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aass
A1.U
x 5^.0
The
Fire
of Gold, Silver,
Assay
and Lead
in
Ores and
Metallurgical Products
by
Leonard S.[Austin
Professor of Metallurgy and Ore-dressing,
Michigan College of Mines.
First Edition
1907
Published by the
Mining and
Scientific Press
San Francisco
GENEBAL
COPYRIGHT,
1907
BY
TABLE OF CONTENTS
PAGE
Preface
I.
The
11
12
III.
15
IV.
Apparatus
II.
V.
VI.
VII.
VIII.
IX.
X.
XL
17
; r ;;
22
."
30
Assay Balances
32
Fluxes Used
in
40
Assaying
48
Ores
The
Scorification
50
Assay
54
Cupelling
Parting
56
XIII.
The
60
XIV.
Roasting of Ores
70
Assay of Matte
72
73
74
XII.
XV.
XVI.
XVII.
Crucible Assay
XVIII.
Assay
of Base r Bullion
XIX.
Assay
Assay
of Blister
XX.
or
Pig-Copper Containing
XXI.
XXII.
XXIII.
Assay
78
Silver
and
82
Gold
of
76
Gold Bullion
84
85
87
179709
PREFACE
The following pages
and of
in the
lead,
and gold)
Rocky Mountain
and products
is
is
to employ.
It has, therefore,
I.
The
fire
assay
is
of the metal sought with the aid of heat and suitable fluxes, and
of weighing it in metallic form. Thus if we desire to determine
The
1.
2.
Sampling.
3.
4.
upon this.
where there is reason to believe that they
may be incorrect owing to faulty manipulation, to losses, or to
the mixing of samples.
Single assays may be made upon grab samples when an apaccuracy, depends largely
Never report
results
IL
The following
handlabel,
upon which is marked the name of the owner, the name of the
Where the assayer has
ore, and the lot-number of the sample.
should
also
describe the ore so
lots
he
to number the
himself,
be distinguished again by the sender.
a good practice to reserve one or more of the larger pieces,
after having partly broken down a sample, since in this way we
that
it
may
It is
may
at another time or
by another assayer.
AUSTIN
This
FIRE ASSAY.
13
is
sample
is
The breaking up
considerable,
is
The work
as follows
of cutting
The ore
is
be performed
in the centre
of the plate, the material being poured or thrown upon the apex
of. the pile so as to effect an even distribution of fine and coarse.
The cone
is
now
flattened out to a
by
scraping the ore outward every way from its apex. Two lines
are marked at right angles, dividing the mass into quarters. The
two opposite quarters are then removed, rejected, and the remainder mixed and quartered as before, taking care, however,
first to
if
necessary.
it
is
better to use a
dried,
it
is
if
riot
or of rubber cloth.
its
from
side to side.
It
mixing proceeds until the operator is sure that the ore is quite
uniform in all its parts. A beginner is very apt not to move or
roll the ore sufficiently to insure its complete
turning over. For
it
would
be
well
for
him
to
mix
some
practice,
argols and soda
in this way, until the absolutely uniform color of the mixture
indicates that the
mixing
is
complete.
14
An
down
riffle.
a sample
The ore
When
reserved,
and more
breaking
is
needed
is
it
must be done.
Prospectors and others, interested in mines, often deceive themselves by thinking that by sending in a piece or lump of rock, they
can arrive at an idea of the value of the ore they are going to
If one will assay separately two such pieces of rock, he
ship.
how much they vary from one another. The only way to
the value of an ore is to sample it in quantity, so that all
will see
know
HI.
When
has to keep his work going steadily, but there are spare moments
when he can brush up and set things in order again. In fact,
stantly in order.
energetic.
Clinkers will form upon the interior of the furnace, and these
are to be removed with a long-handled cutter-bar or chisel. The
assayer also replaces his own muffles, claying up the joint with
fire-clay, to which has been added its own weight of sand, or
preferably, some coarsely ground fire-brick which he can break
up for himself on the grinding-plate. In a reduction works
where tailing, slag, or low-grade products are treated, there
ground on the
plate
off,
in
count for cases where a trace, or even more of metal, has been
when
reported
When
16
will
wash them
out.
IV.
APPARATUS.
FIG.
1.
may
be 10
in.
When
the
AUSTIN
i8
oil-cloth or a
FIRE ASSAY.
is
in.
mixed or
square.
rolled
on a piece of
assays.
FIG.
2.
For handling
shown below:
FIRE TOOLS.
are used as
FIG.
3.
CRUCIBLE TONGS.
in Fig. 3.
FIG. 4.
Fig. 4 shows the short tongs used for removing nails from
the crucible before pouring. They are nine inches long.
19
in
provided,
is
not satisfactory.
FIG.
5.
is
SCORIFIER TONGS.
FIG. 6.
FIG.
7.
CUPEL TONGS.
flat
in.
long.
AUSTIN
2O
FIRE ASSAY.
way
shown
the
damage
It
in Fig. 8.
FIG.
8.
SCRAPER.
CUPEL MOLDS.
in.
diam., are in
two
FIG.
9.
of the cupel when molded, and, in making the cupel, the plunger
In making cupels, the bone-ash is
enters the smaller diameter.
FIG. 10.
moistened with a
that,
it
water until
will cohere.
it
carefully dried
month or more,
hand.
little
when molded,
by being put
21
less iron in
V.
To
these
cities, it
may be added
may be had.
FlG. 11.
Fig. ii is an elevation, and Fig. 12 and 13, two sectional elevations of a two-high muffle furnace for burning soft coal, which
The
flame.
interior
volatile
is
23
constituents to produce a
suitable
so that the furnace can be readily and speedily built. The rest
is of red brick, the whole being firmly clamped
or bound with angle-iron and tie rods. The muffles, of the form
of the furnace
shown
in Fig. 12
FK;. 12
one
is
large
AND
and
13.
enough
13,
SECTIONS
to take
or-
in.,
and each
two 2O-gram
by 3^4
in-
easily
The lower
muffle,
which can be
brought to the higher temperature, is generally reserved for melting and the upper one for cupelling. By means of a tile-damper
the assayer can regulate the heat of the furnace, so that, in
cupelling, he can carry several rows of cupels at a time. He then
subdues the heat at the back of the muffle by putting in cold
The
fire-door
is
placed so
24
way
if
of the assayer.
so desired.
wood as desired.
Where much work has to be done, furnaces having much larger
muffles are used, where as many as four 2O-gm. crucibles can be
take 16 to 24-in.
little
deeper
at the back,
FIG. 14.
using but
little
coal at a time
in.
deep,
and feed-
Be
careful not
to permit any holes through the fuel bed by which cold air can
get up to cool the muffle. The fire must be kept clean and free
from ashes and cinders. As those latter accumulate in the ash-pit
25
The
muffle
is
receiving crucibles.
lid.
The
rows
two
crucibles in a row.
They
FIG. 15.
the level of the top of the muffle and then two inches in depth
of coke broken to egg size or less. If. left larger, these pieces
will not pass down between the muffle and the wall of the furnace.
The
fire
is
then
is
lit,
AUSTIN
26
FIRE ASSAY.
and
is
set,
digging out
a hole for them with the poker and tongs and setting them among
the cold coke. With a good draft the coke is soon burning and
the charge melting down. As soon as the muffle gets sufficiently
When the crucibles
hot, cupelling or scorifying can proceed.
have been poured, the poker is again used to work down the coals,
fresh coke is put in and a new batch of crucibles set. After their
removal, poke down and replenish the fire before cupelling.
Even if there are no more crucible-melts to be made, still the
fire
FIG. 16.
cupelling.
Fig. 15 represents a
Bosworth furnace
for a 9
by
I5~in. muffle.
be
consisting of a base, a body, and a top, on top of which may
noticed the outlet connecting to the chimney by means of a 5 -in.
The top is covered by an iron door and, when the
stove-pipe.
furnace
is
in full operation,
feed opening.
The
it is filled
sill
of the
27
FIG. 17.
Fig.
'
it
when
it is
in-
set,
'to
full
depth
in
AUSTIN
28
FIRE ASSAY.
wheel, the gasoline, under pressure from the tank which has been
first of all pumped up, is heated and gasified as it enters the
furnace from the jet. The issuing vapor is lit by a match imme-
FIG.
18.
FIG.
19.
kept up.
BURNER.
TANK AND
For success
and as the
in operating, therefore,
it
is
necessary
AUSTIN
first
FIRE ASSAY.
29
10 or I5~lb. pressure.
The crucibles to be melted may be
placed within the furnace while it is cold and the heat brought
up on them gradually. It is also possible to put them into a
to
heated furnace, letting them take up the heat, and finally to start
the burner.
These furnaces have the advantage that they are
quickly brought up to the full heat, which can then be retained
indefinitely with but little further attention.
They cost, for the
furnace $25, for the burner $11, and for the pump, tank, pipe,
and
fittings, $20.
_,_KV
'
OF THE
UNIVERSITY
OF
VI.
For ordinary assaying, but few out of the many kinds advermade use of. Thus, for work in the muffle, but two
sizes are used, the 10 and the 2O-gm. crucibles.
(See Fig. 20.)
These crucibles are short enough to be placed in the muffle of the
tised are
and F.
FIG. 20.
FIG. 21.
CLAY CRUCIBLES.
CLAY CRUCIBLES.
(FLAT FORM.)
(POINTED FORM.)
when assaying
silicious ores,
they
may
If
still
be again used.
sound, as
However,
AUSTIN
used for a
These may
FIRE ASSAY.
31
in.
diam. by 3.5
in.
22)
is
used.
high, called
size.
FIG. 22.
made of fire-clay, white and smooth, or of a simiwhich has been mixed a good deal of sand, so that
they are rougher on the surface and of light-brown color. The
Crucibles are
FIG. 23.
SCORIFIERS.
time except for a silicious ore, and, even at the first time, may be
so corroded as to permit the escape of a charge. The size specified is large enough for assaying one-tenth of an assay ton of
ore, and,
is
chosen.
when
VIL
ASSAY BALANCES.
button,
variable load
is
shows a pulp-balance,
FIG. 24.
from
air-currents,
33
chemical determinations, doing away with the necessity of purchasing a chemical balance where one wishes to economize in
1
first
cost of equipment.
FIG. 25.
Price $30.
34
at the
It
should
be set so that the vibrations are equal on either side of the zero
mark. Carry inside the balance a camel's-hair brush with which
making the final adjustment. Somebeam seems out of adjustment, it may be no more
times,
when
the
in
Price $110.
FIG. 26.
BUTTON BALANCE.
beam graduated
The knife-edges
are of
AUSTIN
FIRE ASSAY.
35
FIG. 27.
is
For use
500 to
sufficient.
is sufficient.
weights from.
36
SET OF
FIG. 28.
GRAM WEIGHTS.
if
is thus obtained
A pound
and
the
ounce
avoirdupois weighs 7000 grains
480 grains,
Troy
therefore we have
14.58 Troy ounces to the pound avoir^
400
dupois, or 2000 by 14.58
29,166 ounces per ton of 2000 pounds.
In practice, the weights of one gram and above are cylindrical
and are handled with the fingers, those less than one gram are
flat, and are never touched by the fingers but handled with
pincers. Particular care must be taken of the finer weights, and,
in placing them, the hand or fingers rest on the case.
Where a
number of weights are to be removed the pan is taken off with
pincers and they are dumped from it upon the floor of the case
and there counted. When returned to the box they are counted
In weighing, proceed
again as a check on the first reading.
if
Thus
the
is
we would put on
mg.,
systematically.
weight
378
200
more
too much, 100
too
then
too
200,
much,
little,
500 mg.,
too little, 50 too little, 20 too little, 20 too much, 10 too little, 5 too
little.
The remainder we know to be between 375 and 380, which
=
=
The value
AUSTIN
is
to be determined
FIRE ASSAY.
will
37
weigh
five
milligrams
on the beam.
The pincers or forceps for these weights are of brass with fine
curved points, see Fig. 29, or nickel-plated as in Fig. 30. They
FIG. 29.
FIG. 30.
PINCERS.
NICKEL-PLATED PINCERS.
are used, not only for handling the weights, but also for pickmg
up buttons, for granulations, or other fragments. In preparing
the silver button for assay, it is removed from the cupel by means
of pointed-nose button-pliers (Fig. 31), and the adherent boneFor larger
ash removed with the button brush (Fig. 32).
buttons, of over 100 mg., stouter pliers are to be preferred, since
FIG. 31.
BUTTON
FIG. 32.
BUTTON BRUSH.
PLIERS.
FIG. 33.
FIG. 34.
FIG. 35.
FIG. 36.
SLAGGING HAMMER.
37) with a
quicker.
who
AUSTIN
FIRE ASSAY.
39
MOISTURE SCALES. For determining the percentage of moisture in an ore, or the weight of fines and metallics in a sample,
the moisture scale (Fig. 38) is well suited. It is finished with a
FIG. 37.
SPATULA.
sliding weight,
pan and
i
its
FIG. 38.
MOISTURE SCALES.
VIII.
ceous
as
substance,
metallic form.
We
may
or
argols
flour,
will
reduce
litharge
to
ACID FLUXES,
COLLECTING AGENTS,
REDUCING AGENTS,
OXIDIZING
COVER, as
salt.
The ordinary crude borax of commerce is the prismatic neutral variety (Na 2 B 4 O 7 -(- 10 H 2 O) and when pure conBORAX.
sists of:
Boracic acid (B 2 O e )
Soda (Na 2 O)
Water of crystallization
36.5%
16.4%
47.1
100.0%
Borax-glass may be made by melting this crude borax in
a crucible, or in an iron dish or ladle, taking care to fill the vessel
only
of
more
partly,
its
since
the
original bulk.
of composition
is
driven
hydrated
Under the
off,
salt
swells
to
twice
or
AUSTIN
FIRE ASSAY.
4!
broken
When
cold,
the borax-glass
is
the ore.
tion,
most appropriately used in scorificaplaced upon the top of the charge in the
Borax-glass
where
it
is
is
scorifier.
base that
it is
quite
commonly
amount
we
deficiency of borax is
or thick, but brittle.
stiff
42
beyond bounds
it
If
it
may
indicated.
GLASS.
Glass
is
when used
(K O)
2
an advantage
Glass
is
About one-third
a flour-screen.
SiO 2
though
it
is
95%
found that
it
is
size.
it
reducing power,
43
98%
it
When
It
chemically
forms with
silica
Na CO 3
2
SiO 2
Na 2 SiO 8
+ CO
CO
meltthe escaping
2 gas thoroughly agitating and mixing the
find
contents
of
the
From
the
formula
we
crucible.
by
ing
calculation that one part of silica needs 1.76 part of soda to
form
the mono-silicate.
K CO
90%
(K 2 O)
available to
combine with
silica.
When
the salt
is
mixed
we
such a mixture.
The disadvantage of using pearlash is the
introduction of sulphates into the charge, so that many assayers
use sodium mono-carbonate only. Pearlash is disposed to absorb
moisture from the air and become deliquescent, or at any rate,
lumpy. When used with soda it is mixed in equal parts, or better,
in the ratio of 2.7 parts of
who
use
only,
is
it
claim
Litharge (PbO)
reduced to lead
it
is
is
gives
it
after
AUSTIN
44
There
is
now no
FIRE ASSAY.
litharge
is
readily obtainable
When
flux,
for the purpose of affording a lead button, into which are coland silver of the ore. Before its reduction, the
litharge is largely increased where the impurities arsenic, antimony, copper, or tellurium are large in amount. The reducing
power of various sulphides, or the amount of litharge needed
to oxidize them,
Manganese
is,
(FeS) 28
(FeS
2 )..
46.5"
Ironpyrite
"
23
Copper sulphide
Iron sulphide
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
32.5
Antimony sulphide
23
23
.
Lead sulphide
46.5
30
5O
"
"
25
Copper pyrite
Zinc sulphide
Arsenic sulphide
"
35
25
"25
"
"
"
"
50
"
"
Red
It
lead
contains
PbO
+ C = Pb + CO
(or 2
PbO
+"
= 2 Pb + CO
2 )
the carbon
is
brought to a red
heat in the muffle; it is then withdrawn, the ash blown off, and
the pieces broken small in an iron mortar. The pulverizing is
finished
AUSTIN
FIRE ASSAY.
45
one of the most powerful reducing agents known. Its disadvantage is its lightness, whereby it tends to float on the surface
of the charge into which it has been mixed.
it is
The
FLOUR.
enables
it
ferred by
flour of
to be
many
to argols.
One
ARGOLS.
One
it
When
pure
tains,
besides
it
amount used
regarded.
its
Argols
part of
will
KHC H
of
tartrate
in
It
its dilution,
Two common
One
Wheat
-.
28
parts lead.
12
flour
Argols
1.6
1.8
"
"
"
This reducing power varies, and in any case it is best to deterit when a fresh lot has been
prepared as follows
mine
46
Mix
in a
new
10 gm. soda.
color.
The
OXIDIZING AGENTS.
nitrates of potash
(nitre)
and of
soda, especially the former, are used for oxidizing the sulphides
of the charge, where the ore itself would reduce too large a lead
button. Their oxidizing power is such that one part will reduce
from, litharge:
Nitrate of soda
(NaNO
Nitrate of potash
This
is
(KNU
commercial nitre
at
salt.
4 even.
3)
We
composition.
To determine this oxidizing power prepare two crucibles as
follows
Charge into each 40 gm. PbO, 10 gm. soda, and 3 gm.
The crucibles are
to one of them add 3 gm. nitre.
and
argols,
:
loss,
The
is
feared.
AUSTIN
FIRE ASSAY.
47
dependence
is
more
IX.
ORES.
At the same
Galena containing
Blende containing
Pyrite
containing
87%
67%
46%
lead,
zinc,
iron,
13%
33%
54%
sulphur.
sulphur.
sulphur.
be noticed that the percentage of metal (or base) decreases while the sulphur increases in this list.
Since the lead
It will
in the
galena
is
be regarded as a base. Galena contains but little sulphur as comOf the remaining sulphides
pared with the other sulphides.
(blende and pyrite), we may say that they contain much base,
49
is
into silicious
and basic
ores, since
and
pyrite.
As
regards ores high in lead (leady ores) they are low both in
and bases. Such ores feel heavy, and, when a portion is
weighed out for assay, it occupies but little bulk. Thus the
silica
and
this
X.
charge
suited to
is
is
ail
the regular
30 to 60 gm.
and
to 5
gm. borax.
In a 2^2 -in. scorifier measure one half the specified amount of
test-lead, weigh out the ore, and mix with a spatula in the
Sprinkle on the remainder of the test-lead, completely
covering the mixed portion, then add the required amount of
borax. The quantity of borax will depend upon the amount of
scorifier.
When
much
little
base use
little
there
is
borax.
exposed to the
air,
lead, at that
AUSTIN
2.
whole
its
The
The
1.
51
FIRE ASSAY.
muffle
is
opened and
scorification proceeds
(about
twenty minutes).
The
3.
scorifier is
minutes) and
five
To
mold
When
the con-
tents of the
button as
it
is
rests
upon an
understood that
which was
cupelling,
this
is
thoroughly
be
It is to
in the ore.
silver
(and jgold).
PbS
ZnS
FeS 2
The
+ 3 O =PbO + SO
+ 30 =ZnO + SO
+ heat = FeS + S
The molten
lead
is
2
2
SO
2.
Then
Pb
+ O =
PbO
But any PbO, thus forming, eagerly takes up any silica in the
gangue of the ore. The borax is busy dissolving the oxides as
they form thus
:
FeO
ZnO
=
+ Na B
+ Na BO O =
2
Na 2 FeB O 8
Na 2 ZnB 4 O 8
4
By the time the door has been opened, enough PbO has been
formed to dissolve the silicious gangue, and if not, the increased
access of air at this time speedily produces
it.
At
the period of
partly
+ 2PbO = 3?b + SO 2
ZnS + 3PbO = sPb + ZnO + SO,
FeS + 3?bO = 3?b + FeO + SO,"
CuS + 3?bO = 3?b + CuO + SO~
As S 3 + QPbO = As O + 3SO 2 + pPb
to say, oxidation may be brought about by contact
PbS
That
is
with
centre exposed to the air. When the eye at the centre becomes
small, oxidation necessarily proceeds slowly so that, to save time,
it is better to pour the assay.
The resultant button should weigh
;
we
more than
often have
it
of 20 gm.
grams.
GENERAL REMARKS ON SCORIFICATION. It will be noticed that
the quantity of test-lead prescribed for an ordinary assay is 10
times the weight of the ore.
When, however,
the ore
is
'dirty'
MINERAL
lfl
A. T. OF
53
arge reacts on the impurities of the ore, oxidizing them, and they
enter the slag (formed by the litharge uniting itself to the gangue
of the ore and to whatever borax has been added).
The ore
also tends to float
last,
stiff
much
much
slag).
On
XLCUPELLING.
PREPARATION OF THE CUPEL.
pan with a
little
when grasped
The bone-ash
Ground bone-ash
in the hand.
is
This
is
mixed
in a
is
determined by experience.
it.
there until
it
placed in
it
due to the melting of film of oxide which covers the assayand which goes to the edge of the cupel leaving the surface
exposed to the oxidizing influence of the air. The door is opened
is
piece
and the cupel brought further forward toward the front of the
muffle to 'drive.'
When
the muffle
is
reduces the lead film already mentioned, so that when the door is
opened, and the wood removed, cupellation at once proceeds. The
limits.
it
is
If the
silver,
permitted to
AUSTIN
FIRE ASSAY.
55
At
all
button
is
large
it
is
moving from the muffle and to remove it gradually, since otherwise it is liable to 'spit' or sprout, which may result in a loss
through the projection of microscopic particles of silver from
the substance of the button, which may be observed under the
microscope at the borders of the cavity of the cupel. The reaction,
Pb
O
PbO
51,000 calories, indicates that much heat
evolved as the result of the burning of the lead to litharge.
is
TEMPERATURE
DEGREES C
PARTING.
XII.
The
has
now
book
and
its
should deform
it
is
flattened
Upon
this is
covering the
button to say, J4 in. depth. This is brought to the boiling point
on the hot plate, taking care the ebullition is not violent, since
such action tears apart the newly released gold. When action
nitric acid (i of acid of sp. gr. 1.42 to 3 of water),
leaving the
to 4 of
acid
acid
of
of
behind.
few
(7
stronger
drops
gold
water) are then added to the capsule, brought to boiling, until
acid
is
poured
wide-mouthed
bottle,
*Let the beginner weigh the button without completely cleaning it,
after proper cleaning, weigh again. The difference in weight
will be observable.
and then,
AUSTIN
FIRE ASSAY.
57
The capsule
action of the gold has ceased, and then decanted.
is now nearly filled with hot distilled water from a wash-bottle,
directing the stream tangentially on the border of the capsule
This wash water
is
Where
will
distilled
form a
common water
when
this
happens
with the
first
loosen the gold in it with the point of the pincers, and tap the
capsule with the pincers so as to cause the particle to enter the
pan, which latter has been removed and placed on the clean floor
is
done
The
of gold.
1900
Jan.
Ag
and
Pb
preferably one of
Au
Au
Ag
15.8
3.10
3.10
12.7
17.2
The button
is
i-oz. capacity
58
avoid mechanical
FIG. 39.
PARTING-FLASK.
and some of the stronger acid added in order to remove the last
traces of silver. This is in turn brought to the boiling point and
then poured off. Note, that in all cases the assayer is to see that
the acid has completed its work before pouring it from the flask.
Turn
the flask so that the gold adheres to the upper side of it,
in hot water, or add it from the wash-bottle,
fill
the flask.
Be
is
Turn back
completely
inverted on the flask and the whole suddenly reversed. The
gold is seen to fall through the water to the bottom of the cup.
Cant it a little to one side, and quickly and quietly withdraw the
filled,
is
it
The
gold
cup
tapped together,
necessary, and the water
from
should
be
done promptly, or otherit.
This
work
poured
wise the dry-cup becomes soaked with water, and, when pouring
The cup is
off, the water will not be absorbed from the gold.
dried, and ignited at a low-red heat, and the gold, now showing
in the
its
if
is
Any
is
weighed.
may result in a
Or again particles
loss of particles
of dust
may
get
and
if
59
XIII.
Any variation in
plied by ten in reporting the ounces per ton.
the sample is also exaggerated in the same way. In the crucible
assay, however, one-half an assay-ton is commonly used, and
The difficulty may also be overresults become more accurate.
come by making
several
scorifications
silver
buttons into
two methods.
The
On
The
small cylindrical tin cup provided for each of the fluxes of the
following dimensions:
For soda,
"
i^
#
Y4
litharge,
"
"
argols,
borax-glass,
"
test-lead,
in.
diam. by 1^4
"
"
"
"
"
"
"
"
"
"
"
"
in.
"
high.
"
'"
"
"
"
"
"
7/s
%
i#
when
61
tinner.
They must
all
be
scales,
blade
level full.
is
now used
to
mix
fluxes.
spatula with a 6-in.
the contents of the crucible until they
downward.
points
The
muffle,
though
it is
well to place
may
them
is
cold.
loss.
The
crucible remains
time vary-
an hour. Sometimes,
the
time
is
as
when an occasional
however,
greatly exceeded,
bubble is seen rising through the molten charge. In any case
the charge should be hot, well fused, and liquid, and should pour
smoothly, without lumps and yet not be too thin or easily flowing.
ing, in general,
to half
After pouring, the assayer should look into the crucible to see
that it is perfectly smooth and with no unfused matter sticking
to
its sides.
them,
Sometimes
may adhere
the cupel tongs. Upon removal of the crucible from the furnace,
hold it by the tongs in the left hand, and, with the right, use a pair
are doing the pouring, and then neatly pour into a conical mold
After pouring, do not disturb the mold for five
(Fig. 10).
you have the lead forming a fin at the side of the mold. When
set, the cone of slag and the button are slid out on the grinding
plate, or on an anvil, the button is detached from the slag and
62
hammered
is
into the
remove the
to
form of a cube.
when
slag, and,
ready for the next operation of cupelling. Any slag left adherent
to the button shows itself when cupelling as a slight crust at the
edges of the cupel, and many retain a little lead, thus causing a
loss.
feather-litharge
less important.
is
This
hotter.
removed.
By
close
is
essential to
when
silver loss
The
can occur.
silver bead,
when brushed
to free
it
weaker
is
wrapped up
together with a
little
in
can
now
in the crucible.
memory
is
to say:
S equals S and b
equals
b,
is
63
and the
silica
borax the bases. In an extremely silicious ore the slag, even with
a good heat, may be stiff, so that when poured it runs with dif(sometimes not at all) from the crucible. Now, the 25 gm.
soda already prescribed is sufficient for all ores except the very
silicious ones, and when, as in the above case, this trouble threat-
ficulty
ens,
it
may
When
stone, dolomite, or
have a gritty
On
if
feel
light color,
would not
the other
acting in this
added to
The way
is
significant.
When
it
is
in
its
presence.
With
zinc
The amount
of borax prescribed
is
from
mum
present.
the
In particular,
maximum amount
stiff slag.
of
64
argols is also used, this lead is all reduced. Should there be lead
in the ore, this would also go into the lead button, and hence the
assayer must take care correspondingly to lessen the litharge.
lee- way
much
As
as 25
gm.
little
as 15 or as
and
Where
of nails
little
They
Galena
Blende
Pyrite
It will
is,
thirds.
needed
in
let
PbS
ZnS
FeS
.87% Pb
67% Zn
47% Fe
13% S
33% S
53% S
sulphur is 33%.
twice
the sulphur,
67%
in blende, the sulphur makes up one-third, the zinc twoNext we find the quantities of base varying by 20% up
nails are
and
its
is
Thus
and down.
the
all
65
if
we know
the
sulphur in blende.
Now
not consider the lead as a base, since it enters the button, not
showing up in the slag at all. Of the two remaining bases the
zinc
is
more
basic, blende
For
PbO
CO
C
PbO
Pb
CO
==
+ CO
+ Pb
2
The
or silver
is
is
suited
high temperatures,
is
fluxed by soda
thus:
SiO 2
Na 2 CO 3
Na SiO 3
2
CO,
there
first
Na B 4 O
2
At
ioH 2 O
heat
Na 2 B 4 O-
upon
first it
bases,
much
as follows:
FeO
CaO
+
+
Na 2 B 4 O
Na B 4 O
2
7
7
=
=
Na 2 FeB 4 O 8
Na 2 CaB O
4
66
forming
fusible berates.
all
proportions.
The
nails act
The
PbS
and for lead
in oxidized
PbO
so that, even
Fe
Pb
FeO
FeS
form
Fe
Pb
assay').
used for impure ores, or those containing certain impurities as -As, Sb, Fe, and Cu, which must be eliminated from
the lead button before cupelling. To do this the following charge
This
is
made up:
25 gm. soda (mono-carbonate), 30 to 120 gm. litharge, 0.5
A. T. ore, 3 to 15 gm. borax-glass, with argols or nitre to suit.
The quantity, either of argols or nitre, which is to be used will
is
charge.
To ascertain this reducing power
as follows:
o.i
we
This
it,
oxidized ore, to
upward of 30 gm.
if
the ore
is
an iron
pyrite,
by
five
we have
We
may have
either:
67
In
of one-tenth A. T. less than 4.
divide
subtract the product from 20, and
1.
by
5,
20
(2
5)
gm
2S
This
For
->
8
the quantity of argols to add in the regular assay.
In the second case, the reducing power being greater than
2.
4, we multiply by 5, subtract 20 from it, and divide the remainder
by
the oxidizing
4,
power
to be 22
power of
then
(22
nitre.
Thus suppose
the reducing
we have
20
5)
22.5
gm.
4
to be
added
to the
charge
in
to flux the
we may
silica.
may
much
arsenic, antimony,
It is this litharge
which
acts
This charge
is
68
in the furnace
crucible
is
On
is
made more
be
fluid
impurities.
using a
assay, to act
follows
is
sulphide
litharge 20
gm.
+ 5?bO =
+ 2PbO =
+ 3?bO =
+ FeO +
+ SO
+ SO +
2SO
lead,
much
as
FeS 2
PbS
ZnS
5?b
3?b
3?b
ZnO
The sulphur dioxide escapes as a gas, and the oxides are dissolved by the borax. But there remains a further amount of the
which
and which,
at a
high temperature,
2KNO = K O
3
is
nitre has
been provided,
decomposed.
+ 2NO + 30
the
for
example
FeS 2
CuS
=
=
+
+
+
+
5O
30
SO
+ O = SO
+ S0 = K S0
FeO
CuO
2SO 2
SO
Also
K
and
this floats
We may
note here, that where, in the nail-assay, copper is reduced to metallic form entering the button, it is here oxidized
69
and goes into the slag. Arsenic and antimony sulphides are also
oxidized according to the formula
:
As 2 S 3
Sb 2 S 3
+
+
90
9
=
=
As 2
Sb 2
+
+
3
3
S0
S0
2
2
PbO
We
Pb
we add
in the nail-assay:
more
CO
(as
may
be determined
impurities.
ROASTING OF ORES.
XIV.
Where an
to determine
little
gold,
it
may
be
first
roasted.
To do
snap and
fly,
causing mechanical
loss.
This
be guarded
may
it is
smelling of
its
contents.
CHEMISTRY OF ROASTING.
consist of a silicious
Of
most
decomposed, the
easily
first
FeS 2
The
to
sulphur, as
SO
2.
it is
FeS
S
and is burned
an increased tem-
With an abundance
3FeS
heat
equivalent
iiO
is
of air,
and
at
roasted as follows
2SO 2
Fe 2 O 3
FeSO
is
quite evident.
We
FeCuS 2
As
the heat
is
6O
increased to
decomposed, transferring
FeSO 4
CuO
FeO
2SO
The
of
it is
71
ferrous oxide
2FeO
+ O =
Fe 2 O 3
ZnS
PbS
and
at a
still
+ 30
+ 30
ZnO
PbO
==
+ SO
+ S0
higher temperature
its
decomposed, transferring
where much
(750)
CuSO 4
CuSO
4
+
+
ZnO
PbO
=
==
ZnSO 4
PbSO 4
+
+
CuO
CuO
As 2 S 3
90
As 2 O 3
3SO
-|-
Ores, because '-of the time and attention needed, are seldom
roasted; the assayer generally takes the shorter method of a
nail or regular assay, making them in duplicate, and combining
the cupelled buttons
when
the
amount of gold
is
but small.
THE ASSAY
OF ROASTED ORE FOR SILVER AND GOLD. One assayton of ore has been roasted so that it is oxidized and has lost
its
reducing power.
soda, 40
This
gm.
We
I A. T. ore, 40
accordingly take
gm.
20 gm. borax, and 2.5 gm. argols.
a No. F crucible, if it is to be done in a wind:
litharge,
placed in
the
borax being used as usual as a cover.
furnace,
of litharge, over that needed to form the lead button,
to take care of the impurities present. Where there
is
The
excess
is
intended
is
much
of
The charge
is
The
regular assay.
XV.
ASSAY OF MATTE.
is
The higher
little
button,
the solution
is
Also,
neutralized with a
is
XVI.
small
amount of
which
and the
silver is recovered,
is
added
result in
XVII.
much
Of
the second.
It consists in evaporating to dryness upon a hotsay 2 A. T. solution in a lead-tray made by turning up the
edges of lead-foil such as is used in assaying. This is formed over
a wooden block and may be 2 by 2 by ^4
deep. The evapora-
plate,
directly cupelled.
If,
is
The
results are
Measure
into a
No. 4 beaker
A. T. or 146
c.c.
of the solution.
Add
(If the solution is a 'barren one,' 10 A. T. should be used.)
to
it
Thus
the
solution
to
to
up
0.5%, KCy.*
enough KCy
bring
if the strength is 0.2% we shall need to bring it to 0.5% the addition
of
10
of a
10%
salt.
Add from
(PbA)
slightly acidified
have
+
+
+
PbA
2KAuCy
2KAgCy
and bring
to boiling.
Zn
Zn
Zn
Stir
it
2
2
75
=ZnA
+
= K,ZnCy +
= K ZnCy +
Pb
2Au
2Ag
strong HC1
4
4
Add
15
c.c.
to dissolve
with a flattened glass rod, decant the solution. Wash the sponge
it into a clot with the
fingers, and place it
upon a
To determine
Have 50
follows
Run
precipitate,
in cautiously the
standard
AgNOs
to dissolve
the beaker has been stirred, that is, when only a faint opalescense remains.
Ten c.c. of the standard solution equals \%, so that the reading is to be
divided by 10.
Thus suppose our reading was 14.5 c.c., then we will
have 1.45% KCy present. For very dilute solutions we may take 130
and then the burette reading must be divided by 100.
c.c.,
ASSAY OF BASE-BULLION.
XVIII.
Base-bullion, or work-lead,
and may
upward of one per
blast-furnace,
taining
are taken from each ingot or bar, there would be 800 of them for
a 4OO-bar carload, and amounting in quantity to a quart.
plumbago crucible is made red-hot in the wind-furnace, and the
down, and
is
it
by means of a scoop.
stirred with a
wooden
The
stick.
It
is
then lifted by
J
8
FIG. 40.
BASE-BULLION SAMPLE.
bered;
by means of
one of these
is
in. thick.
This bar is cut longia chisel, into two, each half being numsent to the refinery and one retained by
the
little
higher
is
AUSTIN
FIRE ASSAY.
77
Some
assayers prefer always to scorify before cupellation, contending that the loss is less in scorifying than in cupelling.
to
Where
large
it is
XIX.
in a thousand.
to
refined in a crucible,
some
and
just before
is
or scorifier, and poured from a height of three feet into a bucketThe metal is broken into fragments and shot of
ful of water.
all sizes
selected particles of
any desired
size.
Where
anneal them.
The operation
is
TRIAL ASSAY.
To
as follows:
is
we may
cut out a longitudinal strip 0.3 to 0.4 in. wide and cut this transversely into various sizes, down to mere shavings, in quantity more
than
sufficient for
is
wrapped up
in
20 gm.
79
and the
balance,
is
performed
foil
at a
at a higher temperature.
FIG. 41.
METAL ROLLS.
moment
of blicking,
it
should be put on
8o
been absorbed by the molten metal, and which, upon solidiis seeking to escape.
The cupel is gradually moved
forward to the front of the muffle and as soon as the silver gets
just
fication
removed.
is'
solid,
The
resultant button
is
number
is
The
WEIGHT OF LEAD
IN GRAMS
FINENESS
950 to looo
800 to 950
600 to 800
600 and less
10
15
20
mg. equal
them
all at
the
The
feather-litharge.
considered as being the same.
of the
such a
in
cupellation loss of
The
fineness
3i7
(2
as to
is,
therefore,
form
may be
the sum
loss in cupelling.
which
way
each of these
Thus
Then,
6) == 647,
be noticed that the proof
It will
81
cupellation-loss, or
512
-f-
we may
3/7
FIG. 42.
assumed
to be copper
assay in the
The gold
is
the weight
milligrams being the fineness, and this
checked by parting the proof-button.
in
may
be
XX.
The
and
when
25
c.c.
is
The
in.
put
solution
thus
Cu
Ag + 4 HN0
3 ) 2
We
common
salt
(NaCl)
chloride.
AgNO
The
solution
is
+ H SO =
washed
c.c.
10%
solution of
of sulphuric acid
PbA
cally.
stirring, 2
still
3.
of a
(i part acid to
until settled.
c.c.
PbSO 4
in falling, carries
+ H A,
2
down
and the
The
precipitate
filter
paper
is
gm. of borax
When
is
83
XXI.
100 mg., and for a large one, 500 mg. may be taken.
The base metals are first removed by cupellation, wrapping the
500 mg. in 10 gm. of lead-foil. There remains behind the pure
gold-silver button, which
is
weighed
it is
is
It is
annealed and then passed through the rolls (Fig. 43), which
it out into a piece about four inches in
length. When cold
draws
rolled
The
which
is
contained
quite coherent,
silver.
The
doubled to express
the fineness.
This
assays.
offices,
XXII.
The
is
We
the screen.
arately.
Place that quantity on the pan of the pulpand make up to the half-ton with fines. We thus assay
the whole sample in the proper relative proportions, and easily
centage in grams.
balance,
Thus
if
we would have
29.166
156
623.3 oz
7-3
per ton. Let us say that the fines weighed 720 gm. and assayed
1
720.0
7.3
727.3
Where
X
X
623.3
into
= 82800.0
= 4550-1
87350.1
20.
oz.
per ton.
result to be but
86
_%
An
"-
follows
Ag
to contain 54 oz.
XX)
found
per ton.
The
residue
Hence we have
124.0
0.8
X
X
124.8
0.3
54-0
= 37.2
= 43- 2
into
80.4
X
X
0.64=
54-0
142.00 into
89.12
= 148.50
237.62
= 1.67 oz.
Ag
per ton.
XXIII.
Any
in
10.
roast.
10 gm. ore,
20 gm. soda,
5
gm.
argols,
to 5 ten-penny nails.
is
melted
down
gradually so
is
complete.
Drops
clinging to the nails as they are withdrawn
from the crucible before pouring, indicate incomplete reduction.
The melt is poured into a conical mold, and, as soon as cool, the
lead button at the point of the cone is removed and hammered to
remove adherent slag. The button is weighed to the nearest tenth
of lead,
still
silver assay.
stiffer,
than from a
to fluxing should be
taken as in a nail-assay for silver. The soda fluxes the silica and
dissolves any matte which may be formed. The quantity of borax
to the
amount of bases
present.
Lead,
that
it is
reduced, does not enter the slag and hence is not a base
The nails are put in accord-
"
5
borax.
a lo-mesh screen.
When
The
ore,
cover of
number
salt,
of nails.
one-fourth
Additional
Some
method
that gives
him the
best
4950
179709