TECHNICAL REPORT

IMPALA PLATINUM LTD - REFINERIES

BASE METAL REFINERIES
PO BOX 222
SPRINGS
1560

Distribution: Senior Manager: Operations

Manager: BMR
Manager: Technical
Plant Manager(s)
Author
Technical Library
INVESTIGATION OF NICKEL SEEPAGE INTO JAROSITE SOLIDS WASTE
1. Report Reference BMR-03-030
number
2. Report Category Investigation
3. Report Objective To investigate operating conditions and approach to establish if there
has been process perturbations or deviations which could have
prompted high nickel content being reported in filter press FP2176
solids
4. Project Requested Plant Manager: Leach/PGM
by
5. Project Performed M Ramonotsi
by
6. Inclusive Dates April 2003 — June 2003
7. Report Written by M Ramonotsi
8. Method Analysis of log-sheet data and plant operators interviews
9. Results Operating conditions may be responsible for high nickel in filter press
FP2176 solids, and washing may be insufficient.
10. Recommendations The extending of filter press wash period need to be investigated and
possibly the warming of the wash water. However, concerns are the
excessive water that will be introduced in the system. Recycling of such
water back to ball mill and other areas that may require process water
could be considered.
11. Comments

__________________________ __________________________ __________________________

M RAMONOTSI R RAMKUMAR / B HALL T SPANDIEL, PrEng
Chemical Engineer Plant Manager - BMR Projects Manager: BMR
Plant Manager – Leaches/PGM
 SYNOPSIS
Jarosite plant aims to remove as much as possible iron, arsenic, and lead as solid waste from
nickel sulphate solution without slippage of nickel to this waste. The removal of solid waste as
ammonium jarosite ensures that the precipitate formed is easily filterable from nickel solution.
However, this process requires careful control of acid profile in the jarosite autoclaves to prevent
significant formation of goethite/haematite as this can cause the filter press to clog prematurely.
Moreover, if acid profile is not properly managed in the autoclaves, basic nickel sulphate that is
relatively insoluble could be formed and nickel can be lost as stable precipitate with jarosite solids
at the filter presses. It is also important to maintain the nickel solution at high temperature to
prevent crystallisation of nickel sulphate because the filter press can trap the crystals. Proper
washing of jarosite solids in the filter press is essential to remove any nickel solution that might
have been occluded by the solids.
Last couple of months, nickel content in the solids coming out of the filter press FP2176 has been
fluctuating above specified limit causing considerable amount of nickel loss with jarosite solids. It
was therefore felt necessary to investigate operating conditions and approach to establish if there
have been process perturbations or control deviations, which could have prompted high nickel
content being, reported in filter press solids. This report has explored some findings and
attempted to recommend some modifications that could minimise nickel content in the filter press
solids.
Based on the findings and discussions of this report, it was felt that:
 Amount of total metal does not have an effect on nickel content in jarosite waste solids
 Poor maintenance of acid profile in the jarosite autoclave could have been responsible for
either the formation of basic nickel sulphate or goethite/haematite depending whether the free
acid was too high or too low respectively.
 Insufficient filtering time in the filter press may have led to low solid content in the filter press
thereby creating channels that makes it difficult for solids to be washed properly.
It has thus been recommended that the solid washing efficiency be investigated on a laboratory
scale. If the results of nickel content in the filter press FP2176A/B material improve by extended
washing in the laboratory conditions it would be confirmed whether washing was insufficient or
not. The investigation should also study the effects of temperature on efficient washing. At low
temperature, nickel sulphate solution tends to precipitate out making the washing of jarosite
waste solids inefficient. Pre-heating of wash water with steam could be considered to elevate
wash water temperature in the plant.
If controlled washing of these solids is still not decreasing nickel content in the solids, the solids
will then need to be analysed for basic nickel sulphate. The presence of basic nickel sulphate is a
direct reflection of acid profile control and measures will need to put in place to ensure good
management of acid profile in the jarosite autoclaves.
 TABLE OF CONTENTS
INTRODUCTION....................................................................................................................1

BACKGROUND.....................................................................................................................1

CURRENT SITUATION.........................................................................................................2

METHOD OF INVESTIGATION............................................................................................3

FINDINGS..............................................................................................................................3

DISCUSSION OF FINDINGS................................................................................................6

CONCLUSIONS.....................................................................................................................7

RECOMMENDATIONS..........................................................................................................7

BIBLIOGRAPHY....................................................................................................................7

APPENDICES........................................................................................................................8
 LIST OF FIGURES

FIGURE 1: THE GRAPH OF NICKEL CONTENT IN JAROSITE WASTE SOLIDS FOR MAY 2003.............1

FIGURE 2: THE FREQUENCY DISTRIBUTION OF NICKEL CONTENT IN JAROSITE SOLID FILTER

PRESS FP2176A/B FROM THE BEGINNING OF JULY 2003 TO THE 5TH AUGUST 2003..............................2

FIGURE 3: THE GRAPH OF TOTAL METAL VERSUS NICKEL CONTENT BEFORE AND AFTER
JAROSITE AUTOCLAVES.............................................................................................................................................3

FIGURE 4: THE GRAPH OF PH IN THIRD COMPARTMENT OF THE TWO JAROSITE AUTOCLAVES

OPERATED IN SERIES...................................................................................................................................................4

FIGURE 5: THE GRAPH OF AMOUNT OF TOLLED NICKEL SULPHATE ADDED VERSUS NICKEL
CONTENT IN JAROSITE SOLIDS................................................................................................................................4
 LIST OF TABLES

TABLE 1: TABLE OF NICKEL CONTENT AND TOTAL METALS IN VARIOUS TANKS..............................8

INTRODUCTION
Last couple of months, nickel content in the solids coming out of the filter press FP2176 has been
fluctuating above specified limit.

Nickel Content in FP2176 Solids

12.00

9.00
Ni Content %

Target Upper limit

6.00

3.00

0.00
03/04/24 03/05/02 03/05/10 03/05/18 03/05/26

Figure 1: The graph of nickel content in Jarosite waste solids for May 2003
The nickel content in these solids has once been reported to a high of 9.53% on 20 may 2003.
Considering nickel is preferred to stay below 3% level these observed rises of nickel content in
the filter press solids has called for an investigation. There has already been attempts to ensure
the process controller adhere to operating procedure but little improvement if any has been
observed. It was therefore felt necessary to investigate operating conditions and approach to
establish if there has been perturbations or deviations which could have prompted high nickel
content being reported in filter press solids. This report will explore some findings and attempt to
recommend some modifications that could minimise nickel content in the filter press solids.

BACKGROUND
BMR operates two-stage filter pressure acid leach for treatment of PGM containing matte. The
major constituent of the matte is nickel at roughly 47% and followed copper at 32%. The acidic
nickel sulphate leach solution contains significant levels of iron, arsenic, and trace amount of
lead. These elements must be removed from nickel solution prior to recovery of nickel powder by
hydrogen reduction.
At existing circuit the nickel rich solution from first stage leach is adjusted to an acid condition of
15g/L using sulphuric acid. The acidic solution is then fed to a three-compartment autoclave, to
which oxygen is added, at a filter pressure of 700 kPaG and temperature 140 oC. The acidity is
decreased gradually from 12.0g/L to 1.0g/L through the autoclave using ammonia.
Iron is removed in two stages, firstly by oxidation of the ferrous ion to the ferric, followed by
conversion to ammonium jarosite using aqueous ammonia and oxygen. Secondly, the arsenic is
precipitated with iron as ferric arsenate. The iron is also a good collector of lead, which
precipitates out as plumbo-jarosite. Hence, the iron, arsenic and lead precipitates are filtered off
and removed from the process as waste. The nickel sulphate solution is then sent to nickel
solution adjustment circuit.
The aim of jarosite plant is to remove as much as possible iron, arsenic, and lead from nickel
sulphate solution with minimal loss of nickel to waste. The removal of iron as ammonium jarosite
ensures precipitate formed is easily filterable from nickel solution. However, this process requires

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careful control of acid profile in the jarosite autoclaves to prevent significant formation of
goethite/haematite as this can present filtration challenges. Moreover, if acid profile is not properly
managed in the autoclaves, basic nickel sulphate could be formed thereby loosing nickel as
stable precipitate with jarosite solids at the filter presses. It is also important to maintain the nickel
solution at high temperature to prevent crystallisation of nickel sulphate because the filter press
can trap the crystals. Proper washing of jarosite solids in the filter press is essential to remove
any nickel solution that might have been occluded by the solids.

CURRENT SITUATION
Samples are taken for every batch that is been dispatched from jarosite filter presses FP2176 for
analysis in the lab. The specification in the jarosite solid is currently desired to be below 3.5% with
nickel content. The higher the content of nickel in these solid the more nickel is being lost to
waste.

Figure 2: The Frequency distribution of Nickel content in jarosite solid filter press FP2176A/B from the
beginning of July 2003 to the 5th August 2003.
The number of times nickel content in FP2176A/B solids have been over the specification have
been traced since the beginning of July 2003 to 5th August 2003 as shown in Figure 2 above.
Figure 2 shows that about 11 times nickel content in the jarosite waste solids was reported at
4.39% and in fact 27 times out of 67 batches nickel was reported off spec. This means roughly
40% of the batches produced on jarosite filter presses were above desired specification for this
period. Again looking at nickel content as depicted in Figure1 for the month of May 2003, we
observe the similar trend of high nickel being lost through jarosite waste solids. This situation has
thus called for investigation to determine why nickel is being lost so much in this section.

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METHOD OF INVESTIGATION
In order to carry out this investigation, a systematic approach was adopted which entails the
following:
− Process operating parameters such as total metals and pH to see if they can be correlated
with high nickel content in the solids of filter press FP2176 would be analysed from the
log-sheet data.
− The effect of amount of tolled nickel sulphate added in copper cementation tank TK2124
would be examined against high nickel content in the FP2176A/B solids by studying log-
sheet data as well.
− The method of washing the solids in the filter press FP2176A/B would be investigated by
way of interviewing process controllers.
− And temperature of solution across the filter press FP2176 would be scrutinised if there
are records available.

FINDINGS
1. In order to examine the effect of operating parameters on nickel content in the filter press
FP2176 solids, an average total metals maintained in a day was determined and plotted
against the nickel content in the filter press solids. The graph shown below shows that
little change in total metal concentration has occurred before and after the jarosite

Total metals before jarosite formation and after

200.00

190.00

180.00

170.00
Total Metals

TM 2170
160.00
TM 2177
150.00

140.00

130.00

120.00
0.00 2.00 4.00 6.00 8.00 10.00
Nickel content %

autoclaves:
Figure 3: The graph of total metal versus nickel content before and after jarosite autoclaves

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 2. The similar plot of pH in the third compartment of the two-jarosite autoclaves was made to
determine the effect of acid profile in the claves. The results below show that the pH was
dropped from around 3.4 to about 1.5 but with high pH level in the last compartment of
jarosite autoclaves resulted with high nickel content in the jarosite waste solids in most
cases.

pH in 3rd compartment of jarosite autoclaves Vs. Nickel content

3.90

3.40

2.90
pH 2175A/3
pH

pH 2175B/3
2.40

1.90

1.40
0.00 2.00 4.00 6.00 8.00 10.00
Nickel Content %

Figure 4: The graph of pH in third compartment of the two jarosite autoclaves operated in series.

3. The amount of nickel sulphate bags added was also correlated with the nickel content in
FP 2176 solids in order to determine if addition of tolled nickel sulphate has an effect on
resulting jarosite waste solids. The results observed shows even when very small amount
of bags were added high nickel could still be reported in the jarosite waste solids.

Number of NiSO4 added vs. Nickel Content

80

70

60

50
# bags added

40

30

20

10

0
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
Nickel Content %

Figure 5: The graph of amount of tolled nickel sulphate added versus nickel content in jarosite solids.

4. The method of washing the solid on the filter press FP2176A/B was found to be consistent
with the operating procedures. The filter presses are washed mostly for one hour with
wash water and then air-dried for four hours. It was however found that the amount of
solids in the filter presses might differ depending on how long the filter presses were kept
on filtration mode. Some random selections of solids from the filter press FP2176A/B were

41480720.doc Page 4 of 8
 examined visually and there was indication of the presence of nickel sulphate crystals. It
was pointed out that sometimes the amount of solids in the filter press were not sufficiently
packed in the filter presses, this could have led to the establishments of channels where
wash water may pass preferentially through the channels and thus resulting in other solid
materials not been washed properly.

5. The temperature across the filter press FP2176 is not measured but the average
temperature in filter press feed tank, TK2150 91oC. There are no records that could be
used to examine the effect of temperature drop across the filter press FP2176A/B on
nickel sulphate precipitation. The solution temperature and wash water temperature would
have some influence on maintaining nickel in solution or re-dissolving any nickel sulphate
that might have precipitated or been occluded within jarosite particles. There is no
systematic recording of nickel content in the wash water and is therefore not possible to
infer if washing was sufficient. Test work is proposed to determine the washing efficiency
of these solids.

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DISCUSSION OF FINDINGS
1. Total metals were not depicting any relevant correlation with respect to nickel content in
the solids collected in the filter press FP2176 as shown in Figure 3. Nickel forms most of
the percentage of total metals in jarosite solution and the relation of total metals with
nickel content in the filter press FP2176 would reveal the possibility of nickel complex
resulting from high nickel filter pressure in the solution. Lack of defined correlation
suggests the absence of such complex influence by nickel concentration in the jarosite
claves.
2. From the findings above, it can be seen from Figure 4, acid profile has influence on nickel
content in the filter press FP2176A/B solids. The pH in the last compartments of the
jarosite autoclave can show if free acid inferred by pH in the autoclave have effect on the
nickel content in the filter press solids or not. In general operators have kept pH well
above 1.4, the higher the pH was in the last compartment, there was a steady increase in
the waste filter solids. The high pH would suggest basic conditions, which are favourable
to formation of basic nickel sulphate, and very low acid favours the formation of
goethite/haematite, which is difficult to filter in the filter presses.
3. The number of bags of nickel sulphate added to the process through TK2124 was found
to have no effect on nickel content in the filter press FP2176A/B as shown in Figure 5.
Positive results would have suggested over-saturation of nickel sulphate in jarosite
solution, which would trigger an easy precipitation of nickel sulphate across the filter press
and would make it difficult to wash the filter press solids.
4. Although washing of the solid is done in accordance with procedures, one hour may
however not be sufficient to wash the solids off nickel completely. It may well be possible
that the solution going through the filter presses lost considerable amount of temperature
that could prompt nickel sulphate to precipitate. If nickel sulphate precipitate, that would
require extended washing of the solids with the possibility of elevating wash water
temperature to facilitate re-dissolving of the precipitates. It is also possible that the jarosite
occluded nickel sulphate that is coupled with drop in temperature across the filter press.
This would again require extended washing of the solids in the filter press. Washing test
work of these solid is recommended to establish the efficiency of waste solid washing.

5. Allowing the filter press to filter for longer period could solve the channels that may have
form due to insufficient materials in the filter press. Process controllers are not able to
maintain consistent filtering period due to production demand, and they are sometimes
forced to drop the cake after putting the filter press online shortly. It is not possible to
establish optimal filter press period since the solution may have varying nickel sulphate
crystals depending on what is been feed in tank TK2170. If TK2170 receive more solution
from nickel plant, it provide challenges for leaches operators to control amount of free acid
strength going into jarosite claves. This could contribute to basic nickel sulphate crystals
being introduced in the jarosite autoclaves.

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CONCLUSIONS
Based on the findings of this report, the following conclusions are drawn:
 Total metal does not have an effect on nickel content in jarosite waste solids
 The amount of tolled nickel sulphate added is also not responsible for high nickel content in
jarosite waste solids.
 Poor maintenance of acid profile in the jarosite autoclave could lead to either the formation of
basic nickel sulphate or goethite/haematite depending whether the free acid was too high or
too low respectively.
 Insufficient filtering time in the filter press could lead to low solid content in the filter press
thereby creating channels that makes it difficult for solids to be washed properly.
 Insufficient washing of these solids may also be responsible for the high nickel reported in the
jarosite waste solids.

RECOMMENDATIONS
Based on the findings and conclusions of this report, the following recommendations are made:
 It is thus recommended that the solution washing period be extend by another hour with the
possibility of using steam to elevate wash water temperature, but plans will need to be made
to deal with excess water being introduced in the system. If the results of nickel content in the
filter press FP2176A/B solids improve by extending the washing period, we would know for
sure if washing was insufficient or not. Plans could be made to recycle filter press FP2176A/B
wash water to other areas that may require process water in order to minimise excessive
introduction of water to the system.
 Basic Nickel sulphate that is mostly pumped from nickel plant into TK2170 could be controlled
by adequate control of pH or free acid in TK2170.
 Pre-heating of wash water with steam could be used to elevate wash water temperature.
 Test work is required in the lab scale to establish the efficiency of washing of these solids.
 If controlled washing of these solids is still not decreasing nickel content in the solids, the
solids will need to be analysed for basic nickel sulphate.

BIBLIOGRAPHY
1. Dynatec Corporation, “Diagnosis of Plant Samples”, in House Project Report for Impala”,
February, 2003.
2. Sherritt Gordon Mine Limited, “Jarosite Precipitation Continuous Miniplant Test”, in House
Project Report for Impala”, July 1985.

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APPENDICES
Table 1: Table of nickel content and total metals in various tanks
Ni % TM 2170 TM 2177 NiSO4 pH 2175A/3 pH 2175B/3
1.50 138.08 124.42 35 1.53 3.21
1.63 195.87 150.87 60 1.99 3.41
1.64 144.92 140.38 40 1.78 3.55
1.70 150.46 139.96 30 1.69 3.29
1.83 139.50 134.71 20 1.69 3.30
1.89 124.07 128.11 10 1.73 3.50
1.92 142.01 133.06 40 1.82 3.28
2.06 143.71 137.67 62 1.77 3.41
2.07 123.70 126.57 20 1.75 3.21
2.37 140.52 127.79 50 1.72 3.38
2.54 139.00 147.22 52 1.97 3.51
2.58 136.18 142.13 46 1.90 3.23
2.77 137.10 131.82 50 1.74 3.37
2.77 135.96 126.71 50 2.01 3.70
2.87 137.40 136.85 70 1.97 3.63
2.96 133.97 142.22 20 1.59 3.52
2.98 133.94 135.37 20 1.94 3.50
3.69 132.74 131.16 6 1.76 3.53
3.92 140.70 142.63 50 1.58 3.39
3.94 141.96 141.25 62 1.62 3.26
4.51 134.15 129.53 0 1.80 3.30
4.53 143.69 144.63 30 1.80 3.43
4.65 136.03 134.94 20 1.88 3.51
4.87 133.17 129.67 24 1.90 3.49
5.00 143.28 131.50 23 1.77 3.42
5.13 130.90 132.99 28 1.77 3.40
5.21 131.29 130.08 28 1.81 3.73
9.53 132.49 132.92 10 1.93 3.50

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