Document ZaRZkKjg62J672rv2N8m2nNO
FILE NAME Johnson & Johnson JAJ
DATE 0000
DOC JAJ217
DOCUMENT DESCRIPTION Report - Concentration of Amphibole and Serpentine asbestos from Talc by froth flotation
CONCENTRATION OF AMPHIBOLE
AND SERPENTINE ASBESTOS FROM|
TALC BY FROTH FLOTATION
mM
a)
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TABLE 1 Flotation Results of 0.5 Asbestos Sample
Test Sample Fraction p.p.m. p.p.m. Crocidolite Recovery
K
A 1
1
Conc
0.0
0.0
2
Tailing
8.4
6.0
100
12
~
3
Conc 1
0.0
0.0
4
Conc 2
0.0
.0 0
0.5 Crocidolite
5
Conc 3
0.0
2
6
Conc 4 | 0.0
0.0 0.0
7
Middling
2.16
8
| Tailing | 12.6
1.5 8.5
91.0
17
B
m
,
4
9
Conc
0.0
10
Tailing 8.0
22
Conc 1
0.0
22
Conc 2
0.0
13
Conc 3 | 0.0
14
Conc 4
0.0
15
Middling
2.0
16
Tailing
13.1
0.0 8.0
0.0 0.0
0.0
0.0 1.5
9.0
*
100
12
0.5 Crocidolite + 95 Chrysotile
90.0
18
C S
6
17 18
19
-
20 21 22 22 24
Mg
p.p.m.
g
Chrysotile
Conc
Tailing
0.0 4 .0.0
| 1.18 |" 8.5
100
17
Conc 1
0.0
Conc 2
0.0
Conc 3 | 0.0
Conc 4
0.0
0.0 0.0
0.0
0.0
0.5 Chrysotile
a
Middling
| Tailing .
0.30 0.30
1.70
2.0
13.0
90
26
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examination and the ray tube was operated at 30 KV and
20 ma ^ diffractometer scan rate of 26 per minute
was employed and the inlet and outlet slits were 1" 20
and 0.2 mm respectively Diffractometer traces of Italian
talc chrysotile crocidolite and actinolite used in the
separation experiments are given by Figs 5 - 9
Results
The results of a number of tests upon a talc sample
'
containing 0.5 chrysotile and 0.5 crocidolite by weight
and also a sample containing both crocidolite and chryso-
tile in 0.5 portions are given in Table 1. In Table 1
test No. 1 represents a single stage flotation separation
of crocidolite and talc
It can be seen that the concen-
tration of crocidolite in the tailings is 6 by weight no
crocidolite being detected in the floated talc Test
No. 2 in Table 1 represents a two stage separation of
crocidolite and talc In the two stage separation the
tailings fraction from four single stage tests have
been combined together and retreated to give a final tailings and a secondary flotation product referred to as
middlings By employing two stages of separation it can
be seen that the final tailings is richer in asbestos than
a single stage flotation tailings However some asbestos
is lost in the middlings fraction Tests 3 and 4 in
Table 1 show the results of the crocidolite separation
from the mixture of crocidolite and chrysotile Again
a 6 tailings assay in a single step and a 9.0 assay for crocidolite in a two stage separation The chrysotile
did not therefore interfere with the crocidolite separa-
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TABLE 2 Flotation Results of % Asbestos Sample
Te Test st No.
Sample Sample
No.
Fraction Fraction
Fraction
Fe
p.p.m.
g Crocidolite
"
| Recovery
A 7
25
Conc
0.30
26
Tailing
30.60
0.25 21.00
75.90
27
Conc
0.40
0.25
00
28
Middling
9.60
7.00
29
Tailing
55.60
39.00
81.25
Concentration
Ratio
Ratio
|
K
a}
|
| 21
i
% Crocidolite
39
B
30
Conc
0.10
0.00
}
9
. 31
Tailing
23.60
16.00
32
Conc
0.00
0.00
0.00
100.00
% Crocidolite
+ % Chrysotile
10
33
Middling | 11.60
8.00
34
Tailing
46.60
33.00
66.00
33
Mg
p.p.m.
%
Chrysotile
A
30
Conc
0.00
0.00
;
31
Tailing
2.70
21.00
100.00
21
i
32
Conc
0.00
10
33
Middling
0.50
0.00 4.00
m=
% Crocidolite
+ % Chrysotile
|
34
Tailing
4.80
37.50
90.62
37.50
C
35
Conc
0.00
0.00
|
11
36
Tailing
2.60
20.00
'
37
Conc
0.00
0.00
|
100.00
20
% Chrysotile .
12
38
Middling
0.60
4.50
39
Tailing
5.10
40.00
~
87.32
40
*
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Test No.
A 13
TABLE 3 Flotation Results of % Asbestos Samples
Sample
No.
Fraction
Fraction
Fe
p.p.m.
Crocidolite
40
Conc
0.30
0.25
-
41
Tailing | 37.60
26.00
%
Recovery
88.35
i Concentration
;
Ratio
Ratio ;
13
|
|
14
B 15
16
1
.
a 15
1
16
C
17
18
42
Conc
0.00
43 | Middling
8.60
44
Tailing | 74.60
0.00 6.00 52.00
45
Conc
0.30
46
Tailing
39.60
0.25
.
28.00
47
Conc
48 | Middling
0.00 6.60
0.00 5.00
49
Tailing | 61.60
43.00
Mg
%
p.p.m. | Chrysotile
45
Conc
0.00
0.00
46
Tailing
3.50
27.00
47 | Conc
0.00
48 | Middling 0.80
49
Tailing
5.15
0.00 6.00 40.30
50 51
Conc
Tailing
0.00 3.50
0.00
27.00
Su
Conc
0.00
Su
Middling
1.70
54
Tailing
5.25
;
0.00
13.00 41.00
86.96 89.09 92.95
% Crocidolit
I
26
|
i
14
% Crocidolite
+ % Chrysotil
fF
21.5
|
100.00
13.5
%
+ Chrysotil % Chrysotil |
91.38
20.15
100.00
,
13.5
2 Chrysotile
:
75.93
20.5
-
|
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,
tion
17-26 17-26 @ :
7
4
Mater
:
|
;
Tests 5 and in Tab1l she ow the results obtained
from the separation ofa 0.5 chrysotile mixture
In Test 5 the tailings were found to contain 8.5
chrysotile while test 6 shows that the tailings produced
:
from a two stage separation assayed 13.0 chrysotile
by
weight
a
considerable
upgrading
from
the
original
0.5
Table 2 contains similar results to Table 1 except
all the tests were performed with 1 additions of crocidolite
and chrysotile and a % crocidolite and chrysotile mixture
eS a From test 7 in Table 2 we see that in a single step tailings containing 21 crocidolite was produced while
in a single step for chrysotile test 11 tailings with
ee
20 chrysotile was obtained The two stage separation
chrysotile results for crocidolite and
t
given by tests 8
and 12 respectively show an improvement to 39 and 40
ee
as compared with 29 and 20 in the single stage tests
.
Table 3 contains the results obtained from the
ee
separation of a series of samples containing % crocidolite
and chrysotile respectively and also the results from a
% crocidolite and chrysotile mixture In single stage
ee separation containing for crocidolite test 3 a tailings
26 crocidolite was obtained while a tailings containing
ee
52 crocidolite was obtained in a two stage separation
Fy
test 4 For chrysotile tailings fractions containing
27 and 40.3 chrysotile for single and two stage separa-
tions respectively were obtained tests 15 and 16
ee talc results for the % crocidolite % chrysotile in
The
samples gave 28 and 43 for crocidolite in the tailings
fractions from single and two stage separations and 27
ee
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TABLE 4 Continued
|
Test
NoNo..
a
13
Sample
-
No. No.
Fraction
40
Conc
,
41
Tailings
% Crocidolite
% Chrysotile
A.A.S. X.R.D. A.A.S. | X.R.D.
0.25
0.00
26.00
30.00
42 Conc
0.00
0.00
14
43
Middlings 6.00
7.00
44
Tailings
52.00
54.00
Remarks % Crocidolite
15
45 46
Conc
Tailings
Tailings
0.25 228.00 8.00
0.00 29.00
47
Conc
0.00
0.00
16
48
Middlings
5.00
7.00
49
Tailings
43.00
43.00
29 Crocidolite
% Chrysotile
|
i
45 15
46
.
47
16
48
49
Conc
Tailings
|-
Conc Middlings Tailings
; .
0.00
0.00
27.00 0.00
29.00 0.00
28 Crocidolite % Chrysotile
6.00
7.00
i 40.30 | 38.00
50
Conc
17
;
.51
Tailings
|
; NM
Conc
:
'
18
53
Middlings
;
54
Tailings
a
:
|
0.00 27.00
0.00 30.00
0.00
0.00
13.00 | 12.00
41.00
:
43.00
% Chrysotile
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y TABLE 4 Comparison of the analysis of flotation products by ray
Diffraction and wet chemical analysis
Test Sample Fraction
No.
.
25
Conc
7
.
26
Tailings
% Crocidolite | * Chrysotile
A.A.S. | X.R.D. | A.A.S. | R.D.
0.25 | 0.00
21.00
23.00
27
Conc
0.25 | 0.00
8
28
Middlings | 7.00 | 6.00
29
Tailings
39.00 | 40.00
Remarks 1 Crocidolite
30 = Conc
0
0.00 | 0.00
31
Tailings
16.00
19.00
;
% Crocidolite
% Chrysotile
10
33
Middlings
8.00
7.00
.
34
Tailings
33.00 | 36.00
30 ~= Conc
9
31
Tailings
32
Conc
10
33
Middling
34
Tailings
0.00 | 0.00
21.00
20.00
0.00 4.00
0.00
5.00
37.50 | 35.00
% Crocidolite
% Chrysotile
.
35 Conc
11
j
. 36
Tailings
:
:
37
Conc
:
12
38
Middlings
39
Tailings
0.00
0.00
20.00 | 19.00
0.00 |;
4.50
0.00 6.00
40.00 | 41.00
oo % Chrysotile
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CONCENTRATION OF AMPHIBOLE AND SERPENTINE ASBESTOS FROM
_. TALC BY FROTH FLOTATION
INTRODUCTION
A great deal of concern surrounds the possible
asbestos content of talc powders used in cosmetic pharmacutical and other industrial and consumer products
Asbestos minerals are known to be associated with the
increased incidence of certain types of cancer and it would be of some industrial importance if it were_
possiblteo
t
talc powder
reduce the level of to an insignificant
asbestos minerals in a level with respect to
their possible health hazard Froth flotation is a
technique used wideltyo separate fine mineral particles
and over 90 of the world's non ferrous minerals are
produced from crushed and finely ground rock using this
technique This concentration technique has been applied
to the concentration of commercial and non commercial
forms of asbestos minerals from talc It has been shown to be very efficient in reducing the asbestos content
of a powder and producing a residue which is referred
to in mineral separation terms as a tailings in which
the asbestos minerals can be easily detected and quantified
The technique has therefore a second significant use in the detection and quantification of asbestos
minerals in talc powder samples Most quantiative mineralogical techniques are only capable of detecting
asbestos mineral impurities in talc powders down to the
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FIG 1 Laboratory Flotation Cell
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% by weight level These techniques include ray
diffractometry differential
infrared
impromet Of these
thermal analysis
techniques ray
and diffrac-
tion would appear to be the most useful It allows both
a positive identification of the mineral phase to be made
and also an accurate determination of mass fraction by
comparison of the relative intensity of the asbestos
mineral reflections from the powders being tested to
those of a set of standard reflections obtained from
talc powder samples spiked with various quantities of
different asbestos minerals
The use of froth flotation to concentrate asbestos
minerals from talc is so efficient that their detection
by the ray diffraction method is accurate to an order
or magnitude lower than in the untreated powder i.e
0.1 or less Efficient separation or concentration
depends upon the selection of the most amenable chemical
conditions under which the flotation separation should
be performed The separation is made in an aqueous environment in which both talc and asbestos are in suspension One of the minerals has to be hydrophobic
or made hydrophobic in order to remove it from the aqueous suspension using air bubbles Talc has a well known
natural hydrophobicity can be improved however by
use of suitable cationic chemicals e.g amines which selectively adsorb onto the talc particles and improve
their hydrophobic character Asbestos minerals have no
natural hydrophobic character therefore no natural floatability and will remain in froth flotation cell
while talc is being floated Some care however has to
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be exercised in the choice of frothing agent which is used to produce a froth at the top of flotation
cell in which the floated mineral is held and removed to
ensure that it does not impart hydrophobic properties to any asbestos mineral particles It must also produce
a froth which drains easily removing as low an amount of
water as possible from the cell in which asbestos mineral
particles may be in suspension
The pH of the aqueous medium is also of importance
in the separation as this can also affect the efficiency
of the flotation by interfering with the properties of
the frothing agant | and also influencing the natural .*
floatability of the talc and asbestos minerals ThepH
produces
floculated
control also non floculated system in which particles
of asbestos and talc are separated in suspension The
control of pH is also desirable when a chemical is used
'
to
increase
the
hydrophobic
nature
of
the
talc
as
it
can
easily be adsorbed onto the asbestos minerals as well
Selection of the pH to produce minimum adsorption of
the chemical onto the asbestos should therefore be made
METHODS MATERIALS AND APPARATUS
The froth flotation tests reported here were all
performed in a modified Knapp and Bates flotation cell
with a capacity of 3 litres of mineral suspension An
impeller in the flotation cell keeps the mineral in
suspension and also draws in air for flotation purposes
It then mixes the air with the mineral suspension to
, .
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JNJAZ55_000007958
of
promote rapid adhesion particles to air bubbles the
impeller was operated at 1500 r.p.m. The amount of air
drawn into the cell approximately 17 minute The flotation cell used is illustrated by Fig 1
The minerals used for experimentation were as
follows
1 Italian talc 00000 grade supplied by Zach Cartwright Ltd. Its general formulae Mg6 Sis 029 OH 4
2 Serpentine asbestos chrysotile which is the most
common of the asbestiform minerals It accounts for
more than 95 of the asbestos fibre produced today
Its general formulae is Mg12 Sig 020 OH Like
a sheet talc is
silicate which occurs as very fine
rolled sheetosf magnesium silicate
3 Amphibole asbestos two varieties of which were used
these were
Crocidelite SiO22 OH 2
Actinolite
Ca MgFe Si OH 2
The chrysotile and crocidolite samples were supplied by
the M.R.C. Research Unit Penarth Glam as being
representative of all commercial asbestiform minerals of the serpentine and amphibole varieties
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The Actinolite sample was included to represent the
type of amphibole more likely to be found associated
with tale The actinolite itself came from the same
mine as the talc used in the experimentation but was not
but
found in association with the talc It occurred with other minerals and before additiotno the talc in a
powdered form it was concentrated into a pure fraction using a Franz isodynamic magnetic separator
The chrysetile and crecidolite asbestos were already
in a very finely powdered form and required no size
reduction before addition to the Italian talc for separa-
tion experiments The actinolite was however first
ground to a size similar to that of the talc before
addition
a Ordinary tap water was used in the flotation tests
and the pH of the suspensions was adjusted using sulphuric
acid and sodium hydroxide The frothing agent used was
a commercial product Aerofroth 65 manufactured by Cyanmide Ltd. it is essentially a propylene of high molecular weight which is totally soluble in water
and is therefore easy to add to the flotation cell It
was found that a suitable concentration of 1.5 ml of a % volume solution of the frothing agent gave an easily
i ;
managed froth removing very little liquid from the flotation
cell
Flotation separation tests were performed with talc samples in which asbestos was added represent 0.58 1.0 and 2.0 asbestos by weight A series of tests with
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a mixturoef amphibole and serpentine asbestos was also
performed to investigate the concentrating action in the
presence of two forms of asbestos The talc samples
were weighed and added to the flotation cell and mixed
_
thoroughly with water the weighed asbestos sample was then
added and also mixed thoroughly into the talc suspension
Care was taken to ensure the talc was completely wetted .
melted by mixing thoroughly no wetting agents were used
When the asbestos mixture was considered to be well
mixed the frothing agent was added
The air inlet to the cell was then
and pH opened
adjustment made
and the floated
talc removed from the top of the cell with a
scraper
The
test was run until no visible talc was found to be reporting to the top of the cell care was taken to ensure no tale
froth was sticking to the cell sides which might contamin--
ate the asbestos material remaining in the cell as tailings
From extensive tests the most advantageous conditions for advantageous conditions for asbestos talc separation
was found to be as follows
Water in the cell
pH adjusted to 2.02.0
with
3 litres
sulphuric acid
Solids concentrat2i0o -2n5 grams in 3 litre
Frothing agent 1.5 mls of % v in 3 litre
All flotation tests were performed using these conditions the only variables being the type and quantity of asbestos
mixed with the talc
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S rn
_
100
a no)
=
CROIDLTE
FOR
9.
Ti
CURVE ~
E
a
a
b4
1
>
CALIBRTON
2
IG, 7 * w
~
T
CALIBRATION
CURVE
CROIDOLITE
oO
o
CALIBRATION
CURVE
CROCIDOLITE
o
Oo
o
CALIBRATION
CURVE
CROCIDOLITE
=
.
PHIOPIIOID *7,
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To measure the separation of asbestos from talc a
combination of wet chemical and ray diffraction tech-
EE
- niques were used For measuring crocidolite the iron
concentration in the floated talc and also in the tailings
HE
was measured and the results compared with a standard
curve prepared from the iron analyses of crocidolite
HE mixtures Chrysotile was measured wet chemically by
digestion measuring the magnesium level obtained by
in
HE hydrochloric concentrated
acid and comparing the results
HE
with a standard curve prepared from the magnesium analyses
of chrysotile mixtures The analysis technique for
HEH both iron and magnesium were as follows
.
He
a Wet Chemical determination of Crocidolite in Talc
, -
HE
A small amount
_
0.05
- 0.1 gram of the
sample was_
fused in a P.T.F.E. crucible at approximately 350
Ere with 2 mls of 1
KOH and water The fused pellet
was then disssolved in 3 mls of concentrated Cl The
solution was made up to a known volume and assayefodr
iron using an E.E.L. 240 atomic adsorption spectrophoto-
&
meter The amount of crocidolite was obtained by checking
against a standard calibration curve as shown in Fig 2
EE b Wet Chemical determination of Chrysotile in Talc , ra
Samples FF
were dispersed in concentrated HCl talc
is not affected by HCl and heated till dry The samples
were then retreated with dilute HCl The resulting
m solutions were made up to a known volume and assayed for magnesium using an A.A.S. From standard calibration
fe
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. ;
o
a
~
x
[Io
w
w
=
~
Oo
o
uy
-
[aa
x=
rs)
ras '
\ tw >. 4
i .
.
sary
ow
=
>
=
Eo _ c
Lc
*
z
x
o
- .
< &
wm
4
to)
<
aw
[om
~
4
o
\ io
Th
YN
.
t
o
o
Lo]
o
t
oO
&
CALIBRATION
=
CALIBRATION CURVE
q o
Nn CHRYSOTILE
Pas
.
o
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0.6
0-51 0-51
|
o &
.
Intesity 0.3 0.3
Relative
o
0
0
6
0! co
3 0
Relative Composition by Weight
FIG 4
DIFFRACTOMETER CALIBRATION
\
CURVE
FOR
CROCIDOLITE
IN TALC-
a penn F s O a8
co
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0.67
x
0.5
Intensity 0.4
.
Intensity
Intensity
Intensity Intensity 0.3
.
Z
Relative .2-
Relative
a
0.1-
:
1
6
0.2
0.4
0.6
0.8
1.0
Relative Composition by Weight
FIG 5
DIFFRACTOMETER CALIBRATION CURVE FOR CHRYSOTILE IN TALC
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.
e
curves the amount of chrysotile was determined after
correction for acid soluble magnesium in the talc tailings
due to the presence of carbonate minerals The carbonate
magnesium was obtained by running flotation tests with no asbestos present and assaying the resultant tailings The magnesium calibration curve is shown in Fig 3
ray determination of Chrysotile and Crocidolite
The tailings samples were also subjected to ray
diffraction measurements using a Siemens ray diffracto-
meter Quantitative readings were obtained by measuring
the peak intensity of the amphibole reflection at 10.5
degrees 20 and the chrysotile reflection at 12.2 degrees
20 and expressing these as a ratio with the main talc
reflection at approximately 9.0 degrees 28. This ratio figure was then compared with a calibration curve
constructed from peak ratio figures obtained from mix-
tures of talc and the various asbestos samples these are
shown in Figs 4 and 5. The use of a ratio of chrysotile to talc peak and crocidolite to talc peak removed the
necessity of using an internal standard for quantification
purposes
Care was taken in the preparation of ray standards
to ensure good mixing and this was performed in aqueous
suspension using the froth flotation cell as a mixer
Xlray powder preparations were investigated also and both pressed and loose specimens were examined The loose
powder preparation was preferred and used in all the measurements Copper radiation was used throughout the
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and 41 for the chrysotile in the same tailings fractions
The results show that quantity of asbestos in the
tailings increases dramatically with increase in asbestos
content of the original asbestos mixture Also
the fact that two asbestos minerals may be contained in
the same sample has very little effect upon the recovery
of each mineral in the tailings The highest concentra-
tion ratios K obtained in these tests were with the %
asbestos mixtures where the asbestos was concentrated
in the tailings from 1 to 35 approximately
The tailings fractions were all subjected to ray
diffraction examination as well as wet chemical analysis
and the comparison of some of the quantitative results
obtained are given in Table 4. 10-12 illustrate
portions of diffractometer traces obtained from separated
tailings fractions of tests performed upon 1 crocidolite
1 chrysotile 1 crocidolite and chrysotile in talc
mixtures
Tests with 0.5 additions of actinolite in talc were
also performed and Fig.13 illustrates the diffractometer
trace obtained from a single stage separation of actinolite
from talc No quantification was performed for this sample
as there was insufficient actinolite to prepare diffrac-
tion standards
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Conclusions
.
Froth flotation would appear to be a most efficient
means of separating amphibole and serpentine asbestos
from talc for both detection and quantification of the
asbestos phase No interference appears to occur when
two asbestos minerals are present and are being separa-
ted Two stage separation is slightly more efficient
than a single stage separation
The most suitable flotation conditions for separation were found to be pH - 2.0 with a solids concen-
tration of 6 - 8 grams per litre of water in the flotation
cell The most suitable frothing agent was found to be Frother 65 produced by Cyanimide Ltd.
H
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