Proceedings

Volume 2

The European Metallurgical Conference is organized by

Base and Precious Metal Losses in Magnetic
Separation of Waste Printed Circuit Boards
Ersin Y. Yazici, Haci Deveci, Ridvan Yazici Ata Akcil
Karadeniz Technical University Suleyman Demirel University
Hydromet B&PM Research Group MMR&R Research Group
Div. of Mineral & Coal Processing Div. of Mineral Processing
Dept. of Mining Engineering Dept. of Mining Engineering
61080, Trabzon, Turkey TR32260, Isparta, Turkey

Keywords: Waste printed circuit boards (WPCB), magnetic separation, ferrous metals,
base/precious metal losses, box-behnken design.

Abstract
Waste of printed circuit boards (WPCB) is of economic interest due to its high content of
base/precious metals (e.g. Cu, Au, Ag, and Pd). Physical separation methods can be implemented to
enrich non-ferrous and precious metal content of WPCB by the separation of non-metals, magnetic
and light metals. This study was undertaken to evaluate magnetic separation of ferrous metals as
well as non-ferrous and precious metal losses during magnetic separation. The effects of magnetic
field (330 - 3800 Gauß), roll speed (36 - 72 m/min) and splitter angle (8 - 25°) on the separation of
ferromagnetic metals (i.e. Fe, Co and Ni) from WPCB (- 3.35 + 0.106 mm) were examined. Pre-
cious metals (Au and Pd), which are also of prime economic interest as well as other metals (Cu, Pb
and Sn) were also followed to quantify the loss of these metals. Response surface methodology (i.e.
Box-Behnken design) was adopted to assess the influence of the factors on separation efficiency of
metals in three levels. A statistical software was used to evaluate the experimental results. Magnetic
field was found to be the most significant parameter improving recovery of ferrous metals with in-
creasing its intensity. However, increasing roll speed and splitter angle adversely affected the sepa-
ration of these metals. Separation of iron and nickel into magnetic fraction was high with up to
96 % and 93 % recoveries, respectively. Cobalt recoveries were relatively lower than that of iron
and nickel (i.e. 12 – 76 %). High losses for copper and precious metals were determined e.g. up to
70 %, 79 % and 60 % for copper, gold and palladium, respectively. Metal losses could be attributed
to the heterogeneous character of WPCB in that metals can be found as alloys and/or coatings,
which can adversely affect their response to magnetic field and hence, separation. It can be con-
cluded from these findings that significant base and precious metal losses is the main detraction to
magnetic separation of WPCB.

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1 Introduction
Recycling/recovery of waste electrical and electronic equipments (WEEE or e-waste) has been
forced by regulations in order to mitigate the adverse effect of WEEE to environment when land-
filled as well as to benefit from its significant economic potential due to high base/precious metal
content [1,2]. For the recovery of metals from WEEE, pyrometallurgical methods are currently ex-
ploited at industrial scale where WEEE constitutes only a small portion (10- 15%) of feed material.
However, pyrometallurgical processes are economically less feasible to treat low-grade waste con-
taining typically < 100 ppm Au [3-6]. Physical separation methods can be used to produce a metal-
rich fraction for subsequent metallurgical processes. These methods rely on the differences in phys-
ical properties e.g. specific gravity, conductivity and magnetic susceptibility for the separation of
metals and non-metals with their advantages of being simple, environmentally sound and low-cost
technologies. However, in physical separation processes, metal losses can be high up to 10 – 35 %,
which may adversely affect process economics [7-11].
Low intensity magnetic separation can be employed to remove ferrous metals with high magnetic
susceptibility such as Fe, Ni and Co (Table 1). The forces acting on a spherical particle exposed to a
magnetic field are magnetic (Fm), gravity (Fg), centrifugal (Fc) and friction force (Ff) (Figure 1 and
Eqs. 1-3) [12-14].
Table 1: Some metals with corresponding magnetic susceptibilities [15-17]
Metals Magnetic peculiarity Magnetic susceptibility X (10-6 cm3 mol-1)
Iron (Fe) Ferromagnetic
Cobalt (Co) Ferromagnetic
Nickel (Ni) Ferromagnetic
Tin (ȕ-Sn, white) Paramagnetic + 0.19
Copper (Cu) Diamagnetic ԟ 5.46
Lead (Pb) Diamagnetic ԟ 23.00
Gold (Au) Diamagnetic ԟ 28.00
Silver (Ag) Diamagnetic ԟ 19.50

Figure 1: Forces acting on a spherical particle in a magnetic field (adopted from Liang [18])

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 Base and Precious Metal Losses in Magnetic Separation of Waste Printed Circuit Boards

Fm = [(Ȥp ԟ Ȥf) / μo] m B ǻB (Ȥp >> Ȥf) (1)

Fg = m g (2)
Fc = m Ȧ2 R (3)
Where Fm: Magnetic force (Newton, N);
Fg: Gravity force (N);
Fc: Centrifugal force (N);
Ȥp : Mass magnetic susceptibility of a particle (m3/kg);
Ȥf : Mass magnetic susceptibility of fluid medium (m3/kg) (zero for air);
m: Mass of a spherical particle (kg);
B: Magnetic flux density (magnetic field) (Tesla, T);
ǻB: Magnetic field gradient (T/m);
g: Acceleration of gravity (9.807 m/s2);
Ȧ: Angular velocity of a drum (rad/s) and
R: Radius of a drum (m).
Magnetic separation of ferromagnetic metals from waste of printed circuit boards (WPCB) has been
reported in the literature [19-22], but metal losses seem to be overlooked in most studies. Although
some researchers [23,24] reported metal losses in magnetic separation tests, there appear to be only
a limited number of comprehensive studies for assessment of the performance of magnetic separa-
tion in detail.
In this study, magnetic separation of ferrous metals as well as non-ferrous and precious metal losses
during magnetic separation was studied in detail. The effects of magnetic field (330 - 3800 Gauß),
drum speed (36 - 72 m/min) and splitter angle (8 - 25°) on the separation of ferromagnetic metals
(i.e. Fe, Co and Ni) from waste of printed circuit boards (- 3.35 + 0.106 mm) were examined using
an experimental design approach i.e. response surface methodology. Behaviour of precious metals
(Au and Pd) as well as other metals (Cu, Pb and Sn) in magnetic separation was also followed to
quantify the loss of these metals. A statistical software was used to evaluate the experimental data.

2 Experimental
2.1 Waste sample
Waste of printed circuit boards (WPCB) used in magnetic separation tests was collected from obsolete
computers (keyboards, motherboards, monitors etc.) (Figure 2a) and then mixed prior to the manual
separation of the board components. WPCB (components removed, ~ 200 kg) was then reduced in
size down to - 3.35 mm in a two-stage crushing operation using a rotary cutting shredder (Figure 2b).
Size distribution of the crushed sample (- 3.35 mm) was presented in Figure 3. Table 2 shows metals
content (Cu, Fe, Al, Pb and Au) of the size fractions obtained from the crushed sample by dry sieving.

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Detailed chemical analysis of WPCB sample is shown in Table 3. The sample contains 18.5 % Cu
and noticeable amount of precious metals with 86 ppm Au, 694 ppm Ag and 97 ppm Pd.

Figure 2: (a) Collected WPCB from obsolete computers , (b) Size reduced (- 3.35 mm) WPCB
(components removed)

Figure 3: Particle size distribution of crushed WPCB (-3.35 mm)

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 Base and Precious Metal Losses in Magnetic Separation of Waste Printed Circuit Boards

Table 2: Metal content of size fractions in WPCB (- 3.35 mm)

Size fraction (mm) Cu (%) Fe (%) Al (%) Pb (%) Au (ppm)
- 3.35 + 2.36 10.1 0.55 1.28 0.40 62
- 2.36 + 2.00 10.2 4.47 1.95 2.47 35
- 2.00 + 1.40 13.6 0.98 0.95 1.89 104
- 1.40 + 1.00 27.2 2.15 0.72 4.15 116
- 1.00 + 0.85 24.6 1.96 0.72 3.46 211
- 0.85 + 0.50 32.1 1.90 0.81 2.99 143
- 0.50 + 0.212 21.0 0.81 1.06 2.82 145
- 0.212 + 0.075 10.7 0.33 0.97 2.74 92
- 0.075 3.20 0.87 1.79 1.55 245

Table 3: Chemical composition of WPCB sample

Cu Fe Ni Al Pb Sn Au Ag Pd
Metal
% g/t
Assay 18.5 2.05 0.43 1.33 2.66 4.91 86 694 97
Fine fraction (- 0.106 mm) was separated using a screen prior to magnetic separation tests. A sample
amount of ~ 100 g (- 3.35 + 0.106 mm) was used in each test. A roll type magnetic separator with per-
manent magnets (Nd-Fe-B), which is able to generate different magnetic fields i.e. 330 - 3800 Gauß was
used in the experiments (Figure 4). Separation tests were carried out in three stages in that the magnetic
fraction obtained in the first stage was further subjected to two subsequent cleaning stages. The final
magnetic and non-magnetic fractions obtained from each test were ground to - 250 μm using an ultra-
centrifugal mill (Retsch ZM 200) prior to hot aqua regia digestion for analysis of metals (Fe, Ni, Co, Cu,
Pb, Sn, Au and Pd) using an atomic absorption spectrometer (Perkin Elmer AAnalyst 400).

Figure 4: Roll type magnetic separator used in the tests (a = 4 cm, b = 7.5 cm, c = 10 cm)

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2.2 Design of experiments

Box-Behnken design (BBD), essentially a type of response surface methodology (RSM) at three lev-
els was adopted for the evaluation of linear/square/interaction effects of magnetic field (330 - 3800
Gauß), roll speed (36 - 72 m/min) and splitter angle (8 - 25°) on the separation of metals from WPCB.
Table 4 presents the parameters with their corresponding coded and actual levels. Design-Expert [25]
software was used for the statistical analysis of the experimental data and production of response sur-
face plots. P-values were used to determine the statistical significance of parameters. Simply, the null
hypothesis is rejected when the P−value is smaller than the selected confidence level (e.g. 95 %,
Į = 0.05). This indicates the statistical significance of the parameter tested [26].
Table 4: Parameters investigated with corresponding coded and actual levels
Low Medium High
Parameters
-1 0 +1
A Magnetic field (Gauß) 330 1860 3800
B Roll speed (m/min) 36 54 72
C Splitter angle (ș, °) 8 16.5 25

Table 5: Experimental layout adopted in the magnetic separation tests

Exp. No. Magnetic field (Gauß) Roll speed (m/min) Splitter angle (ș, °)
1 -1 (330) -1 (36) 0 (16.5)
2 +1 (3800) -1 (36) 0 (16.5)
3 -1 (330) +1 (72) 0 (16.5)
4 +1 (3800) +1 (72) 0 (16.5)
5 -1 (330) 0 (54) -1 (8)
6 +1 (3800) 0 (54) -1 (8)
7 -1 (330) 0 (54) +1 (25)
8 +1 (3800) 0 (54) +1 (25)
9 0 (1860) -1 (36) -1 (8)
10 0 (1860) +1 (72) -1 (8)
11 0 (1860) -1 (36) +1 (25)
12 0 (1860) +1 (72) +1 (25)
13-15 0 (1860) 0 (54) 0 (16.5)

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3 Results and Discussion

The results of magnetic separation tests with metal contents (% or ppm) of magnetic and non-
magnetic fractions as well as metal recoveries (%) are presented in Table 6 (Fe, Ni and Co), Table 7
(Pb and Sn) and Table 8 (Cu, Au and Pd). Recovery of Fe and Ni in magnetic fraction was in the
range of 76 - 96 % and 55 - 93 %, respectively, while cobalt recovery was relatively low i.e. 12 -76 %
(Table 6). Significant losses of base and precious metals were observed in that high portion of copper
(” 70 %), gold (” 79 %) and palladium (” 60 %) was reported in magnetic fraction (Table 8). SEM-
EDS analysis of WPCB sample showed that iron was present as alloyed with Ni/Co or Cr [9]. Lead
and tin recoveries were found to be close to each other (Table 7) indicating similar behaviour in mag-
netic separation. This can be attributed to the presence of Pb and Sn mainly as solder (Pb-Sn alloy) in
WPCB as evidenced by SEM-EDS analysis [9]. High correlation of Pb recovery with Sn recovery i.e.
r = 0.994 was in compliance with these observations. Further, Sn/Pb ratios in magnetic and non-
magnetic fractions were determined to be 1.80 and 1.55, respectively (Table 7), which are close to the
Sn/Pb ratio (i.e. 1.70) in Sn63Pb37 alloy – a commonly used solder type in electronics industry. SEM-
EDS analysis also detected that Pb-Sn alloy is associated with Fe-Ni-Co or Fe-Cr alloys [9].
Table 6: Results of separation tests for Fe, Ni and Co (M: Magnetic; NM: Non-magnetic)
Iron (Fe) Nickel (Ni) Cobalt (Co)
No Content (%) Recovery (%) Content (%) Recovery (%) Content (ppm) Recovery (%)
M NM M M NM M M NM M
1 3.86 0.21 77.8 0.76 0.11 57.5 149 209 11.9
2 2.21 0.20 95.0 0.83 0.13 91.4 225 228 62.5
3 15.6 0.47 76.0 3.53 0.23 59.7 983 188 33.4
4 6.39 0.22 89.0 1.58 0.10 82.1 417 181 39.6
5 11.4 0.33 82.0 3.08 0.16 71.7 599 154 33.5
6 3.29 0.23 92.5 0.95 0.12 87.6 306 172 61.1
7 9.00 0.35 75.7 1.73 0.17 55.1 379 180 20.5
8 4.58 0.17 91.9 1.32 0.08 86.8 398 230 42.1
9 2.14 0.22 96.0 0.54 0.11 92.5 361 292 75.6
10 8.90 0.21 88.9 2.62 0.11 81.2 1077 237 45.8
11 4.86 0.14 93.4 1.49 0.07 89.6 604 378 39.7
12 7.61 0.21 89.0 2.37 0.10 83.3 683 321 31.9
13-15 7.11 0.12 92.7 2.01 0.08 86.9 1471 589 34.1

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Table 7: Results of separation tests for Pb and Sn (M: Magnetic; NM: Non-magnetic)
Lead (Pb) Tin (Sn)
Sn/Pb Ratio
No Content (%) Recovery(%) Content (%) Recovery (%)
M NM M M M M M NM
1 1.17 2.12 9.41 2.19 3.32 11.1 1.88 1.57
2 2.09 3.39 51.0 4.13 5.23 57.2 1.98 1.54
3 2.64 2.30 9.90 4.66 3.55 11.2 1.77 1.54
4 2.88 2.13 27.8 5.45 3.31 31.9 1.89 1.55
5 3.49 2.19 17.1 5.99 3.46 18.3 1.71 1.58
6 2.42 3.11 40.7 4.22 4.49 45.4 1.74 1.44
7 2.74 2.28 12.8 4.67 3.59 13.7 1.70 1.57
8 2.72 2.08 35.5 5.50 3.23 41.8 2.02 1.55
9 2.07 4.28 54.7 3.76 6.36 59.7 1.82 1.49
10 3.92 2.08 26.0 7.94 3.30 31.0 2.03 1.59
11 3.07 2.38 34.6 5.28 3.48 38.4 1.72 1.46
12 3.36 2.63 21.9 5.71 4.39 22.2 1.70 1.67
13-15 3.60 1.89 33.0 5.40 3.48 32.8 1.50 1.84
Table 8: Results of separation tests for Cu, Au and Pd (M: Magnetic; NM: Non-magnetic)
Copper (Cu) Gold (Au) Palladium (Pd)
No Content (%) Recovery (%) Content (ppm) Recovery (%) Content (ppm) Recovery (%)
M NM M M NM M M NM M
1 7.83 16.2 8.37 99.2 79.6 19.0 36.7 127 5.16
2 17.7 19.4 60.5 120 104 66.0 122 137 60.1
3 16.8 24.7 6.13 153 98.2 13.0 80.9 67.4 10.3
4 21.8 15.2 29.1 158 64.0 41.3 157 163 21.6
5 17.7 20.8 9.92 289 85.4 30.4 99.8 109 10.6
6 20.6 16.8 52.0 131 99.2 53.9 103 105 46.4
7 12.5 16.9 8.29 310 93.0 29.0 78.7 108 8.18
8 22.2 15.2 38.1 150 64.3 49.6 115 102 32.2
9 16.9 18.1 70.0 102 69.1 78.7 83.6 179 53.8
10 18.4 14.8 18.8 84.5 80.6 16.4 129 104 18.8
11 23.2 14.8 39.2 180 55.8 57.0 179 144 33.8
12 18.9 17.0 19.7 278 92.3 39.9 87.2 83.6 18.7
13-15 23.4 14.2 33.7 282 59.9 55.2 285 107 51.0

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Metal recovery (%) for Fe, Ni and Co (Table 6), Pb and Sn (Table 7), Cu, Au and Pd (Table 8) was
used as response to establish regression models. The mode of regression coefficients for linear
terms (Table 9) indicated that magnetic field positively influenced the recovery of metals whilst roll
speed and splitter angle had negative impact. The relative magnitude of linear terms also suggests
that magnetic field is the most important parameter affecting the response (Table 9).
Table 9: Regression model terms with corresponding regression coefficients
Regression coefficients
Model Term
Fe Ni Co Pb Sn Cu Au Pd
Constant 93.5 86.9 34.1 33.0 32.8 33.7 55.2 51.0
A- Magnetic field 7.1 13.0 13.3 13.2 15.3 18.4 14.9 15.8
B- Roll speed -2.4 -3.1 -4.9 -8.0 -8.8 -13.1 -13.8 -10.4
C- Splitter angle -1.2 -2.3 -10.2 -4.2 -4.8 -5.7 -0.5 -4.6
AB -1.0 -2.9 -11.1 -5.9 -6.3 -7.3 -4.7 -10.9
AC 1.4 3.9 -1.5 -0.2 0.2 -3.1 -0.7 -3.0
BC 0.7 1.2 5.5 4.0 3.1 7.9 11.3 5.0
2
A -7.7 -12.8 -3.1 -8.1 -6.5 -8.7 -13.8 -16.8
2
B -1.3 -1.4 5.8 -0.3 1.6 1.1 -6.5 -9.9
2
C -0.3 1.2 8.3 1.7 3.5 2.1 -0.6 -9.9
2
R of the model 0.995 0.972 0.942 0.963 0.960 0.963 0.911 0.992
The statistical analysis of linear/square/interaction terms of regression models is presented in Table
10. All the regression models were statistically significant at 95 % confidence level (P < 0.05). The
linear (main) effect of magnetic field on the recovery of metals (%) was significant even at 99 %
(Į = 0.01). Roll speed was determined to be significant at Į = 0.05 for all metals except from Ni and
Co for which roll speed was significant only at Į = 0.1. Splitter angle was a significant parameter
for Co, Pb, Sn and Pd at Į = 0.05 and for Cu and Fe at Į = 0.1 while it was insignificant for Fe, Ni
and Au (P > 0.1). The statistical analysis detected the significance of interaction effects of magnetic
field-roll speed (AB) for Co, Pb and Pd, and roll speed-splitter angle (BC) for Pd at Į = 0.05.

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Table 10: Statistical analysis of linear/square/interaction effects of the regression models

P-value
Source
Fe Ni Co Pb Sn Cu Au Pd
Model 0.0005 0.0024 0.0132 0.0044 0.0053 0.0045 0.0347 0.0001
A- Magnetic field < 0.0001 0.0002 0.0023 0.0004 0.0004 0.0004 0.0070 < 0.0001
B- Roll speed 0.0051 0.0595 0.0907 0.0036 0.0044 0.0021 0.0097 0.0002
C- Splitter angle 0.0668 0.1320 0.0070 0.0425 0.0446 0.0513 0.8920 0.0072
AB 0.2039 0.1684 0.0197 0.0432 0.0540 0.0682 0.3739 0.0007
AC 0.1056 0.0792 0.6668 0.9169 0.9277 0.3753 0.8864 0.1022
BC 0.3995 0.5175 0.1549 0.1282 0.2701 0.0533 0.0648 0.0199
A2 0.0002 0.0010 0.4067 0.0163 0.0566 0.0446 0.0393 0.0001
2
B 0.1316 0.4825 0.1480 0.8888 0.5802 0.7541 0.2473 0.0014
2
C 0.7141 0.5572 0.0592 0.4967 0.2389 0.5433 0.9019 0.0014
Response surface plots showing simultaneous influence of selected dual parameters are presented in
Figure 5 (Fe, Ni and Co), Figure 6 (Pb and Sn) and Figure 7 (Cu, Au and Pd). It can be clearly ob-
served from Figure 5 that increasing magnetic field induced a positive effect on the recovery of fer-
romagnetic metals (i.e. Fe, Ni and Co) apparently due to the increased magnetic force (Fm) on these
metals at high magnetic fields (B) Eq. 1). Concurrently, at high magnetic fields, the recovery of
other metals (Figures 6 - 7) was also observed to improve. The positive influence of magnetic field
was independent of the level of roll speed or splitter angle (Figures 5 -7). Losses of Pb, Sn and Cu
can be ascribed to their association with Fe-alloys as confirmed by SEM-EDS [9]. Similarly, high
gold losses may be linked with the presence of gold associated with iron and nickel [25,26], and/or
as alloyed with Co/Ni [29]. These associations of non-ferrous metals (Cu, Pb, Sn) and precious
metals (such as Au) with ferromagnetic metals/alloys appear to result in the deportment of these
metals into magnetic fraction.
The adverse effect of increasing roll speed and splitter angle on metal recoveries was most evident
at high magnetic fields (Figures 5 - 7). Increasing the speed culminates in the generation of higher
centrifugal forces (Fc, Eq. 3), which lead to strong throwing of ferromagnetic particles (and
base/precious metals associated with ferromagnetics) to non-magnetic fraction.

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Figure 5: Response surface plots for metal recoveries (%) of (a) Fe, (a) Ni and (c,d) Co
These results revealed that losses of base and precious metals can be significant during magnetic
separation. Accordingly, the performance of magnetic separation of ferromagnetic metals from
WPCB should be evaluated against base and precious metal losses, which may adversely affect
economics of the recycling process.

Figure 6: Response surface plots for metal recoveries (%) of (a) Pb and (b) Sn

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Figure 7: Response surface plots for metal recoveries (%) of (a) Cu, (b) Au and (c,d) Pd

4 Conclusions
This study investigated magnetic separation of ferromagnetic metals from WPCB (- 3.35 + 0.106 mm)
containing appreciable quantities of base and precious metals (i.e. 18.5 % Cu, 86 ppm Au, 694 ppm Ag
and 97 ppm Pd content). Effects of magnetic field, roll speed and splitter angle on the separation of Fe,
Co and Ni were demonstrated using Box-Behnken design. The loss of base and precious metals which
are of main economic interest was also determined. The statistical analysis of data showed that magnetic
field was the most influential parameter on the recovery of metals. Despite high recoveries obtained for
ferromagnetic metals particularly for Fe (” 96 %) and Ni (” 93 %), significant losses occurred for Cu,
Au and Pd as up to 60 - 79%. Metal losses appear to result from their association with Fe-alloys leading
to the deportment of these metals into magnetic fraction. SEM-EDS studies confirmed the presence of
Cu and Pb-Sn as associated with Fe-alloys. These findings highlight that base/precious metal losses
should be taken into account for the development and application of magnetic separation processes for
removal/recovery of ferrous metals.

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Acknowledgement
The authors would like to appreciate The Scientific and Technological Research Council of Turkey
(TUBITAK) for the financial support (Project code: 109M111) and to Mr. Ahmet Deniz Bas for his
help during preparation of WPCB samples.

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662 Proceedings of EMC 2015