UN I V E RS I T Y O F C A L I F O RN I A

D E PA RT ME N T O F MI N I N G AND ME TA L L URG Y

A SS A YI N G L A B O RA T O RY

S . B . C H RI S TY

De a n

L A BO RA T O RY I NS T RUC T I O NS F O R

F I RE A S S A YS O F GO L D,

S I L VE R, A ND L E A D

MI N I N G 1 07 a -
b

W A LT E R S . MO RL E Y
A s s i s ta n t P r o fe s s o r of Me t a l l u r g y

I
UN V E RS I TY O F C AL FO I R N I A PR E S S
BE R$ E LEY

1913
 PRE FA C E

These instruction sheets h ave bee n prepared in this f orm to

take the p l ace o f mimeograph copies whi ch were former l y used
by s tuden t s e l ecting the course in fire assayin g at t h e University
of C aliforn ia These notes are co n cise directions for th e carry
.

ing out o f cert ain l ab o ra t ory work an d in no w ise cover the

,

ground o f the l ec t ures whi ch supplement the instruction in t he

la b oratory .

The purpose o f th e course i s not to teach mere l y practical

fire ass ayin g but a l so t o f ami l i arize the student w ith meta l
,

l u r g ic a l principles w hich underlie sme l tin g op erations on the

l a rge scale ; and in the l ectures as much emph asis is placed on
the underlying metallurgica l p rinciples as on the p ractica l
details o f fire assayin g.

The laboratory work is divided i n to twenty fi v e assignm e nts

'

-
,

thirteen o f which are intended to cover the work o f the first

‘

half year and the remaining t e l ve the work of the second half
-
, ,

y e ar In addition to the twe l ve assign ment s o f the seco n d half

.

year there will be given as time p ermits assign ments relating

, , ,

to the fire assays of mercury tin cobalt and antimon y a n d the

, , , ,

determination o f carb on sulphur and ash in coal and coke

, ,
.
 TA B L E OF C ONT E NT S

C HA P T E R I

P RE L I MI N ARY W OR$
1 .

2 . P r a c t ic e in C u p e l l a t io n
3 . P a r t in gGo l d a n d S i l v e r
4 . Fir e A s s a y o f L e a d B u l l io n

C HA P T E R I I

S CORI F I CATIO N A S S AY S

S c o r ifi c a t io n in Ge n e r a l
S c o r ifi c a t ion o f S il v e r Or es
$ u a r t z Go l d O r e s c o n t a in i n g l e s s t h a n o n e h a l f P y ri t e
- -

$ u a r t z G o l d O r es c o n t a i n i n g m or e t h a n o n e h a l f P
-
y r
-
it e

S c o rifi c a t ion A s s a y o f S a mp l e s H ig h in C opp e r

S c or ifi c a t ion A ss a y o f Or e s a n d P rod u c t s F u s ib l e w i t h D i ffic u l t y .

Ge n e r a l P r a ct ic e

C HA P T E R I I I

CRU CI BL E A S S AY S
D e t e rm in a t io n o f Go l d a n d S i l v e r in L it h a rg e : o f t h e R e d u ci n g
P o w e r s o f C h a rc o a l A rgo ] a n d F l o u r a n d A s s a y o f F l u x e s
, , ,

$ u a r t z Or e s $

N it r e A s s a y f or Or e s c o n t a in i n g M od e r a t e A m o u n t s o f P y ri t e
Ni t r e A s sa y f or Or e s c o n t a in in g L a rg e A m o u n t s o f P y ri t e
R o a s t in g Me th od f or Or e s c o n t a i n i n g L a rg e A m o u n t s o f P y r it e
A ssa y o f S ul p hid e Or es b y Na il Me th o d
$ ”

A s s a y o f T a il in g s

C HA P T E R I V

B U L L I ON A S S AY S

A s sa yo f Go l d B u l l io n
Fir e A s s a y o f S il v e r B u l l io n

CHA P T E R V

MI S CE L L A N E OU S W OR$
F u r n a c e R e p a ir s M a ki n g Cu p e l s
.

M e l t in g Re fi n in g a n d S a m p l i n g o f Go l d a n d S il v e r B u l l io n
, ,

C omp a r is o n o f Me t h od s f or A s s a y o f C opp e r b e a r in g Ma t e ri a l s
-

P r a c t ic e in S a mp l i n g P a n n in g a n d A m a l g a m a t in g
, ,

F ir e A ss a y o f L e a d Or e s
[5]
 THE —
N O T E B O O$

$ S t m
ys e a i
t c, t
n eaa n d a c c u r a t e n o t e t a k in g is o f j u s t a s m u c h
-
,
i f n ot

m or e impor t a n c e t o t h e s t u d e n t o f fi r e a s s a y in g th a n t h e a c t u a l d e t a i l s
,

o f t h e w ork i t s e l f Ca r e f u l n o t e t a ki n g in v o l v es c l o s e ob s e r v a t io n a n d
.
-

co n c e n t r a t io n . A m e r e n u m e r ic a l r e s u l t w ith o u t a s t a t e m e n t o f t h e
,

c o n d it io n s go v e r n in g t h e e x p e r im en t is n ot w a n t e d W i t h a p a rt ic u l a r
, .

num e r ic a l r e s u l t s h o u l d b e gi v e n a l l t h e e s s e n t i a l f a c t s c o n c e r n in g t h e
e x p e r im e n t ,
a s d e t e rmi n e d b y ob s e r v a t io n r e a d in g a n d t h o u g ht
,

Sy s t e m a n d n e a t n e s s a r e e s s e n t ia l ch a r a ct e r is t ic s o f a goo d e n g i n e e r
,

e s p e c ia l l y a m in in g e n g in e e r ,
wh o s e d u t ies o ft e n t a k e h im in t o p l a c e s
wh e r e h a rd s h ip dir t a n d di s ord e r a r e t h e r u l e
.

.
, ,

Y ou s h o u l d t a k e y o u r n o t e book n o t o n l y i n t o t h e l e c t u r e roo m b u t
-
,

in t o t h e f u r n a c e room a s w e l l . W ri t e do w n y o u r ob s e r v a t io n s wh il e
t h e y a r e f r e s h in y o u r m e m ory $ e e p y o u r n o t e b ook c l e a n y o u r w r it in g
.
-
,

l e g ib l e a n d y o u r dr a w i n g s n e a t
,
.

P rop e r l y t a k e n c a rb o n c op ie s a r e e xp e c t e d a n d th ey s h o u l d b e h a n d e d
,

in n o t l a t e r t h a n o n e w e e k a f t e r t h e e x p e r im e n t h a s b e e n p e r f orm e d .

[ ]
6
RE GULATION S C OVE RING W OR $ IN THE A S S AYING
LA B ORAT ORY

B e f ore commencin g w ork each studen t shou l d be supp l ie d ,

with the f o l owing art ic l es

1 . Copy o f Fu l ton s Ma n u a l f
’
o F ir e A s s a y in g .

2. C apsu l e box containin g six porce l ain capsu l es three

-
,

ung l azed capsu l es three $ ennedy p ar t ing fl asks three

,
-
,

t es t t ubes needle a n d mag nifier

,
.

Laborator y f older with centime t er ru l ed paper -

,
ar
ran g ed f or ca rbon copy .

k
l
i H H H l ead penci l
'

m S et o f B ecker ( or equi v a l en t ) w ei ghts f rom 1 gram to

1
/1 0
/
mi ll i g ram .

Pai r o f bone t ipped p incers

-
.

Pair o f stee l p incers -

.

Pair o f bead p l i ers .

Bl o w p ipe
-
.

10 . Laboratory suit .

E ach student should repor t prompt l y f or work at the a p

poin t ed hour and s h ould stay t he fu ll l abora t ory period unless
, ,

excused .

’
‘

A l l fires shou l d be drawn by o c l ock .

A ll apparatus shou l d be l e f t in its proper p l ace and in order .

[7]
 CH A P TE R I

P R E L I M I N A R Y W OR $
A SS I GNME N T 1

W E I G H ING
In this assi g n ment you are exp e cted t o become thoroughly
famili ar with the const r uctio n a d j u s t m en t u s e and care o f an
, ,
~

assay balance . Read carefully all the references given at the

end of this assi gn ment
An assay balan ce is similar to a chemi cal balance except t h at ,

the movi n g parts are made li ghter and instead o f l im it in g the

,

sensibility to 1 0 mg it i s made to weigh accurately to 0 1 mg

. . . .

W ith t h e bala n c e you use this is do n e entirely b y the method of

d e fl e ctio n s L ater on you will b e given a b alance with a rid e r
. .

C alculat e the se n sibility of the balance assi g n ed to use as ,

follows : After a couple of oscillations take readings first on one ,

sid e and then o the oth r for example :

n e —

P A N s E MP TY

2) . 05
- 03 Res t i n g p oi n t l e ft
,

Repeat the r e adi n gs u n ti l u n iform results are obtained

the restin g points do n ot agree i n creas e t h e number of readings
,

o n a side. After a little practi ce two readin gs on on e side and

,

o n e on th e other will su ffi ce .

I n this assi gn men t record all readings in your notes Aft e r .

you have become skillful in r e ading recordi n g will not be n ec es

,
.

sary In taki n g re a dings do not let the needle vibrate more than
.

a total of five divisions .

[ ]
8
 Now place your mg weight on the l e ft p an allow needle
.
,

— f or
to swi n g as b efore a n d det e rmine t h e new restin g point -
,

example

MG . W E I GH T ON L EFT PAN

7 15
3 33
2)
5 24 2nd es t i n g p oi n t r i g h t
r ,

03 l t
s r es t i n g p o i n t l e f t
,

5 27 D i ff eren e c

The difference between the two restin g points is the numb e r

o f divisio n s on the ivory index th rou gh whi ch é mg has caused
l .

the n eed l e to be de fl ected .

The sens ibility of a balance may be defined as the de fl ection

caused by 1 mg ; Or express ed in a n other way t h e sensibi l ity
, ,

is th e wei ght in hundredths of a mi lli gram which wil l cause t h e

ne e dle to b e defle cted on e divisi on on the i n dex .

In the above example the sensibi l ity is

,
divisio n s or .

.0 95 mg.

As you can readily r e ad to tenths o f a division the bala n c e ,

will be sensible to 0 1 mg Were the beam p erfectly rigi d this

. .
,

se n sibility would hold for much great e r loads than are usually
wei ghed on an as say balan c e, but f or a load o f even grm
$

there is a perceptib l e ch an ge To t e st thi s place a load of 1 gram

.
,

on each pan o f the balan ce and determi n e the sensibility as you

did wh en the l oad was zero Comp are results . .

You are now ready to wei gh by the d efl ec t ion method Obtain -

a number of pieces of gold or silver weighing from 1 to 1 0 m e

Weigh each separately and the n all together Add up the .

separate weights and comp are with the total weight Repeat .

until your results are consistent .

[9 ]
 Make a fu l l a n d c omp l e t e record of yo ur observations .

B efore leaving the balance see that the beam is l owered and .

the case c l osed .

The f oregoing method of weighin g is speci ally adapted to

the poorer grades o f bal an ces in use When a rider attachment .

$ ”
is available the rider d efl ec t ion
,
method may be used the
-
,

rider taki n g th e place o f the 2 m g and smaller weights This . .

method is the one ordinarily used in ass ay work W ith an .

exceedingly sensible and w ell constructed balance the method -

of n o d efl ect ion s ( see Fulton s Ma n u al of A ssa yin g ) m ay be

”
'

$ ’

used .

Make a drawi n g o f your bala n ce shelf showin g the method ,

used to secure a firm founda t ion : give dimensions of f ounda t ion

supports width of S hel f e t c
, ,
.

RE F E RE N C E S
F u l t o n : Ma n u a l o f A ss a y l g pp 4 2—5 2
/
,
. .

A a ro n : A s s a y in g p a r t I pp 2 7—38 a n d 1 2 7
, ,
.

T h orp e : $ u a n t it a t ive Ch emic a l A n a l y s is pp 3 33 , .

-
.

C a t a l o g u e s d e s c r ip t iv e O f t h e b a l a n c e s m a d e b y B e ck e r ,
T r o e mn er ,
A in s w or th S m ith
,
T h omp s o n a n d $ e l l e r ,
.

A SS I GN ME NT 2

PRAC TI C E IN CUPE LLATI ON

A Place h a lf a doz en dry cup e ls in the mu ffl e and build a
.

fire in the usua l manner As coke is used for f uel it is necessary

.
,

to have a good coal fire start ed be f ore addin g the coke Let the .

mu ffle heat up unti l a bright red is reached th e n arran ge the ,

dampers so tha t t h e heat re m ains u n iform B efore cupelling .

,

s e e that the fire is so l id aroun d the mu ffle .

Now obtain six lead b uttons wei ghing app roximately 1 5 ,

grams each Cupe l in se t s o f t wo each in the fol l owing man ner :

.

B ring two o f the cup els forward say withi n two inches of the
front of the mu ffle Place a lead b fit t on in each using the cupe l
.
,

[1 0 ]
tongs then shove t h e cupel s back i n to the hotter part o f the
,

mu ffl e Close the muffl e door for a few mi n utes When t h e

$

. .

buttons have melted and cup ellation has commenced as sh own $

by t he fumes o f litharge Op en the door and arran ge the dam pers

.

so tha t the fumes are drawn slowly off through the rear of the
mu ffle Try to kee p the t emp erature const ant i n creas ing it only
.
,

when t he l ead has almos t disappeared . The heat is t oo l ow .

w hen the fume s become heavy a n d dark an d a scum f orms ,

aroun d the edge o f the molten T h e h e a t is too high when

the f umes o f l itharge rise rapidly t o t he t op Of th e mu ffl e and
‘

the l e a d a p pe a r s to be boilin g The h eat is j ust ri ght w hen

$ '

c rysta l s o f lith arge f o rm in the cu pe l P ractice wi l l enab l e you .

to fix upon the p roper co n diti on s .

Cupel the remainin g f ou r and as many more as you h a ve time

f or du ring the p eriod '
.

Make a f u l l an d c o mp l et e re cord o f your observ ations .

S tudy care fully the f o l lowi ng r ef e rences

RE F E RE NCE S

B ro w Ma n u a l Of
n : A s s a y in g ,
’

pp . 2 1 4 —2 2 3 .

F u rm a n : A ssa yin g pp 1 38 1 4 2 ,
.
-
.

B od e m a n $ e r l : A ss a y in g pp 1 1 0— 1 2 4 ,
. .

R h e a d $ S e x t o n : pp 1 0 9— 1 1 5
’

. .

B .Rol l out a si l ver coin to t he thickness of an ordi n ary

visi t ing card A n nea l the coin repeatedly during the Oper a tion
.
.

Clean w ith sandp ap er No w wei gh out on your bead balance six

$

ass ays o f t his coin t hree weighi gn 2 5— 30 mgs e ach and three
,
.
,

wei ghin g 90 1 00 mgs each Wei gh each bead accurate l y Wr a p

— . . .

each as say in 1 5 grams of sheet lead weighed approximately on ,

the pulp ba l ance Arrange th ese six assays in sets of two each
.
,

so th at each set wi ll co n tain on e 2 5 30 mg assay and one 90

— .

”
1 0 0 mg ass a y. Cupe l one set at a time as in A
. only using ,
$
,

more care on accoun t of t h e resulti n g silver b ead Try t o

‘

f eather the cupe l s and at the same time bri g h t en t h e beads .

[ 1 1 ]
 R emove the be a ds from the cupels and clean thoroughly by
brushin g Place th e m in thei r respective capsu l es and take to
.
,
‘

the balance room Weigh and report in this form .

,

S il e
v r
A ss ay N o . Re m k s
C oi n Wt . B e d
a fi neness ar

1 88 0 W e l l f ea th e r e d ;
brig ht e n e d a t
prop e r h e a t .

T h e term si l ver fineness as used above refers to the number , ,

of parts of si lver found in 1 000 p arts of the coin .

C ompare the results a n d note the average p ercentage si l ver ,

losses for the 2 5 30 mg ass ays and for t h e 90 1 00 mg as says

— — . .
,

taking into account o f course the known fineness o f the si l ver , ,

coin used .

Dissolve a piece o f coin si l ver in nitri c acid and test with

ammonium hydroxid for copper ; a l so test a we l l bri ghtened bead -

in the same ma n n er What deductions do you make ? .

C Obtain from the storeroom six lead buttons

.
,
packets ,

havi n g res pectiv e ly the followin g compositions

, ,

1 . Lead an silverd .

Lead silver a n d gold

w
,
.

Lead ,
silver a n d antimony .

Lead ,
si lver and copper .

‘
9 Lead ,
silver and tin .

Lead silver and iro n

3
3
5 .
,

Cupel in s e ts of two e ach E n deavor in each cas e to make .

, ,

a p erfect cupellatio n Observe carefully in each case the h e at .

, , , ,

tim e and manner Of brightening ; observe the f ormation of any

s coria its color etc ; note in each cas e the colo r and genera l
, ,
.
, ,

appearance o f the cupe l after brightening .

Make a fu l l a n d c omp l e t e report .

[1 2]
 A SS I GNME N T 3

PAR TING GOLD AND S ILVE R

To be a success f ul assayer one must be able to p art correctly
and rapid l y Nicety o f man i pu l ation i s required and the only
.
,

way to acquire this is to p ractice conscientiously DO not t a ke .

’
anythi n g for granted There are three steps in an assayer s .

work whe re he must be sure viz : ( 1 ) That th e sample is what ,

it rep resents ; ( 2 ) that nothin g but go l d i s wei ghed as such ;

( 3 ) th at the weighing is done accurate l y W i t h these points .

looked to carefully the rest wi ll be comparatively easy Per f orm,

.

care fully t h e f o ll owin g experiments

/
W e ig lit ou t six pieces of gold foi l on your be a d ba l an ce to
.0 1 m g ; each piece shou l d co n tain about 5 mgs
. A ll oy the pieces .

o f go l d with 1 2 3 4 5 and 8 times their wei ght of silver

, , , , , ,

respective l y Wei gh the S i l ver also on your bead bal ance to

.
,

.1 0 mg on l y . .

To alloy wrap the gol d and si l ver in about 1 gram o f sheet

,

l ead and cupel in the mu f fle t akin g care to ha v e the cup e l ,

smooth dry and h ot Th e mu ffle shou l d be sl ightly hotter than

,
.

f or ordi n a ry cupell a tion After alloyin g remove the bead from

.
.

the cupe l b y ¥ m e an s o f the bead plyers brush thorou ghly and

~

, ,

place i n t h e porcelain capsu l e used f or p arting Tr eat each of .

.

the five beads thus and remove to th e p ar t in g room Now fl atten .

ea c h bead usi n g the sma ll b l owpi p e hammer and anvil Return

, ,
.

t hem to thei r respective capsules whi ch should the n be filled ,

with hot w eak parting acid ; heat s l o w l y on th e hot plate and

, ,

when al l action has ceased repl a ce the spent acid wi t h strong ,

acid and heat f or three minutes at boilin g point Then remove .

from the p l ate p our Off the acid a n d was h three times with
, ,

distil l ed water ( preferably warm ) Dry over the hot plate then .
,

annea l by heatin g to redness over the B unsen fl ame Coo l and .

weigh Report results in this f orm :

.

Wt . G old t k en a S il v er R a t io Wt . of P r t e d Gold
a Rem k s ar

1 to 1 No t a ct e d u po n by a c id .

Wha t do your experiments determine ?

[ 3]
1
 D escribe niin u t el y the action o f the acid on the sev era l bea ds .

NO E
T — Flatten a ll doré bea ds un l ess they are known to
co n tain more than ei ght p arts o f si lv er

RE F E RE N C E S
B ro w n : Ma n u a l o f A ssa y in g pp 2 2 4—2 39 , . .

F u rm a n : Ma n u a l o f A s s a y in g pp 1 45—1 46
.

,
.
_
.

B od e m a n $ e r l : A s s a y in g pp 1 98 — 2 0 0
, . _ .

F u l t o n : Ma n u a l o f A ss a y m g pp 1 0 7— 1 1 0
/

, . .

A SS I GNME NT 4

FIRE A S S AY OF L E AD B ULLI ON
Chip or sa w off four A T s a mfl es f rom the bul l ion gi v en
. .

you and a ssay according to the directions given in F ul ton s

,
’

Ma n u a l of A ssa yin g .

Repor t both gold and S i lv er v alues I n this f orm

Per t o n

To get correct results in this as si gnment the cupe l la t ion must

be do n e perfectly so in a measure this assignment w ill tes t your
,

ability to cupe l .

Explai n the term A T . .

RE F E RE N C E S

F u rm a n : Ma n u a l of A s s a y in g , pp . 1 4—1 7 an d 2 7 2 2 75 .

[1 4]
 CHA P T E R I I

S CORI E I OA T I ON A S SA Y S

A SS I GN M E N T 5

S C ORIFI CA TI ON IN GENE RAL

In this s i gnmen t you are expected to get a genera l i dea o f
a s

the sc o r ifi c a t ion process as f ar as can be done by readin g

A brie f outline Of the work in s c or ifi ca t ion is gi v en belo w
1 . S or ific a t ion f sil ver or es
ass a y o

( a ) S i l v er l ead ores
-

Those containing no lead but quartz me t a ll i c si l ver , ,

and si lv er comp ounds .

A genera l ch arge for ores o f the abo v e c l as s is :

Or e 4
$ 0 A . T .

Gr a n ul a t e d l ea d 3 0— 35 gr a m s
B or a x gl a s s gra m
Us e in . s c o r ifi e r s

Thi s cha rge with sli ght modifications wil l t rea t any si lv er ore ;
, ,
'

if t he ore c onta i n s more than 50 p er cen t o f p y r it e t h e l ead

‘

may be i ncr eas ed up to 4 5 grams And i f much l ime zinc or .

,

antimony is present the borax glass must be incre a sed up to as

,

much as th ree grams in exception al cases Where the samp l e .

is r ich and at the same time homogeneous t he w ei ght o f the

sample t aken may be decreased to A T .

2 . S c or ific a t ion fas sa y o r ic h g l d or es

o

As wi ll be noti ced from your readin g the s eo r ifi ca t ion ,

”
assay is primarily adapted f or si l ver ores and rich g old ores .

f or e v iden t reasons To ge t the required amount o f samp l e f or

.

a med ium or p oor go l d ore i t becomes necess ary t o make severa l

,

s c o r ifi ca t ion s and t hen scori f y the resultin g buttons t o g ether ,

or cupe l sep arately and p art t oge t her .

[1 5]
 ( ) $ uartz
a gold or e s co n sisti n g la rgely of quartz —The .

charge give n for silv e r or e s c a n be used e qually well for quartz

gold or e s co n tai n in g less than 50 per ce n t pyrite though in most ,

cas e s it is bett e r to take mor e than A T a n d co n sequen tly . .

more lead a n d a larger sc o r ifi e r i f n ecessary .

Whe n A T of ore is used 30 grams are su fficient a n d

. .
,

with A T 5 0 grams of lead had better be u s ed

. .
.

$ uartz pyrit e gold ores consistin g larg ely of pyrite

-
.

O w i n g to th e large amou n t of lead required to scori fy ores of

this class it i s impracticable to u s e more than
, A T of ore . .

in on e s c o r ifi e r so to accomplish the sa me result it b e c o mes

,

n ecessary to u nit e the lead buttons as sugges ted above .

T h e u s u a l c h arge is
'

Or e $4 0 A T
. .

Gr a n u l a t e d l ea d 4 0 —4 5 g ra m s
B or a x g l a s s 1 )
7 4 gra m .

3 . S c o r ific a t io n a s sa y o f sa mp l es c o n t a in in g a l a r g e p er c e n tag e
of c op p er .

In samples of thi s class it is necessary to use a small amou n t

of ore a n d at the s a me tim e a l arg e amount of l e ad ; this is due
to the rete n tion of copper in t h e lead a n d the di ffi culty in
r e movi n g it unl e ss a su ffici en t amou n t of lead is used If a n y .

great amou n t of copp e r is r e tai n ed in the lead butto n a hi gh ,

heat will b e n ec e ss ary to remov e i t duri n g cupellatio n This .

will produce a hi gh loss in silver va l ue ; so it is al most imperative

to add enough lead durin g s c o r ifi c a t ion to i n sure the r e moval
o f the copp e r wh en th e silver loss will be small in comparison
,
.

The usual charge is

Or e 1
7 0 4 or A T . .

Gr a n u l a t e d l e a d 45 or 5 0 gr a m s
S il ic a an d b or a x .

4 . S c or ific a t io n a ss a y f
o o r es an d p r od u c t s fu s ib l e w it h
d iflic u l t y .

[ 1 6]
 Make the six s c or ifi c a t ion s at o n e tim e in the mu ffle as sign e d
'

to you H ave the mu ffl e at a bright red b e fore placi n g t h e

.

charges in it ; when the charges are in close the mu ffl e door I n , .

a few mi n utes draw the door aside sli ghtly and if the lead is ,

me l ted remove the door compl e tely and arra n ge the dra fts so
,

that there wi ll be a strong current of ai r through the muffle .

Durin g the s c or ifi c a t ion the heat should be maintai n ed at a

mediu morange or a litt l e above a good heat for cup elli n g
,
.

Increase toward the e n d to a full ye l low As soon as the bul l s ’

.
$

”
eye h as di s appeared pour into a warm ed s c o r ifi c a t ion mould
, .

When al l the charges have been remov ed from the mu ffle place ,

six cupe l s in so they may be i gnited by the time the buttons are
s l agged and ready for cupe ll in g .

Cupe l the six buttons a t one time featherin g them a l l ; Wei gh ,

each be ad separately ; part the beads together in sets o f t hree in

$ ennedy partin g fl asks and wei gh the go l d ,
.

S a mp l e A S i l ver ore containin g a quartz ose gan g ue .

S a mp l e A quar t z silver ore -

.

Prepare six ch arges o f this sa mple each as fo l lows ,

Ol '

e A T . .

Gr a n u l a t e d l ea d 30—35 gr a m s
B or a x g l a s s gr a m
Us e in . s c o r ifi e r s

Cupe l the six buttons at one time f e a therin g them al l Wei gh , .

each bead sep ara t e l y ; part the beads together in sets o f three in
t es t t ubes an d w ei gh t he go l d Record the resu l ts in this form : .

P er t on
A ss ay S a mp l e Wt . Oz . Oz .

Dat e NO . N o . Or e Gold S il er
v

Oct 1
. 1 226 94
1
0 A T . . . 4

Average the results of the as says of each samp l e a f ter cal eu

l atin g them separa t ely for each assay .

Under remarks g i ve composition of t he ore manner of ,

scorifying and cupellin g .

If there is any reason to doubt the a ccuracy of the assay the .

res u l ts S hou l d never under any cir cu mstances be accep t ed

, ,
.

[ 8]
1
 Describe i n your notes the appearance o f the s c o r ifi er s an d the -

charac t er of the lead bu t tons W eigh out . A T o f the ore . .

and wash on a batea makin g you r se l f f amili ar with the con

,

s t it uen t minera l s and t he approxima t e percentage of each Use .

t h e b IOW p ip e i f necessary Make a det ailed report in your no t es

. .

Fo ll o w t he above direc t ions in al l f u t ure ass i g nments .

A SS I GN ME N T 7

$ UAR T $ G OLD ORE S C ONTAINING LE S S T H AN

ONE —H AL F PYRI T E

as says o f t his samp l e as f o ll ows

Or e l
3 A T . .

Gr ted
an u l a l ea d 30— 35 gr a m s
B o ra x g l a s s gr a m
Us e 2 % in . s c o r ifi e r s

and t hree ass a ys

Or e A T .

Gr a n u l a t e d l ea d 45— 5 0 gr a m s
B or a x g l a s s gr a m
U s e 2 34 in . s c o r ifi e r s .

Uni t e t h e t hre e bu tt ons from t h e fi r st ch a rge by r e sc or ifi c a -

t ion be f ore cupe l ling .Cupe l t he other three buttons directly

_

and in separate cupels ; wei gh separately for doré ; part one

a l one and two t o g et h er I f necess ary t o add sil v er be f ore part
.

in g a ll oy by means of blowpip e and dry cup el

,
.

Note the t ime requi red by each charge a nd t he size o f the

l ead button . Reduce by scori fyin g the size o f any b u t t On ,

w eighing o v er 2 0 grams Observ e t he f ollowin g p eriods in

.

scor ifi c a t ion o f su l phide ores ( consult your l ecture no t es )

1 . .

m
Mel t in g H a v e u ffle a t a lo w ye ll o w h eat . I n t roduce t he
s c or ifi e r and close t he mu ffle door .

[ ]
1 9
 2 Roas ting When t h e charges have thoroughly melt e d op en
. .
,

the door carefu l ly a n d allow as much ai r as p oss ible to pass

through the muffl e ; i f they begi n to bubble clos e the door so as ,

to decrease the ai r supply T h e heat duri n g the ro a sti n g period

.

S hould be kept at about a m e dium ora n g e A high h e at will .

cause mecha n i cal loss by too rapi d oxi datio n .

’
3 Fusion or formation of the
.
,
$
bull s ey e Wh en the
roasti n g has ce as ed close the door ,
a n d fuse dow n the charg e

thoroughly .

4 . S c o r ifi c a t ion
When t h e charge has thoroughly fused as
.
,

’ $
show n by the formation of the bull s ey e op e n t h e do o r a n d ,

allow a good curre n t of ai r to pas s through t h e mu ffl e Duri n g .

this p eriod the lead content i s reduc e d and the slag becomes more
fl uid .

5 Fina l heating Wh e
. n t h e lead is cover e d or almost cov e r e d
.

by t h e slag close t h e door a n d i n crease the heat to a full y ellow

,

an d then pour into heated moulds .

A SS I GN M E N T 8

$ UAR T $ GOLD ORE S C ONTAINING MOR E T H AN

ONE H ALF PYRIT E
—

S a mp l e

Prep are six charges of this sample as follows ,

OT C A T . .

Gr a n u l a t e d l ea d 4 5— 5 0 g ra ms
B or a x g l a s s g ra m

Us e in . s c o r ifi e r s .

S cori fy as directed in previous assig n ment ; cup e l separa t ely ,

f e ath e ri n g car e fully Clean the b e ads carefully combi n e in s et s

.
,

o f three wei gh and p art ; weigh ag a in Report both gold a n d

,
.

si l ver .

[2 0]
 A SS I GN ME N T 9

SC ORIF I CATI ON A S S AY OF S AMPLE S H I G HI N C OPP ER

S a mp l e and S a mp l e A copper matte .

Prep are five charges of each sample as follow s : ,

Or e A T . .

Gr a n u l a t e d l e a d 5 0— 55 gr a m s
B or a x g l a s s 1 gr a m
U s e 3 in . s c o r ifi e r s .

For copper matte add 1 gram o f si l ica with borax g l ass .

Control the furn ace as in ass ayi n g ores rich in pyrite B uttons .

from matte must be r es c o r ifi e d ; use in s c or ifi er s and h a ve .

total lead 40 grams Cupel sep arately the fi v e buttons f rom

. .

each sample featherin g the cupels at first and raisi n g the heat
,

at the end so as to ensure the remova l of a l l the copper B eads .

from each sample should be wei g hed sep arate l y bu t p art e d ,

t ogether .

What are the di fficulties encountered in assayin g ores ri ch

in c Op p e r ?

R E F E RE NCE S
F u rm a n : Ma n u a l o f A ss a y in g pp 2 9 0— 2 91
,
. .

P e t e r s : Mo d er n Co pp er S me l t in g pp 6 7— 7 1
,
. .

A SS I GN ME N T 10

'

S OORI E I OA T I ON A S S A Y OF ORE S A ND PR ODUC T S

FU S I B LE W I T H D IFF I CUL TY

S a mp l e Contains much antimony .

Prepare three charges as follows :

Or e A T . .

Gr a n u l a t e d l ea d 30— 3 5 gr a m s
B or a x l
g a ss 3—4 g ra m s

U s e 2 34 in . s c o r ifi e r s .

[21 ]
 S cori fy in the usua l man n er except at th e end when the heat
,

mus t be raised to a fu l l ye ll ow The buttons should be perfectly

.

mal l e able ; if they are no t r esc or if y w ith an addition Of t es t

,

lead Cupel f eatherin g care fully ; wei gh the beads separately

.
,

Part in one capsu l e .

A SS I GN ME NT 11

GE NE RAL PRA C TI C E

Take the samp l e given you and reduce by methods suggested

unti l you have at l east two p oun ds pass in g a 1 00 mesh sie v e ;
bott l e thi s and keep f or assay .

In this assig n ment you wil l be gi v en three or more ores in

,

addition to the one sampled You are to determi n e thei r com

.

position and then decide on charge you w ould use for assay by
s c o r ifi c a t io n method
.

Make a detailed report indi catin g the compositi on o f each

,

samp l e the ch arge used etc Give both go l d and si lv er v a l ues

, ,
.

[ ]
2 2
 CHA P T E R I I I

CRU OI RL E A SSA Y S
. A S S I G N ME N T 1 2

D E TE RMINATI ON OF GOLD AND S ILVE R IN LI T H ARGE

OF THE R E DUC ING P OWE R S OF C H AR C O AL ,

ARGOL ,
AND FL OUR ,
AND A S S AY
OF FLU $ E S

B e f ore making any assays t he as sayer shou l d de t ermine the

,

p reci ous meta l conten t o f t he l i t ha r g e used Lithar g e contain .

in g more than a trace o f g o l d shou l d be re j ected The p resence .

o f a smal l but uni form amoun t o f si l ver is rather an adv antage

than Otherwise as the si lv er ser v es to he l p collec t the g o l d
,
.

The ass ayer must a l so determin e the reducin g po w ers o f the

v arious reducin g a g ents ; and an assay o f a ll t he reagents used
” $
shou l d be made in order t o de t ec t any sa l tin g o f t he fl uxes .

F ir s t T o de t e rmine t he precious me t a l con t en t o f the

.

l itharge prep are t wo char g es as f o ll o w s

,

L i t h a rg e 1 00 gr a m s
A rgo l 2 gr a m s
Sa l t c ov er .

U s e a No 7 cr u c ib l e . .

To one charge a d d a smal l amount o f tes t si l ver

,
Fuse .

quick l y bo t h ch ar g es in a ho t fire unti l thorough l y l i quid the n ,

withdra w and pour ; cup e l the res ultin g buttons D e t ermine .

go l d and si l ver by weighin g the un all oyed bead f or t he doré ,

and p artin g the other f or g o l d I f more than a trace o f go l d is

.

f ound the l ithar g e must b e re j ected Note the S i lv er conten t

, . .
,

and correc t a ll assays accordin g to t he amoun t o f l i t harge used .

F or examp l e
in 1 00 grams o f l itharge w ei ghs 50 m g
S i l ver . .
,
l i t harge used
in assays weighs 60 grams doré bead wei ghs ,
mg . then
,

mg and the corrected doré is

.
,
or
mg .

[ ]
23
 S ec on d
To d e termi n e the reduci n g po w ers o f the reduci n g
.

age n ts argol fl our an d charcoal pr e pare charges as follows

, , ,
:

A rg o l 1 g r a m
S il ic a 30 gr a m s
L ith a r g e 75 gr a m s
S od a 25 g ra m s
B or a x c o v e r .

U s e a No F cr u c ib l e
. .

S u b s t it u t e f or a r g o l ,

Fl ou r 1 gr a m

3 . S u b s t it u t e f or a r g o l ,

Ch a r c o a l 1 g ra m

Reducing agen ts only should be wei ghed carefully Fuse

, ,
.
,

at o n e tim e th e above charges ; wh e n qu i et pou r into clean warm

, , ,

sl a g moulds Clean a n d weigh the resulting l ead buttons

. .

Wei gh usi n g pulp scales to the near e st 1 0 mg

, ,
.

Note that the above d e termi n ati o n s are made under normal
w orki n g co n di t io n s .

T h ir d
To make an as say of the fl uxes us e d prepare
.
,

ch arge as follows
,

S il ic a ra m s
30 g
L ith a rg e ra m s
75 g
S od a 2 5 g ra m s
B or a x gl a s s 5 gr a m s
R e d u c e r f or 1 8 g r a m b u tt o n
-
.

S a l t a n d B or a x co v e r .

U s e a No F c r u c ib l e
. .

Add a w e ighed amou n t Of test S i l ver to the char g e and f use

in t h e usual w ay D etermine gold and S ilv e r if any , .

[24 ]
 S u fficient
reducer should be used to produce an 1 8— 2 5 gram
lead bu t ton I f the ore is oxidizing se v era l grams o f reducer
.
,

may be neces sary I f the ore contai n s more than about 1 0 p e r

.

cent pyrites and no oxidizing age n t reducer will be at a mini ,

mum and a smal l amount o f oxi dizer as nitre may be necessary .

An ore containing more than about 1 5 p er cent pyrites cannot

be p rop er l y treated by this charge
Other reducin g a g en t s w hi ch may be used instead o f fl our
$

are argo l charcoa l or su g ar

,

Prep are three ch arges o f S ample usin g the charge

given be f ore and an F crucib l e This sample consists mainly of .

quartz w ith l ess th an 5 per cen t of su l phides o f i ro n lead a n d ,

copper and reduces

,
grams o f l ead per one assay ton of ore .

Un l es s the propor t ion o f S i lver to go l d in an ore is kn own to

be at l e as t five to one tes t S ilver S houl d be added to all charges
,

except one Wei gh the test silver added to on e o f the ch arges

. .

Thi s i l l ustrates three methods o f workin g an d w e h ave t w o .

checks on the go l d and two on the S i lv er The amount o f silver .

'

in the l i t harge w i ll o f course be d ed u c t ed f r Om the w ei gh t of

the doré .

On one charge use a salt co v er on t he others a borax cover ,

.

H ea t t he ch arge un t i l in quie t f us ion , then increase the h eat

to l ow yel l ow f or about fiv e minutes or u n til the charge becomes ,
.

smooth on t op Pour into c l ean warm slag moul ds an d w hen

.
, ,

c oOl break away the lead button ; c l ean hammer into cubes and , ,

t hen cupe l in t he usua l manner .

Repor t results in t he f o ll o win g form

Per t on

G old
Ass y a S a mp l e old
G S il ev r G old S il ev r
No . N o . Or e D o re mg . mg . oz . oz .
per oz .

1 483 1 A T.

Under remarks indicate everythin g t h at h as a bearin g upon

the resu l ts Describe the appearance of sl ag buttons e t c Which
.
, ,
.

co v er do you pre f er and w hy ? ,

[ 2 6]
 Make a v annin g t es t o f the ore usin g abou t A T o f ore , . .

and a batea Repor t this tes t a l so

. .

I f neces sary to use A T o f ore or t o make t he fusi ons in a

. .

mu ffle the fo ll owin g ch arge wi ll be f oun d suitab l e :

,

Or e A T .

L i th a rg e gr a m s 60
S oda 2 0 gr a m s
B or a x gl a s s 5 gr a m s
R e d u c e r t o g iv e a 2 0 g ra m b u tt o n -
.

Gro u n d b or a x co v e r .

U s e a No F cr u c ib l e
.

Prep are t wo ch ar g es o f S amp l e usin g the above

charge Add a w eighed amoun t o f t est silver to one char ge and
.
,

an un w eighed amoun t o f t es t S i l ver t o t he other Make the usual .

tes t s and f use as be f ore

,
.

To mix any charge put the soda into the crucib l e first then
, ,

the l i t harge and o t her fl uxes l ast l y t he ore and m ix all together
, ,

w ith a fork ; S prinkle salt or borax over the t Op Make certain .

the ore and flux es are t h o r ou g h l y mixed .

A SS I GNME NT 14

NI T R E A S S AY F OR OR E S C ONTAINING MOD E RAT E

AM OUNT S OF PYRI TE
Ores o f t his c l as s are usua ll y ri cher in gold and si l ver t han
t hose o f the p re v ious c l ass a n d c on s e qu en t l y less ma t eria l ma y
‘

be taken in assayin g t hem .

T he f o l lowin g ch arge w il l be f ound sui t ab l e f or ores o f this

c l ass
:

Or e A T .

L i t h a rg e gr a m s 90
S od a 2 0 gr a m s
S il ic a 1 0 gr a m s
B or a x gl a s s 5 gr a m s
N it r e a cc or d i n g t o pr e l im in a r y .

C ov e r

U s e a No 7 fl u xin g po t
. .

[ 2 7]
 '

Fusion of the c h a r g es sh ou l d be carri e d on as before .

C alculate the amount of n itre ( see below ) to add so that a

2 0 gram butto n will be produced from
-
A T of ore . . .

Make three a s a y s of S ample using the charge given

above S ample
. contai n s about sulphides .

Add test S i lver to all charges but on e B e fore comm e n cing .

work on this assignm ent be sure tha t the previous one is ,

thoroughly u n d e rstood .

T h e reducing ag ents whi ch are commo n ly prese n t in ores are

a n timony zi n c arseni c and sulphur Iro n pyrites the sulphide
, ,
.
,

commo n ly met with reduces as follows ,

F ifteen per c en t o f pyrite will reduce abo ut ni n etee n grams

of lead and there wil l be n o excess Mor e tha n 1 5 p e r ce n t Of
,
.

pyrit e usi n g,
A T of ore wil l reduce too larg e a lead button
. .
,
.

Nitre an oxidiz e r is us e d to co n trol t h e S ize of the l e ad butto n

, , ,

a n d is usually stated in terms of lead ; that is one gram of nitre ,

oxidizes four grams of lead more or l e s s accordi n g to conditi o n s , ,

.

In order to k n ow how much nitre to add so as to reduce , ,

within a few grams a 2 0 gram lead butto n w e must d e t e rmine

,
-
,

or guess correctly the amount of lead which will be reduc ed

befor e maki n g an ass ay .

The reducin g power of a sample may be determined b y making

a preliminary thus : ,

S a mp l e
L ith a rg e
Sal t c over .

U s e a N o 7 fl u x in g po t . .

H ave the fire hot when the charge is put in an d fuse qui ckly ;
wh en in quiet fusion r em ov e a n d pour Clea n a n d w e i gh t h e
’

.
, ,

button .

C alculate the amou n t of n itre which must be used on a basis

o f one gram of n itre to four grams of lead .

I n prep ari n g charg e of S ampl e add to on e charg e

gram more nitre a n d to the other gram less nitre than the
calculated amou n t Weigh the resulti n g l e ad buttons a n d
.
,

calcul ate the oxidizing power of nitre u n der these co n dition s .

Compare this res ult with the amou n t used above .

[28]
 A SS I GNME N T 15

NI TRE A SS AY F OR ORE S C ON TAINING LARGE

AMOUNT S OF PYRI TE

Materi a l of comp osition as indi cated above is in general

$

, ,

assayed in the same way as that of the previous assi gn ment .

T h e increas e in the amount of iron pyrites calls for an increas e

of litharge to complete th e oxidation ; and as the amount o f
sili ca in the ore is decreased and the charge becomes more basi c ,

more acid in the form of sili ca or wi n dow glass must be ad d e d -

.

The following charge wil l su ffi ce

Or e
L ith a rg e ra m s
1 20 g
S od a gr a m s 20
S il ic a 1 5 gr a m s
B ora x gl a ss 1 0 g ra m s
Nit r e a c c ord in g t o pr el im in a ry .

S a l t or B or a x co v e r .

Us e a No F or
. 30 g r a m
-
cr u c ib l e .

C alculate f or 20 gram button .

When the materi al to be ass ayed is a pure concentrate o r

nearly so the amount of nitre to be added can usually be p l aced
,

at about 2 5 grams for A T o f ore For materi a l of u nknown

. . .

percentage of pyrites a prelimi

,
n ary assay mus t be made .

In genera l ores of this typ e are ri cher than the type treated
,

in Ass i gnme n t 1 4 and a smaller amount of ore can be assayed

, ,

thus effectin g a saving in time and fl uxes ; when a sensitive

balan ce is available a n d the values are uniforml y distribut e d .
.

the results obtained by using a smal l er amount 14 A T will ,

. .
,

be even more accurate t h a n t h os e from z A T . .

[ 29 ]
 followin g charge will do wh en 14 A T . .

Or e A T .

L it h a r g e 75 g r a m s
S od a 1 5 gr a m s
S il ic a 5 gr a m s
B or a x g l a s s 5 gr a m s
N it r e a cc ord in g t o pr e l im in a r y .

S a l t or B or a x c o v e r .

U s e a 2 0 gr a m cr u c ib l e
-
.

Ca l cu l ate for 1 6— 2 0 gram but t on .

The ore t o be assayed in this assi gnmen t is a concentrate

ob t ained f rom one o f our mi ll runs and is a typica l concentrate,
.

Prepare three charges o f S ample usin g A T

. .
,
and
three using A T . .

Time requi red f or fusion about thi rty minu t es ten minutes ,

ye ll ow heat at the end Avoid h eati n g too rapid l y as a sudden

.
, ,

unev en heating may cause the assay t o boi l over

Report the mean o f the several as says as the correc t v a lue ,

first discardi n g any assay that appears to have been ab n orma l

in any manner

A S S I GN NIE N T 1 6

R OA S TING ME T H OD F OR ORE S C ON TAINING LARGE

AMOUNT S OF PYR I TE
Obtain two 4 inch ro a stin g di shes with covers
_
-
Lin e each .

dish thoroughly by rubbi n g a b l ackboard crayon over it s in t erior .

Wei g h out A T of S amp l e

. . i n to each dish Place .

the dishes covered in the muffl e which should be heated to low

, , ,

redness o n ly around th e edges and cor n ers The ma t e r ial to be .

ro as ted S hou l d be spread out in the roastin g dishes a n d ridged

across so as to expose as much surface as possible to the air
,
.

After one ha l f hour take out the roasts l etting them coo l a
-
, ,

little before removin g the covers ; then turn the ore over wi th
$

a w i re pro v ided for the purp ose leavin g i t sp read about and
,

[ 30 ]
ridged ,
be f ore
as Re turn the dishes without covers to the
.
, ,

m u ffi e i f the heat is s t il l low

,
After one ha l f hour take out and
.
-

stir again C o n tinue t his treatment gradua l ly i n creas in g the

.
,

heat til l no odor of sulphur dioxide i s p erc e ived on stirri n g

, .

Fin ally increas e the heat to a brigh t red for about t en minutes
, ,

to d ecompose a n y i ron su l pha t e which may h ave f ormed .

S melt the roa sted concentra t e with this char g e :

cr u cib l e .

After the concentrates have been trans f erred to t he crucib l e ,

” $
the ro as ti n g dish S hou l d be dry w ashed out w ith a litt l e soda
-
,

w hich i s added to the ch a rge .

Comp are resu lt s with t hose obtained f rom the ni t re assay .

A SS I GNME N T 17

A S S AY OF S ULP H ID E ORE S B Y THE NAIL M E T H OD

The nail method is adapted to gold or es conta i n i ng vary
$ ”

ing amou n ts of sulphid e s althou gh it may with certai n m o d ifi

,

cations b e app l ied t o a ll gold ores Ores containing appreciable .

amounts o f arsenic a n d an t imony can not be as sayed by this

method with this ex ceptio n : arsen i c f requently occurs in van ner
concentrates and m
,

a y then be removed in the firs t stag e s of the

assay by oxid a t iOn with nitre p a rt o f the sulphur being ,

oxidized at the Same time .

In gen e ral gold va l ues w ill be hi gher by this method and

,

S ilver v alues lower

[ 31 ]
 Prepare charg e s of S ample as follows :

Or e A T . .

L ith a r g e 30 g ra m s
Fl o u r gr a m s
S od a 45 g r a m s

S a l t or bor a x c o v e r .

T h r e e t w e n t y p e n n y n a il s
-
.

U s e a No F cr u c ib l e
. .

Add a w e ighed amount o f test silver ea c h charge

'

to

S ti ck t h e ails i n to the charge after the borax cover h as b e en

n

added poi n ts dow n

, S hould th e n ails first added be eat e n up
.

by th e ch arg e b efore fusi o n is fin ished tak e out what r emains ,

of t h e old o n es a n d a d d two or three fresh ones .

First fuse t h e ch arges in the usu al way ; when foaming has

‘

ceas ed give a very bri ght yellow heat for t en or fifteen minutes
, ,

conti n ui n g t h e h eati n g u n til on r emovi n g t h e nails and rinsing

,

them in the slag th e y are seen to be free f rom adheri n g globules

,

of lead .

Prepar e on e ch arg e of S ample as directed for S ampl e

except add 5 grams 8 1 0 an d a d d no test si lver .

Prepare two ch arg e s of S ample as f o l lows :

Or e A T . .

L ith a r g e$ 25 gr a m s
S od a 45 gr a m s
B or a x gl a s s 10 gr a m s
S il ic a 15 gr a m s
F iv e tw e n t y p e n n y n a il s
-
.

S a l t or b or a x c o v e r
U s e a N O F c r u c ib l e
.

Make the fusion as instructe d before .

When arse n i c is prese n t it is w ell to omit t h e nails add 1 0

to 2 0 grams of nitr e and boil dowp t h e ch arge ; the n add t h e
$

nails a n d fin ish at a hi gh heat as usual .

[ 32 ]
 CHA P T E R I V

B U L L I ON A S S A Y S

B u ll ion in genera l is c l ass ifi e d follows

f
,
as

1 Lead bullion usua l ly the product of the lead blas t furn ace ;
.
,
-

95 per ce n t an d more lead containing some copper antimony , , ,

et c .
,
S i l ver and gold .

B ase bullion containin g from 1 0 0 to 92 5 parts of S i l ver

2 .
,

per 1 000 gold in varyin g amounts and a large percent age of

, ,

b a se metals chi e fl y copper zinc lead etc

,
Produced most , , ,
.

frequently by cyanide mil ls .

D oré bullion containing 92 5 to 990 parts of silver p er

3 .
,

1 0 00 some gold and bas e metals mostly copper but also l ead
, , , , ,

antimony zinc e t c , ,
.

Fine si l ver bulli on f ree f rom gold containing 990 to

4 .
, ,
1 00 0
p arts S i l ver p er 1 0 0 0 but some b a se m e t als usually copper
, ,
.

5 . S ilver
bulli o n contai n ing little base metal ,
an d l ess than
h a l f its w ei ght in gold .

Go l d bul l ion contai n i n g little base meta l and more than

6 .
,

half i ts wei ght in gold .

7 . Fine go l d bullion free from S i l ver containing from , ,

990 to
1 000 p arts g o l d p er 1 00 0 .

Y ou ha v e had p racti ce in assayin g lead bu l lion ( see A ssign

ment Gold bullio n and fine gold bullion may be con sid e red
under a genera l case ; likewise base bullion doré bullion fine , ,

silver bu l lion and silver bullion ,

it F u l t o n : Ma n u a l of A ss a y in g .

[ ]
3 4
 A SS I GNME N T 19

A S S AY OF GOLD B ULL I ON

The bu ll ion tha t you are t o as say in this assignmen t is made

to represen t as c l ose l y as possib l e that which comes f rom C a l i
f or n ia mines .

Th e P r el i min a r y —
t his cl as s o f bullion an exper t ea n te ll
In
with su fficien t exac t ness t he fineness o f a p arti cul ar samp l e and
so can all oy in the p rop ort ion o f to 1 w ithou t makin g a ,

pre l iminary surv ey O rdin ari l y the b as e me t a l fin eness is no t

.

taken into accoun t a sma ll amount Of copper bein g added to the

,

proo f cen t er t o pre v ent sprou tin g and t o t oughen the bead ,
.

B ut f or the g enera l c a se and f or comp l eteness a p re l iminary

, ,
,
,

as say must be m a de in order t o d e t ermin e the approxima t e fin e

ness o f g o l d si l ver and bas e
,
.

Wei gh ou t 90— 1 00 m gs o f t he bu l lion gi v en you ; a lso 300 mg s

. .

o f test si l ver ; wrap si l ver and bu ll ion t ogether in 3 grams o f

S heet lead ,
and cupe l at a l itt l e above the f eatherin g point .

B righten w e l l ; cle an and p ar t the bead

,
.

Repor t t he resu l ts accordi ng to t he f ol l oWin g examp l e

B u l l io n t a k en
T e s t s il v e r

B u l l io n a n d t e s t s il v e r
C u p el l e d b e a d

Ba s e m etal
Go l d ( b y p a r t i n g )
S il ver ( b y d iffer en c e )

These resu l ts hould be corrected by addin g

S points t o 1 5— 2 0
the S ilver fineness and substracti n g the same amount from the
b a se me t a l finen ess This is to al l o w for S i l ver lost during
.

cup ell ation

[ 35 ]
 H avi n g d e termi n ed the app roximate fineness of the bulli on
given you weigh out two samples of 50 0 mgs each ( withi n
, .

.05 also weigh out test S ilver ( withi n 1 0 mgs ) so that . .

the ratio o f silver to gold will be to 1

Make a proof center of pure gold si l ver an d copper to
correspo n d with the regul ar samples .

Wrap e ach sample in 6 grams of sh eet lead or a s many as ,

the followi n g table calls for For bullion co n taining over 900 .

poi n ts of preci ous m e tal 5 grams of l e ad are su ffi ci en t to remove

all the ba s e metal The followin g tabl e is valuable for d et e r m in
.
f

in g the least amou n t of lead to use

P e i o s Me t l i n A llo y
r c u a

900
8 00
7 00
60 0
5 00

B efore i n troduci n g the samples into the muffl e

C u p el l a t io n —
,

have the t emperatur e at a bright red ( hi gh e r tha n for o r d in a r v

cupellation ) and the cupels whi ch S hould be smooth ho t
, , ,
.

Place the l e ad p ackets in thei r respective cupels the proo f ,

in the center a n d the n close t h e muffl e door

,
As soon as they .

uncover op en the door and allow the cup ellation to proceed in

,

the usual manner .

Take care that no metal is sticki n g to the S ides of the cupe l s .

B righten the cupels at a bri ght red heat cover w ith hot cupels ,

and remove gradually from the muffl e C lean carefu l ly and .

wei gh .

Now hammer the beads i n to the shape of a recta n gular bar ,

then roll out to the thi cknes s Of an ordi n ary visiti n g card by
mea n s o f the rolls ; or in the abse n ce of rolls h ammeri n g wil l do ,
.

I n rolli n g an n eal the alloy Whenev e r it becomes hard a n d elasti c

,

Mit c h el l : Ma n u a l o f A s sa y in g , p . 61 0 .

[ 3 6]
and before it begi n s to g et rough on the edges T h e three b e ads .

S hould be of the same thick n ess aft e r rolli n g Great care S hould .

b e taken to prev en t mechani cal loss .

P a r t in g
Cl e an thoroughly th ree matrass fl as ks P l ace 2 ozs
—
‘

. . .

of sp gr ni tri c aci d in each ; n e w i ntroduce the fl att e ned

. .

a n d annealed b e ads first rolling them into a spiral coil and

, ,

heat to boili n g .

B oi l g ently u n til acti on ceases ( ten to fifteen minutes ) then ,

p our off th e spe n t acid a n d add 2 ozs of stron g aci d sp . .

B oil gent l y with this aci d for fifteen to twen ty minutes .

Place a pi ece Of ch arcoal or burnt br i ck in each fl ask to p reve n t

bumping Po u r off this acid and wash the go l d three times in
.

hot water Transfer to ann e al in g cups and annea l

. .

W eigh the gold carefully ; and record the results according

to the following example

S a mp l e A Proo f en t e
c r Sa ml e
p B

mg . mg .

mg .

mg . mg . mg .

7 5 mg .

6 g ra m s 6 gr a m s 6 gr a ms
S il ver mg . mg . mg .

mg . mg . mg .

Cu p e l l a t io n l OS S '
mg .

P roo f c en te r l oss
mg . mg .

mg . mg . mg .

mg .

S u rc h a rg e

C orr e ct e d g o l d
Ba s e m et a l
S il v e r ( b y d iff e r e n c e )
S il v e r fi n e n e s s
B a s e m e t a l fi n en es s
Go l d fi n en ess

[ 37 ]
 Rema r ks —
Gold results should agree within 14 poi n t S ilver .

resu l ts w ill dep e n d on the care used in cup ellation as will the ,
.

b a se metal fineness S urcharge is the differe n ce between gold

.

los t durin g cupellation and partin g ( gold may be los t by

volatilization cupel absorptio n or so l ution in the acid ) a n d the
, ,

amount of silve r retain e d in the p ar t e d It is ge n erally positive . .

A n egative surcharge is to be regard e d with suspi cion .

In order to get p recise results it is n ecessary to have pure

gold for the proof ; p arted gold from previous as says will do but -
,
-

then an arbitrary surcharge will have to be used say 14 to 1 ,

poin t .

When rolls canno t be obtained the gold bu ll ion assay may ,

be made as follows :

1 . Make a preliminary assay as usua l .

2 Wei gh out 2 50 mgs o f bullion instead of

. .
,
500 mgs .
,
and
a d d sufficient test S ilver to make the p r Op o r t ion 3 to 1 . Make
up t he proo f in the usua l way .

A ft er wei ghing the cup e l led bea ds hammer un t il fl a t anneal ,

and p art usi n g aci d of

,
s p gr B oi l for five mi n u t es decant . .
, ,

w as h three tim e s annea l a n d weigh

,
.

This method has the advantag e o f bein g much more rapid

tha n the f ormer and at the same time i f care fully done is , ,

su fficiently acc u ra t e

RE FE RE N CE S

Ros e : Met a l l u r g y
f opp 4 6 2 Go l d ,
—4 9 2 .

A a ro n : A s s a y in g p a r t 2 pp 3 0—4 7
, ,
. .

”
P a ck : A s s a y in g o f Go l d a n d S il v e r in t h e U S Min t
$
Min ,
. and

S ci P r es s No v 1 4 1 9 0 3
.
,
.
,
.

”
W h it e h e a d U l ke : T h e S a mp ling a n d A s sa y in g o f Gol d B u ll io n ’
,
Th e
E n g in eer in g a n d Min in g $ ou r n a l F eb 1 2 1 8 9 8 , .
,
.

[ 38 ]
 A SS I GN ME N T 20

F IRE A S S AY OF S ILVE R B ULLION

Mak e an ass ay of the sample of S ilver bullion obtained in
Assign ment 2 2 f ol lowin g the directions given in F u lton s Ma n u a l
,
’

of A ss a y i n g .

Record resu l ts according to the following example

P RE L I MI N AR Y A S S AY

B u l l io n 500 mg .

L ea d 1 0 grm .

Cu p e l l e d b e a d mg .

P a r t e d go l d n on e

S il v e r t o b e u s e d in proo f 44 5—4 5 0 mg .

Go l d t o b e u s e d in proo f n on e

C opp e r t o b e u s e d in proo f 5 0—5 5 m g .

F I N AL A S S AY
le A
S a mp Proo f
B u l l io n 5 00 m g
S il v e r mg .

G o l d in proo f n on e
C opp e r in proo f 5 2 mg .

L ea d grm . gr m . grm .

Go l d a n d S il v e r in mg .

C u p el l e d b e a d mg . mg . mg .

C u p e l l a t io n l o s s mg .

P roo f c en t er l oss
Ba s e m eta l
P a rt e d g ol d n on e
B a s e m et a l fin en e ss
Go l d fi n e n e s s
S il v er fi n en e ss

1 0 00 1 0 00

Use the utmost care in cupelli n g D o not neg l ect to cove r .

the cupels with h ot cupels when the beads h ave brightened ; a

bead that h as sprouted must b e discarded and the entire assay
'

r 6 p ea t e d
RE F E R E N CE S
F u l t o n : Ma n u a l o f A s sa yin g pp 1 75— 1 7 7
,
. .

F u rm a n : Ma n u a l o f A ssa y in g pp 2 7 6— 2 8 0
,
. .

[ 39 ]
 CH A P TE R V
M I S CE L L A N E OU S W OR $
A SS I GN ME N T 21

F URNAC E RE PAIR S . MA $ ING CUPE L S

1 .You are assi gned to a p articular furnace and you a r e ,

e xpected to ke e p it in repair Exami ne it carefully ; especi ally s e e

.

that the mu ffl e is in g oo d c on d it ion If it is not remove it a n d .

,

put in a n e w on e The followi n g poi n ts sh ould b e considered in

.

placing a n ew muffl e : H ave the mu ffl e well supp orted in the back

a n d front give it a S light i n cli n ati o n downwards toward the
,

front an d hav e the c e m en ti n g mat e rial of t h e ri ght consiste n cy

, .

Fi re —clay with a certai n proporti on of sa n d or b r oken tire bri ck -

is the cem en ti n g materi al us e d .

Mak e up t h e cement in t h e following man n er : Take fi r e clay -

a n d fi r e brick in t h e proportio n o f on e to three

-
C rush the fi r e .

brick to p as s a n e i ght or t en m e sh scre en Mix the two dry and .

then add wat e r u n ti l the whol e is in a plasti c conditio n Moisten .

thoroughly th e b ri ck work a n d thos e porti ons of the muffle that

-

come in co n tact with t h e clay then press the clay in firm l y a n d

,

allow to dry at l e as t tw enty four h ours -

.

Make a drawi n g ( pla n and s e ctions ) of your furnace to s cale , .

2 Mak e 2 00 good cup els a s follows

.
,

Take the box us e d for th e purpose a n d fill with bone —ash ,

add water and mix Use as ma n y ou n c e s of water as pounds of

.

bone ash The right amou n t of water h as b ee n added wh en the

-
.

bon e ash loses it s h a rsh gritty fe e li n g a n d at the same tim e is

-

, ,

not pasty A small amou n t of potassium carbo n a te ( 2 per cent

$

solutio n ) m
.

a y be add e d to as s ist in ceme n ting the b on e ash but -

,

this is not nec essary Wh en the bon e ash is thoroughly mixed

.
-

a n d is of t h e ri ght co n siste n cy S i ft through a twenty mes h si eve

,

a n d the n place a su ffici en t amou n t in the mould and hammer ,

dow n firmly ; two hard blo w s a r e en ough ; do n ot use a n ythi n g

but th e wo od en mallet i n striki n g the mould Place your cupels .

on a board a n d set away to dry .

[ 40 ]
 A SS I GNME NT 23

C OMPARI S ON OF M E T H OD S F OR A S S AY OF C OPP E R
ORE S AND C OPPE R—B E ARING MATE RIAL S
S c or ific a t iThe standard charge f or the assay of C opp er
o n .
—

or es and copper bearin g materi al by the s c o r ifi c a t ion meth od is

as f o ll o ws
Or e A T to A T . . .

Gra n u l a t e d l e a d 5 0 g r a m s
B or a x gl a s s 1 g ra m
S il ic a 1 gr a m

Us e 3 in . s c o r ifi e r s .

'

Re -
scorify l ead buttons us ing /2 inch sc o r ifi e r s and enough
,
2 1

test l ead to m ake total wei ght of l e ad not l ess than 35 grams .

Wh e n the ore or copper bearin g materi al is poor in copper the

-

si l i ca a n d r e s c or ifi c a t ion may be omitted As many assay s may

-
.

be run as are necessary to give accurate res ults

Cupe l an d slag correcti ons either or both are sometimes , ,

requi red a n d may be made as fo l lows :

The cup els are taken in lots of two each the unused portion ,

discarded the remainder crushed to p ass 1 00 mesh and fused

, ,

with 1 00 grams o f l itharg e 2 0 grams sodium carbonate 40 gra ms

, ,

borax glass a n d 3 grams of argo l

,
.

The slag is merely groun d to pass 1 00 mesh and fuse d with ,

the addition of sa y 40 grams o f litharge 2 0 grams Of sodium

, , ,

carbon ate an d 3 grams o f argo l .

In both cases the res ulting l ead but t ons are cupelled and
the si l ver and gold obtained add e d to the first wei ghts
r i
C uc b e l — A st andard method f or the ass ay of the abo v e by
the crucible method i s as f ollo w s :
Or e 730 t o A T
1

L it h a rg e 8 0 gr a m s
S il ic a 1 2 gr a m s
S od C a rb . . 1 6 gr a m s
B or a x g l a s s 1 2 gr a m s

R e d u c e r or o x id iz e r f or a 2 0 g r a m b u t t o n

U s e a No F c r u c ib l e
. .

[ 42 ]
 For ores or ot h er material containi n g less than 40 per cent
copper the amou n t used for a ssay may be increased up to 1A; A T
, . .

S ome or al l o f the S ilica may b e omitted .

Prep are ei ght ch arges o f S ample a cop per matte

ri ch in copper according to the methods already outlined , f our
,

by s c or ifi c a t ion and four by crucible fusion Use proper p re .

cautions in meltin g and cupel l a t ion .

Make a tabular report showi ng comp arative losses etc

, ,
.

A S S I GN ME N T 24

PRAC TI C E I N S AMPLING PANNING ,

A ND

AMAL GAMATING
i

sample o f ore given you ; Wei gh and

$

S a mp l in g — T a k e gt h e
‘

then reduce in size ( wei ght and m esh ) b y a p p r ov e d metho ds .

Your as say samp l e S h ould weigh at l east lb and S hou l d p ass

$

a t l eas t a 1 0 0 mesh screen

-
T ake car e th at a l l scale s p as s t he
. ,

screens used .

Reserv e al l discarded ore p a ssing th e 40 mes h screen and keep -

f or the pannin g and a ma l gamatin g experimen t s .

A ma l g a m a t in g fiW ei gh ou t five ch ar g es ( 1 00 grams each )

f—

o f the 40 mesh lot and place I n b ot t l es p r ovid e d f or th e pu rp ose

'

-
,
.

with mercu ry ( 1 0 grams ) and 1 50 c c o f w ater ; an d ag ita t e f or

,
.

thir t y minutes S ep arat e the mercury by p annin g ( see below )

.

a n d transf e r to a porcelain dish dry with filter or blo ttin g p aper

,
.

P l ace t he thoroughly dry mercury in a 2 0 gram or F crucible

in w hi ch 2 0 grams o f l ead have been placed Add t othe crucibl e .

a char g e con sistin g o f 3 0 gr ams o f litharge 1 0 grams of s oda , ,

5 grams o f b orax gla ss and grams of argol and silver e nough

, ,

to part t h e go l d .

Fuse the ch arge very slowly starti n g with a slow fire in the ,

wind furn ace or i f usin g a muffle one th at h as no t ye t become ,

A m od ific a t io n o f F u l t o n ’
s m e t h od .

[ 4 3]
red and has a go od draught through it to preve n t the escape .

o f fumes into the room When fusio n i s qui et pour and cupe l
.
,

the resultin g l ead button Part a n d wei gh the gold . .

P a n n in g —
The conten t s o f the bottles are to be panned
sep arately and then together Pour the contents of one bottle .

i n to a gold pan add water i f necessary and was h by givi ng the

, ,

pan a vibratory motion as in v anning washin g off the light ,

particles of gan gue an d lea v ing on l y the mercury and the heavy
portion o f the ore as black s an d sulphides et c
,
The li ght , ,
.

portion o f the ore S hou l d be washed int o a p an or vesse l o f

somewhat larger size than the gold p a n Repeat the pa n nin g of .

the mercury a n d co n centrates in order to separate the mercury

’

If the mercury i s fl oured add a small globule of l i quid sodium,

amalgam .

Treat the contents o f the other bottles in the same way T he .

light portion or tailings o f the severa l bottles may be p oured

i n to the same v esse l Re p an this material to make sure that
.
-

n o mercury or sulphides have e scaped I f a n y is recovered add .

,

to the amou nt recovered be f ore .

Treat the collected mercury as di rected above ( see amalga

mating ) .

Al l ow the tailings to settle p our OR the surplus water an d , ,

dry by any conveni ent means When dry weigh p as s th rough .

, ,

a 1 00 mesh screen mix wel l and a ssay

-
,
.

W as h th e heav y materi a l or con cen t rates into a small por

c el a in p an or if more convenient on to a batea
,
Examine under .

a magnifyin g glass or low p ower mi croscope and note t he ,

d ifi e r en t kinds Of sulphid e s or other constituent an d the a p p r oxi ,

mate amoun t o f each .

D ry weigh crush to p ass a

, ,
1 00 -
mes h screen ,
an d as say
From your r e sults calculate the fol l owing
1 . Assay v alue of ore in oun ces and do l lars and cents p er ,
t en .

2 . Gold amalgamated in ounces ,

an d dollars and c e nts per t en .

3 .Assay v alue of concentrates in ounces and dollars and ,

c en ts p er ton .

[ 44 ]
 4 Assay v alue of tailings in ounces and dollars and cents , p er

5 . Percentage of go l d amalgamated .

6 T otal gold contents in com parison with assay va lue

.

1 . Percentage and di ff erent ki n ds of sulphides or other h ea vv

ma t e r ia l

RE F E RE N CE S

F u l t o n : Ma n u a l of A ssay in g pp 36—4 l a n d 1 54—1 5 6 , . .

F u rm a n : Ma n u a l o f A ssa y in g c h a p 2 , . .

B ro w n : Ma n u a l o f A ss a y in g pp 1 8 5— 1 94 , . .

H er sa m : P r in c ip l e s in t h e P r a c t ic e o f S a mp l i n g ” Min
$
, . a nd

W o r l d No v 2 5 1 9 1 1
'

.
, , .

B r u n t o n : Mod e r n P r a c t ic e in Or e S a mp l in g T r a n s A m
$
, . . I ns t . Min .

E ng vol 4 0 p 5 67
, .
,
.

H o f m a n : T h e Me t a l l u r g y o f L e a d c h a p t e r V , .

A SS I GNME NT 25

FIRE A S S A Y OF L E AD OR E S

Lead as says are usu al ly made in th e muffl e ; bu t in t he absence ,

o f such a wind furnace may b e used

,
The mu ffle i s to be ,
.

p re f erred because the hea t can be more uniform l y con t ro l led ,

and there is l ess danger of l oss by volati l ization .

Al l our lead assays wi ll be made in the mu ffle furnace .

The fire ass ays of lead ores may be placed under three heads ,

accordin g to t he kind and proportion o f fl u x used

1 . Fusion with sodium bic arbo n ate borax ar g o l and iron , , ,
.

2 Fusion w ith mixture o f sodium bi carbonate and p otas sium

.

carbonate borax argol and iron

, , ,
.

3 . Fusion w ith p otassium cyan ide .

S a mp l e Pure assayers lithar g e .

[ 5]
4
 Prep ar e three charges as follows
Or e 1 0 gr a m s
L ea d fl u x 35 gr a m s
Sa l t c over
Us e B a tt e r s e a P cr u c ib l e s

Manage heats as directed be l ow ; p our into s c or ifi c at ion

moulds .

C lean buttons by brushing a n d hammerin g . Wei gh on pu l p

ba l ance to 0 1 gram Report to 1 0 per cen t
. . . .

S a mp l e Pure Galen a .

Prep are three charges as b e fore with the addition o f four ,

nails to each crucible and five grams of borax glas s on t Op of

,

each charge be f ore salt cover .

Assay S amp l e in the same manner

Your res ults should check to within . 5 per cent . Write your
notes care fu l ly .

The lead fl u x is a mixture of sodium bic arbonate ( 1 2 parts )

potass ium carbonate ( 1 2 parts ) argol ( 3 p arts ) , .

The first method should b e us e d o n ly whe n potassium car

bon ate ca n n ot be procured The third shoul d be us e d only on
.

pure ores The seco n d is preferable in all cases

.

H ea ts The f usions are b est man aged by giving a l ow h e at

—

for a b out twenty mi n utes a n d then a high heat to finish This .

is necessary for two reasons : ( 1 ) Lead and its compounds are

volatile ; and i f the heat is so high that boi l in g takes place
violently some lead is almost certain to be lost ( 2 ) Lead forms .

a doub l e sulphide with sodium; a n d to reduce this by mea n s of

,

iron a hi gh heat is necessary

,
.

Th e nails should not be remo v ed unti l entirely free f rom lead .

Fusion w ith cyanide requires a very l ow heat .

RE F E RE N CE S
H o f m a n : T h e Me t a l l u r g y o f L ea d ,
ch a p t er V .

F u t o : Ma u a l of A s y g
l n n sa in ,
pp 1.99 —2 01 .

[ 6]
4
T HI S B O O$ I S DU E ON T H E L A S T D A TE

AN I N IT IAL F I N E O F C E NTS
W I L L B E A S S E S S E D F O R F A I L U R E T O R ET U R N
TH I S B O O $ O N T H E D AT E D U E T H E P E N A L TY
.

W I L L I N C R E A S E T O s o C E N TS O N T H E F O U R TH
DA Y A N D TO ON THE S E V E N TH DA Y
O V E RD U E .

SEP 1 4 1 9383 VI 7 1975

S E? 1 5 1 932

950 1 0 1 9
33

UN1 7 1976
4

L D 2 1 —2 0 m