__ Che~cal
analym

analysis

Mmeragt~hy
QEM*SF.IVl
>2.96spA~
~ysis
Dilulioa
with
quartz

Stage1
lcJtch

Stage2
laeh

Fig. 1 Flowsheet for processing the teUuride/gold concentrate.


On completion of the Stage 1 leach, the liquor was analysed for Au and a range of other elements and the
residue was filtered, washed, dried and rotary subsampled to give portions which were analysed for
mercury-soluble Au, mercury-insoluble Au, total Au and a wide range of elements. A portion was
separated centrifugally in a heavy liquid of specific gravity 2.96 to concentrate residual heavy minerals
(from the quartz diluent) for microscopic study.
The major portion of the residue from the Stage 1 leach was subjected to 96 hours strong cyanide bottle-roll
leaching nominally to extract gold + silver tellurides (termed the Stage 2 leach). Leaching was carried out
as specified by KCGM at 40% solids in distilled water, pH 12.5, 2.0% NaCN initial concentration and 1
kg/t PbO. The NaCN concentration decreased to 1.74% NaCN after 96 hours, at which point the recorded
pH was 12.54.
On completion of the Stage 2 leach, the liquor was analysed for Au and a range of other elements and the
residue was filtered, washed, dried and rotary subsampled to give portions which were analysed for
mercury-soluble Au, mercury-insoluble Au, total Au and a wide range of elements. A portion was
separated centrifugally in a heavy liquid of specific gravity 2.96 to concentrate residual heavy minerals
(from the quartz diluent) for microscopic study.
The >2.96 sp. gr. products from the residues from Stages 1 and 2 were examined mineragraphically and the
mineral proportions were quantified by QEM*SEM analysis.

MINERALOGY
The gold + silver telluride minerals identified in the telluride/gold concentrate were calaverite (AuTe2),
petzite (AgaAuTe2) and Au-bearing hessite ((Ag,Au)2Te), with calaverite predominating. Quantitative
electron-probe microanalyses of typical grains of native gold and the gold + silver tellurides are given in
Table 2, from which it can be seen that there is some variability in the Ag content of native gold, from
4.24% to 15.54% with an average of 7.45%. There is also some variation in the compositions of Au-bearing
hessite and calaverite. The native gold and gold + silver tellurides were predominantly liberated and
between 100 ~tm and 20 ktm size. Other minerals present in significant proportions in the telluride/gold
concentrate included coloradoite (HgTe), altaite (PbTe), pyrite, sphalerite, galena, tetrahedrite, pyrrhotite,
chalcopyrite and arsenopyrite. A photomicrograph of a typical field is given in Figure 2.

Evaluationof diagnosticleachingtechniquefor gold

TABLE 2 Electron-probe microanalyses of gold m i n e r a l s


Weight, %

Grain
No.

Au

Ag

Te

Suggested formula

Atomic proportions, %
Total

Au

Ag

Te

Au

Ag

(Au

Te

Total

+Ag)

I
Native gold
1
2
3
4
5
6
7
8
9
10
11
Avge

83.49
84.09
91.59
92.64
91.49
93.14
92.83
91.75
93.76
94.83
93.78
91.22

15.54
13.94
"7.06
6.82
6.70
45.29
6.16
6.13
,1.67
,1.38
,1.24
'7.45

NA*
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA

99.03
98.03
98.65
99.46
98.19
99.43
98.99
97.88
98.43
99.21
98.02
98.67

0.75
0.77
0.88
0.88
0.88
0.89
0.89
0.89
0.92
0.92
0.92
0.87

0.25
0.23
0.12
0.12
0.12
0.11
0.11
0.11
0.08
0.08
0.08
0.13

1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA

1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00

34.7
34.8
34.6
33.3
34.0
34.3

0.31
0.33
0.35
0.40
0.41
0.36

3.45
3.42
3.43
3.61
3.48
3.48

3.76
3.75
3.78
4.01
3.88
3.84

2.00
2.00
2.00
2.00
2.00
2.00

5.76
5.75
5.78
6.01
5.88
5.84

29.3

1.12

3.71

4.83

2.00

6.83

27.5
5.2
67.3
31.5
0.9
67.6
3 i.6
0.8
67.6
3 ! .8
0.9
67.3
3 !.6
0.8
67.6
32.1
0.4
67.5
31.0
1.5
67.5
*NA = not analysed.

0.82
0.93
0.93
0.95
0.93
0.95
0.92

0.15
0.03
0.02
0.03
0.02
0.01
0.04

0.97
0.96
0.96
0.97
0.96
0.96
0.96

2.00
2.00
2.00
2.00
2.00
2.00
2.00

74.6
76.8
87.7
88.1
88.2
89.0
89.2
89.1
91.7
92.2
92.4
87.2

25.4
23.2
12.3
11.9
11.8
11.0
10.8
10.9
8.3
7.8
7.6
12.8

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA

Au-bearing hessite
12
13
14
15
16
Av~e

8.97
9.41
9.90
11.06
11.29
10.13

53.93
53.30
53.88
54.77
53.19
53.81

37.02
36.90
37.10
35.85
36.19
36.61

99.92
99.61
100.88
101.68
100.67
100.55

5.4
5.7
6.0
6.6
6.9
6.1

17

24.35

4.4.16

28.20

96.71

16.4

59.9
59.5
59.4
60.1
59.1
59.6
Petzite
54.3
Calaverite

18
19
20
21
22
23
Avge

37.13
41.42
41.53
41.57
41.75
41.82
40.87

13.83
0.63
0.58
0.63
0.56
0.32
1.09

58.80
57.63
57.58
56.92
57.88
56.98
57.63

99.76
99.68
99.69
99.12
100.19
99.12
99.59

2.97
2.96
2.96
2.97
2.96
2.96
2.96

In both the Stage 1 and Stage 2 residues, calaverite was the main gold-bearing mineral present, with
virtually all of the native gold having dissolved during eyanidation. The calaverite was present in both
residues as angular and, in the case of the Stage 2 residue, slightly rounded particles showing little, if any,
marginal corrosion by cyanide (Figures 3-7).

K.J. Henleyet al.

Fig. 2

General field of view in reflected light of the telluride/go!d concentrate. The field contains native
gold (N), calaverite (C), coloradoite (O), Au-bearing hessite (H), petzite (P) and pyrite (Y). The
native gold commonly shows flattened and irregular shapes.

Fig. 3 Residue from Stage 1 (24 hours leach). The field contains three particles of calaverite (C).
Mineralogical analyses of the telluride/gold concentrate and the >2.96 sp. gr. products of the Stage 1 and
Stage 2 residues are given in Tables 3, and Table 4 gives the calculated chemical compositions Of the
materials based on the QEM*SEM analyses.

Evaluationof diagnosticle~clain$techniquefor gold

Fig. 4

Enlargenaent of the calaverite particle shown in upper right of Figure 3. The calaverite shows
minimal evidence of marginal dissolution by cyanide.

Fig. 5

Residue from Stage 2 (96 hours leach). A particle of calaverite shows rounded margins possibly
indicating some marginal dissolution by cyanide.

Using the data in Table 3 and the mercury-soluble Au values for the Stage 1 and Stage 2 residues (12.2ppm
and 1.53ppm Au respectively), it is possible to calculate the Au distributions among the various goldbearing minerals (Table 5). This shows that native gold accounted for ~77% of the total Au in the
telluride/gold concentrate with calaverite accounting for the bulk of the remainder. In the Stage 1 and Stage
2 residues, calaverite accounted for most of the Au.

K.J. Henleyet al.

Fig. 6

Residue from Stage 2 (96 hours leach). An angular particle of calaverite shows no obvious
evidence of marginal dissolution by cyanide.

Fig. 7

Residue from Stage 2 (96 hours leach). A calaverite particle (C) shows possible slight evidence
of marginal dissolution by cyanide (rounding, presence of marginal serrations). The altaite (A)
particle shows more evidence of such dissolution (well developed marginal serrations).

Evaluationof diagnosticle~hingtechniqueforgold

TABLE 3 Mineralogical compositions determined by QEM*SEM


Gold/telluride
Concentrate

Mineral

Native gold, %
Calaverite, %
Au-bearing hessite and petzite, %
Hessite, %
Coloradoite, %
Altaite, %
Pyrite, %
Pyrrhotite, %
Chalcopyrite, %
Sphalerite, %
Galena, %
Arsenopy~dte, %
Tetrahedrite, %
Other minerals, %
Total, %
*QEM*SEM data on the >2.96 sp. gr. products

Stage 1
residue*

Stage 2
residue*

36.96
23.92
29.98
22.28
2.13
1.32
0.16
1.01
1.23
0.03
10.21
9.53
10.24
1.32
1.29
3.27
15.87
22.73
24.70
0.13
0.36
3.30
0.64
0.71
0.78
2.67
2.24
3.43
1.33
1.20
2.19
0.18
0.13
0.11
2.22
3.70
3.26
1.97
25.01
26.26
100.00
100.00
100.00
after recalculation free of -25% c uartz in these products.

TABLE 4 Chemical compositions calculated from QEM*SEM data


Element

Gold/telluride
Stage 1
Stage 2
concentrate
Residue *
residue *
43.93
12.88
9.34
Au, %
Te, %
19.26
22.11
18.00
Ag, %
5.65
2.34
0.88
Hg, %
6.25
5.82
6.26
0.63
0.92
0.86
Cu, %
1.85
Pb, %
1.97
3.90
Zn, %
1.53
1.83
2.34
As, %
0.21
0.22
0.20
Sb, %
1.05
1.74
1.57
10.33
S,%
14.69
16.98
*QEM*SEM data on the >2.96 sp. gr. products after recalculation free of -25%
TABLE 5 Gold distributions among various gold-bearing minerals

Telluride/gold concentrate
Stage 1 residue
Stage 2 residue

Native
gold
76.7
15.8
3.1

Au distribution (%) among mineralogical sites


Calaverite
Au-bearing hessite &
petzite
22.8
0.5
83.2
0.9
96.7
0.2

Total
100.0
100.0
100.0

CYANIDATION RESULTS
Table 6 summarases the cyanide extraction data for Stage 1, Stage 2 and Stages 1+2 relating to mercurysoluble Au (i.e., liberated or exposed native gold), mercury-insoluble Au (i.e., Au in gold + silver tellurides
and in occluded native gold), total Au (mercury-soluble Au plus mercury-insoluble Au) and Te in the
diluted telluride/gold concentrate, which assayed 270 ppm Au and 118 ppm Te.

10

K.J. Henley et

al.

TABLE 6 Stage cyanidation extractions of various types of gold and tellurium


Stage extraction, %*
Stage 1
Stage 2
Stage 1 + Stage 2
Mercury-soluble Au
93.6
87.4
99.2
Mercury-insoluble Au
27.9
12.5
36.9
Total Au
73.9
25.5
80.5
Te
0.2
8.9
9.1
*Percentage in the feed to a stage extracted by the stage.
Using the data in Tables 3 and 6 it is possible to calculate the amounts of Au in native gold, calaverite and
Au-bearing hessite (and petzite) in the head, the residue after Stage 1 and the residue after Stage 2, and
hence the proportion of each mineral leached after 24 hours and 96 hours. These are given in Table 7 and
illustrated in Figure 8 and show that most (94%) of the native gold (with very little of the gold + silver
tellurides) was extracted in Stage 1 but that only 11% of the calaverite and 40% of the Au-bearing hessite
(and petzite) were extracted in Stage 2.
The evidence clearly indicates that the Stage 2 leach was relatively ineffective in dissolving calaverite and
the photomicrographs of calaverite particles in the Stage 2 residue (Figures 5 - 7) show little, if any,
evidence of marginal dissolution, as do those in the Stage 1 residue (Figures 3 and 4).
TABLE 7 Cyanide extractions of gold minerals from the telluride/gold concentrate (diluted)
Native gold

In head
Extracted in Stage 1
In Stage 1 residue
Extracted in Stage 2
Extracted in Stages 1 + 2
In Stage 2 residue

207.09
194.89
12.20
10.67
205.56
1.53

In head
Extracted in Stage 1
In Stage 1 residue
Extracted in Stage 2
Extracted in Stages 1 + 2
In Stage 2 residue

100
94
6
5
99
1

Au-bearing hessite
and petzite
Au, p ~m in mineral
1.35
61.56
0.71
3.90
57.66
0.64
0.54
6.76
1.25
10.66
50.90
0.10
Au distribution, % in mineral
100
100
53
6
47
94
40
11
17
93
83
7

Calaverite

Total

270.0
199.50
70.50
17.97
217.47
52.53
100
74
26
7
81
20

CONCLUSIONS
Our investigation has tested a diagnostic leach procedure to quantify Au in native gold and in gold + silver
tellurides in a telluride/gold concentrate in which the Au is present in native gold (~77%), calaverite
(-23%) and Au-bearing hessite and petzite (<1%).
The Stage 1 leach (0.1% NaCN, pH 9.5, 24 hours) dissolved most of the native gold and about half of the
Au-bearing hessite and petzite but very little of the calaverite. Because Au-bearing hessite and petzite
accounted for very little of the total Au in the sample examined, the Stage 1 extraction of Au provided a
good estimate of the amount of Au present in native gold.

Evaluationof diagnosticleachingtechniquefor gold

11

Au-beaflng hesslte
and petzlte

;
Native gold
100

Calaverite

In
to,:l
sample

Gold ex~action

~////////////////////~

u)

Exlrscted In Stage 2

i '

I .

Exlmolecl in Stage 1

20

0
0

20

40

60

100

80

GOLD [XSTRIBUTION(*/*)~IONG ~ C N .

SITES

Fig. 8 Mineralogical distribution of gold in the telluride/gold concentrate.


The Stage 2 leach (12% NaCN, pH 12.5, 96 hours) dissolved most of the remaining native gold, Au-bearing
hessite and petzite but only very little of the calaverite. The Stage 2 extraction of Au did not therefore
provide a good estimate of the amount of Au in gold + silver tellurides.
It is concluded that, overall, the diagnostic leach procedure tested was not effective in quantifying the
amount of Au gold + silver tellurides in the KCGM material because of the refractoriness of calaverite. The
refractoriness of calaverite found in the present investigation confirms previous works on synthetic
calaverite by Padmanaban and Lawson (1991). For the diagnostic leach procedure to be effective, a
treatment, such as chlorination (Cornwall and Hisshion, 1976), which breaks down calaverite prior to the
Stage 2 cyanidation is required.

ACKNOWLEDGEMENTS
We wish to thank the management of Kalgoorlie Consolidated Gold Mines Pty Ltd and Amdel Limited for
permission to publish this paper and G Wilkie and the QEM*SEM group at the CSIRO Division of
Exploration and Mining for provision of the QEM*SEM analyses.

REFERENCES
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