UC-NRLF

121

fllS

/BERKELEY

LIBRARY
I

UNIVERSITY OF

\CALIFORNIA
EARTH

Geology

THE ELEMENTS OF BLOWPIPE

ANALYSIS

THE

ELEMENTS

OF

BLOWPIPE

ANALYSIS

BY

FREDERICK HUTTON GETMAN,

F.C.S.

INSTRUCTOR IN CHEMISTRY IN THE STAMFORD HIGH SCHOOL

godt

THE MACMILLAN COMPANY

LONDON MACMILLAN &
:

CO., LTD.

1899
All rights reserved

BY

THE MACMILLAN COMPANY.

Nortoonfi
J. 8.

Gushing

& Co. - Berwick Sc Smith

Norwood Mass. U.S.A.

PREFACE
THESE few pages
a
are intended
to
of

to serve

twofold purpose,
general
outline

give

the

student
Analysis,
of

Blowpipe
to

and to introduce him

the

methods

Determinative Mineralogy.

Every

effort

has been
the

made

to simplify in

details so

that

book may be used

"

both High Schools and Colleges.

Tables for

"

systematic

examination have

been intentionally omitted, for in the author's

estimation

these

tend

to

dull to

the

student's

power
little

of observation,

and

make

him place

value upon minute details.

The

alphabetic

arrangement

has

been

followed for the sake of convenience

referring to the book.

when

819488

Vi

PREFACE

The

last

chapter

is

not intended to serve

as a key to determining the minerals therein

described, but

rather

it

is

added

to

give

the student exercise in Blowpipe Analysis,

and

at

the

same time

to

point

out

the

methods of Determinative Mineralogy.

Finally, the author

would acknowledge
"
:

his

indebtedness to the following works

ual
of

Man-

Qualitative

Analysis,"

Fresenius;

"Qualitative

Chemical Analysis," Venable;

Schorlemmer's
"

Roscoe and
Chemistry";
eralogy";

"

Treatise
of

on

Foye's

Hand- Book

Min-

Dana's "Mineralogy";

Kobell's

"Tafeln zur Bestimmung der Mineralien";

etc.

FREDERICK HUTTON GETMAN.

STAMFORD, CONN.,
Feb. 22, 1899.

TABLE OF CONTENTS
CHAPTER
Apparatus and Reagents
I

PAGE

1-7

CHAPTER
General Outline of Blowpipe Analysis
Definitions

II

8 9
10
.

Examination on Charcoal Alone

Examination on Charcoal with Sodium Carbonate
.

13
.

Examination in Tube with Sodium Carbonate and Charcoal

15

Examination on Platinum Wire Examination in Borax Bead Examination with Cobalt Nitrate

16
17

20

CHAPTER

III

General Reactions for the Detection of the Metallic Ele-

ments in Simple Compounds

22
23

Aluminum
Antimony
Arsenic
'

24
25
-

Bismuth

25

Cadmium
Chromium
Cobalt

26

..........
vii

26
27

viii

CONTENTS
PAGE

Copper
Iron

28
28 29

Lead
Manganese
Mercury
Nickel
Silver

30

30
31

32 32
33

Tin
Zinc

The

Alkali Metals

34

Ammonium
Potassium

34
35

Sodium
Lithium

35

36
36 36
37 37
37

The Alkaline Earths

Barium
Calcium
Strontium

The Acid Elements

Borates

37

Bromides
Chlorides
Fluorides

38

38
38 39 39

Iodides
Nitrates

Phosphates
Silicates
.
.

40
.

Sulphides

.40 .41

CONTENTS
CHAPTER
Behavior of

IX

IV
PAGE

Some

of the Principal Ores before the Blowpipe

'..

43

Ores of Antimony
"*

.
.

46

Ores of Arsenic
Ores of Bismuth Ores of Chromium

-47
.

48
49
50

Ores of Cobalt Ores of Copper

Ores of Iron
,
,

52
57

Ores of Lead
Ores of Manganese

60
63

Ores of Mercury

64
65

Ores of Nickel
Ores of Silver

66
i .
.

Ores of Tin

69 70

Ores of Zinc

COMPARATIVE TABLES
I.

Colors of Coatings on Charcoal

73

II.

Flame Colorations

'

III.

Colors of Borax Beads in oxidizing

Flame

IV.

Colors of Borax Beads in reducing Flame

... ...
.

73

74
75

V.
VI.

Colors of Microcosmic Salt Beads in oxidizing Flame

Colors of Microcosmic Salt Beads in reducing

76
77

Flame

FORCEPS
Fig. 5

AGATE MORTAR & PESTLE

Fig.

HAMMER
Fig,
6,

-CORNERED
Fig, 7

FIJ_ES

BLOWPIPE ANALYSIS
CHAPTER
THE
blowpipe was
first
I

applied to mineral
its

analysis in

1733 by Anton Swab, and

applications have since been improved and

extended by various chemists,

among whom
Cronstedt,

may be mentioned Bergmann,

Gahn,
Berzelius,

and Plattner.

Blowpipe.
jeweller
is

The common blowpipe

of the to

not particularly well suited

analysis,

the operations of blowpipe the

since

flame has

often
for

to

be

kept
time,

playing

upon the assay

some
of

and the
would

condensed moisture

the

breath

seriously interfere with the passage of the

BLOWPIPE ANALYSIS
air

through the

jet.

One

of

the best and

is

least expensive
in

forms of blowpipe
consists, as
is

shown

Fig.

i.

This

seen from

the illustration, of a conical-shaped tube of

tin closed at the

wide end and formed into

soldered

a mouthpiece at the small end;

into

the

tube

at
its

the

large
is

end,

and

at

right

angles to

axis,

a small

brass
tip

tube

which

terminates

in

conical

pierced with a very fine hole.

With
all

this

pipe

it

is

possible

to

perform

of

the

operations of mineral analysis.

Some

little

practice

is

necessary to keep

the flame steady and to take the breath at

the

same

time.

No
ner,

rule can well be given to the begin-

but his experience becomes his best

guide.

Bunsen Flame.

Any

kind of flame can

it

be used for the blowpipe, provided

be

BUNSEN FLAME
not too small
ratory to-day
;

but since almost every labofurnished with gas and the

(Fig.
2),

is

Bunsen burner

it

will

only

be

necessary to describe the use of the flame

from

this

source.

Upon examining
care,
it

the

Bunsen flame with

will

be seen that

the flame consists of three distinct parts.

A
yond

dark inner cone which consists

of gas

not yet raised to the ignition point.

this there is a
is

Be-

luminous cone, where

combustion

incomplete owing to lack of

outside of
this

oxygen, and

we

find
is

the

non-luminous cone where the gas

pletely burned.

com-

This outer envelope

tion
"

is

the hottest poris

of

the
"

flame,

and

known
is

as

the

oxidizing
of

flame because there

is

an excess

oxygen which

imparted to substances

placed therein.

The luminous cone

"reducing" flame, for
in

is
it

known

as

the

metallic oxides

4
are

BLOWPIPE ANALYSIS
reduced, the oxygen

being taken
particles of

up
car-

by the small incandescent

bon.
If

the air-holes at the base of the Bun-

sen burner be opened, the two inner cones

become elongated, and the flame appears

almost colorless.

The blowpipe

enables us to get an oxidiz-

ing and a reducing flame of better form

and greater power.

the air supply at

To do

this

we
the

cut off

the base of

burner
is

and turn
about
the
i

off

the

gas until

the

flame

cm. high; then upon introducing

a

blowpipe, and blowing

strong con-

tinuous jet of air across the Bunsen flame,

we produce an
cm. in length.

oxidizing
If

flame about 4-5

the tip of the blowpipe

be held outside of the Bunsen flame, and

the pressure of the stream of air be diminished,

we

obtain a reducing flame.

BUNSEN FLAME
Supports.

For supports, charcoal,

glass

plati-

num, and

are

chiefly

used.

The
light

charcoal should be

made from some

It

wood, such as

alder.

should be well

burnt, and should not scintillate or smoke.

The platinum
are

supports are generally in

foil.

the form of wire and

forceps

Platinum-tipped
in

frequently employed

blow-

pipe analysis.

Glass

is

used in the form of tubing.

Hard
off

glass tubing, 3

mm.

bore,

is

drawn
length.

into ignition tubes 7-8 cm. in

Several

dozen

of

these

tubes

should
tests

be
the

made

before

commencing the

of

next chapter.

Apparatus.

small agate mortar, 4-5

cm.

in

diameter,
to

should

be

provided

in

which
ined.

grind the samples to be exam-

The

pestle,

which should also be

of agate,

BLOWPIPE ANALYSIS
to

must be adapted
and
size.

the mortar in shape

Two
One

pairs of forceps will also be needed.

pair should be of steel,

and the other

pair of brass, with fine points.

Of other apparatus, the most necessary

is:

small

hammer and

anvil.

Two
cm.

three-cornered

files.

Small piece of cobalt

glass,

about

x 10

Pocket magnifying

lens.

Several small watch glasses

beads, etc.

for metallic

Chemicals.

list
:

of the principal chemi-

cals is here given

Sodium
Borax,

carbonate,
2
7

Na CO 3
2 2

Na B 4 O + ioH
salt,

O.
4 ), 4
2

Microcosmic

(HNaNH PO + 8 H

O.

BUNSEN FLAME
Cobalt nitrate,

Potassium

Co(NO 3 2 +5 cyanide, KCN.

)

O.

Hydrochloric acid,

(dilute),

HCl + nH

O.

Litmus paper, red and

Brazil-wood paper.

blue.

Any
needed

other special reagents which

will

may be

be mentioned as required.

CHAPTER

II

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

[ABBREVIATIONS
Ch.
:

O. F. for oxidizing flame, R. F. for reducing flame,

Bp. for blowpipe.]

for charcoal, Ct. for coating,

IN order to examine a substance before

the

blowpipe

to

determine

the
it

presence

or absence of certain elements,

becomes

necessary to arrange a systematic method.

As

with

all

branches
is

of

chemical work,

one's

success

largely

dependent

upon

neatness of manipulation and carefulness of

observation.

The

following

order of

observation
:

is

essentially that given

by Berzelius

1.

Examination on charcoal by

itself.

2.

Examination on charcoal with

8

Na CO 3
z

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

3.
2

Examination

in

ignition

tube

with

Na CO 8 and
4.
5.

charcoal.

Examination on platinum wire.

Examination
in borax bead.

6.

Examination with

Co(NO

3)2.

After having examined a body in these

six different ways,

we

shall

be able to say

what are

its

principal constituents.

Before describing the method of carrying

out these six different operations,
it

will

be

necessary to give a few definitions of terms

which we
employ.

shall

have frequent occasion to

Definitions.

Ignition

is

the heating of a

substance to a high temperature.

Fusion

is

the heating of a substance to

the melting-point.

Intumescence
stance

is

the swelling of

the sub-

upon heating.

10

BLOWPIPE ANALYSIS
Decrepitation
is

the crackling of a sub-

stance due

to

the

sudden

expansion

of

combined water upon heating.

Deflagration
stance
is

the

burning
violence,

of

sub-

with

explosive

generally

due

to excess of oxygen.
is

Incandescence

the white
is

light

emitted
sub-

by a substance that

infusible

when

jected to a high temperature.

Examination on Charcoal alone.

of

The

size

the

assay should

be about that of
is

mustard seed.

This

sufficiently large to

show

all of

the reactions clearly, and though

a larger piece would exhibit the characteristic

phenomena, yet much more

effort

is

required.

very small, shallow hole should

be cut in the Ch. to receive the assay.

The

Bp. flame should be directed at an angle of

about 30 with the surface of the Ch.

siderable care

Con-

must be taken

lest the hole in

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

the Ch.
is

II

burned too deep and the assay

lost in the coal.

The

force of

the air from the jet

must

also be borne in

mind

for a strong blast, or

sudden puffs may blow the substance away.

The
for:
a.

following changes are to be looked

Whether

the substance

is

volatile or

non-volatile.

Examine before the Bp. on Ch. some arsenious oxide, As 2 O 3 also some
Illustrations.
,

alumina, A1 2
b.

3.

Whether

the

substance

is

fusible or

infusible.

Illustrations.

Ch. some silver

oxide,

Examine before the Bp. on oxide, AgO, also some zinc

ZnO.
the substance
is

c.

Whether

alkaline or

non-alkaline

when placed upon moistened

red litmus.

12

BLOWPIPE ANALYSIS
Illustrations.

Ignite

some calcium

car-

bonate,

CaCO

3,

before the Bp. on Ch., and

place residue on moistened red litmus.

like

In
car-

manner, examine some magnesium

bonate,

MgCO

3.

d.

Color of
of

coating on

Ch. caused by

combination

metal and oxygen due to

heat of Bp. flame.

Illustrations.
lead,

Examine some oxide

Ch., also

of

PbO, before the Bp. on oxide of cadmium, CdO.

some

e.

Decrepitation.

Illustration.
ride,

Examine some sodium

chlo-

NaCl, before the Bp. on Ch.

f.

Deflagration.

Illustrations.
nitrate,

Examine some potassium

before the Bp. on Ch., also
nitrate,

KNO

3,

some ammonium

NH NO
4

3.

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

g.

13

Intumescence.

Illustration.

Examine some alum,

A1 2 (S0 4)4

:
,

before the Bp. on Ch.

h.

Incandescence.

Illustration.

Examine some

oxide

of

barium, BaO, before the Bp. on Ch.

i.

Formation
malleability.

of a

metallic bead

color

and

Illustration.

Examine some

silver oxide,

AgO,

before the Bp. on Ch.

Examination on Charcoal with Na 2 C0 3

Metallic

compounds

are

often

difficult

to

reduce with the blowpipe flame alone, and

hence no bead
facilitate

is

obtained.

In order to

reduction and the obtaining of a

bead,

metallic

the

substance
is

in

finely

powdered

condition

mixed

with

four

14

BLOWPIPE ANALYSIS
of

parts

sodium
before
the

carbonate,

Na CO3
2

and

ignited
tallic

Bp.

on Ch.

The me-

compound

is

decomposed, the metal

being transformed into the carbonate, which

in turn,

through the agency of the Ch. and

is

the
free

heat of the flame,

metal.
easier
its

reduced to the
reduction
the
is

Sometimes
by adding
of

the
to

made
about

substance

own bulk

potassium cyanide,
the

KCN,

which takes up oxygen from

is

compound and
cyanate,

converted into potassium

KCNO.
reactions
in

The
phate,

reducing copper
2

sul-

CuSO

4,

with

Na CO and
3

with
:

KCN

before the blowpipe, are here given

4
3 3 2

CuS0 + Na C0 = CuC0 + Na SO 2 CuCO + C = 3 CO + 2 Cu

2

CuSO 4 + Na CO = CuCO + Na SO
2 3

CuO + KCN = Cu + KCNO

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

After obtaining beads,
it

15

is

well to obtain
it

their coatings, for oftentimes

this

is

only in

way

that

we can

distinguish between

the metals.

Examination
Charcoal.
If

in

Tube

with

Na 2 C03
in

and

the

substance

finely

pulverized condition be mixed with twelve

parts,

Na CO
2

3,

and

six

parts

of

charcoal

powder and the mixture be placed in an ignition tube and subjected to heat, the
acid
of

the

substance combines with the

is

soda and the metal

If

set free.

this

metal

is

volatile,

a sublimate

is

formed

in the

upper end
in

of the tube.

Mercury

deposits

minute

globules,

which may be seen with the magnifying

glass.

Arsenic forms a ring, which, when

glass, is seen

examined with the magnifying

to

be

made up
is

of

minute

crystals.

Am-

monia

recognized

by

its

characteristic

BLOWPIPE ANALYSIS
and
also

odor,

by

its

turning

slip

of

moistened red litmus (held over the mouth

of the tube) blue.

Examination

on

Platinum

Wire.

Many
Bunsen

substances possess the property of impart-

ing to the colorless flame of the

burner characteristic colors.

The

chlorides of these substances exhibit

these flame reactions best, and hence before

applying the flame tests we dip the wire

which serves as a support into hydrochloric

acid and then
into the substance.

When

the substance has been

wire,
it

taken

up on the

is

placed in the edge of the long

the

colorless flame of

Bunsen burner near

becomes

the apex,

when

instantly the flame

tinged with the characteristic color of the

substance.
Illustrations.

Sodium compounds

color

the flame yellow, and a crystal of potas-

GENERAL OUTLINE OF BLOWPIPE ANAL YSIS

sium dichromate appears colorless
in

the

sodium

light.
is

This sodium reaction

cate,
it

extremely

deli-

being possible to detect with ease

of

quantity

sodium

salt

less

than

innnhnnr of a milligram in weight.

Potassium colors the flame purplish-violet.

Barium colors the flame apple-green.

Strontium colors the flame crimson.

Calcium colors the flame orange-red,

tinguished

dis-

from

strontium,

by

appearing

gray when seen through blue glass.

Boracic acid colors the flame green
the

when
with

substance

has

been

moistened

glycerine.

Examination

in

Borax

Bead.
salt,

Borax,

Na B 4 O
2

7,

and microcosmic
4
.

NaNH H P0

4,

possess the property of dissolving

many

of

18

BLOWPIPE ANALYSIS
metallic oxides at

the

the

temperature of

the Bunsen flame.

For example, with oxide

of

cobalt,

the

following reactions take place with the two

fluxes
:

CoO + Na B O = Co(BO + 2 NaBO

2

2) 2

2.

On

heating,

NaNH H.PO
4

4,

it

is

decom-

posed into the metaphosphate of sodium,

NaPO

8,

CoO + NaPO = CoNaPO 4

3

Now
tallic

in

such cases of solution the me-

oxides

impart a characteristic color

to the flux.

The platinum
it is

wire

is

the best support,

heated to incandescence in the Bunsen

flame,

and then

is

quickly dipped into the

borax,
this
is

when

a small globule will adhere,

to the flame

removed

again
glassy

when
bead.
it

the

borax melts to
is

clear

While the bead

still

melted, touch

to

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

the finely pulverized substance and replace

in

the flame.
of

In a few seconds the small

the

particles

substance will
will

have

dis-

solved,

and the bead

be seen to have

assumed the color

stance.

characteristic of the sub-

Note the color when hot and then

;

when
Then,

cold

often there

is

a wide difference.

too, the test

should be

made

in

both

O. F. and R. F.

Some

analysts

prefer

to

make

small

loop in the end of the wire before taking

up the borax

to

make

the

bead.

Care
is

should be taken to see that the bead

colorless before bringing
it

in contact with

the substance.

As

the depth of color produced

is

largely

dependent upon the amount of substance

taken,

some

little

caution should be exer-

cised to insure taking

up about the same

quantity each time.

Illustrations.

Make

several

beads, and

20

BLOWPIPE ANALYSIS

note the colors characteristic of the following oxides: cobalt, nickel, iron, manganese,

chromium, and copper.

The microcosmic

salt

bead dissolves
silica,
,

al-

most every oxide except

this
is

SiO 2 and

seen to float about in the melted

mass.

This

is

used as a

test for silica.

Examination with Co(N0 3 ) 2

If

after ex-

amination on the Ch. per

residue remains,
of
it

se,

a white infusible

is

moistened with a drop

3 )2

cobalt

nitrate

Co(NO

and

re-ignited

before the Bp.,

when

a change of color will

is

be observed.

This change in color

owing

to the fact that the heat of the

Bp. flame
nitric

decomposes the cobalt

being driven
off,

nitrate,

acid

and the remaining

oxide of
the

CoO
a

forming with
colored mass.
Illustrations.

the

residue

Ignite

before

the

Bp. on

Ch. the following oxides,

allow to cool,

GENERAL OUTLINE OF BLOWPIPE ANALYSIS

add a drop
color,

21

of

Co(NO

8)2 ,

re-ignite,

and note
zinc,

aluminum,

magnesium,

and

calcium.

Care should be taken to thoroughly ignite

before adding the cobalt nitrate solution.

With

the six methods of examination just

given almost every simple substance can be

detected, but

should any doubt remain, a

"

few simple

tests in the

"

liquid

way

will

be

sufficient to substantiate the

blowpipe exam-

ination.

CHAPTER

III

GENERAL REACTIONS FOR THE DETECTION OF THE METALLIC ELEMENTS IN SIMPLE COMPOUNDS

FOR
for

the sake of convenience, rather than

reasons,

scientific

the

following
in

com-

pounds have been arranged

order.

alphabetic

Also the oxides

of the

elements have

been taken, since they exhibit the reactions

to best advantage.

The
fully

student should work through care-

each one of the tests and satisfy himthe characteristic reactions of the

self as to

various elements, for only in this

he expect
presented

to recognize the

way can substances when

It
is

to

him

as

"

unknowns."

advisable to provide a note-book and rule

it

as follows

22

GENERAL REACTIONS
BEHAVIOR OF SUBSTANCE

24
dissolves

BLOWPIPE ANALYSIS
slowly,

forming a colorless glass

which remains so on cooling.

With Co(NO 3 ) 2
re-ignition.

Mass becomes blue upon

2.

Antimony, Sb 2
In

3.

Before the Bp. on

Ch.

O. F.
is

volatilizes

without change.

In R. F.

reduced and

volatilized.

White

coating of antimonious oxide deposited on

Ch.

Blue tinge imparted to flame.

the

Before

Bp.
'

on

Ch.

with

Na CO
2

3.

Readily reduced.
volatile,

White

brittle bead.

Very
coat-

giving

characteristic

white

ing.

In

ignition

tube with

Na CO 3 and
2

Ch.

Volatilized.

In flame on platinum wire.

Volatilized.

Colors flame greenish blue.

With borax bead on platinum

With Co(N0 3) 2

wire.

In

O. F. dissolves to a colorless glass.

GENERAL REACTIONS
3.

2$

Arsenic,
volatile.

As 2

3.

Before the Bp. on Ch.

Very

Strong garlic odor to fumes.

Bp. on

Before

the

Ch.

with

Na^COs.

Reduced with emission

In
ignition

of arsenical fumes.

tube with
a

Na CO3 and
2

Ch.

Volatilizes,
of

forming

mirror-like

deposit

metallic

As

in the cooler part of tube.

In flame on platinum wire

With borax bead on platinum wire

With Co(N0 3

)2

_.

4.

Bismuth,
Yields
hot,

Bi 2
a

3.

Before

the

Bp. on

Ch.

coating

orange-yellow
cold.

when

lemon-yellow when

The

yellow coating usually has a white outline.

Before
the

Bp. on

Ch.

with

Na

CO

3.

Easily reduced to metallic bismuth.

Yellow

bead

brittle,

but less so than antimony.

In ignition tube with

Na CO and
2

Ch.

26

BLOWPIPE ANALYSIS
In flame on platinum wire

With

borax

bead

on

platinum

wire.

In O. F. small quantity dissolves to a clear

yellow glass, which becomes colorless

when

cold

With Co(NO 3 ) 2
5.

_..

._

Cadmium, CdO.

Before the

Bp.

on

Ch.

Gives a coating on the coal.

Red-

dish-brown when cold.

Before the

Very
Ch.

volatile.

Bp.

on

with

Na2 CO 3

Readily
easily,

reduced.

The

metal

volatilizes

giving the characteristic coating.

In ignition tube with

Na CO 3 and
2

Ch.

In flame on platinum wire

With borax

bead.

In O. F. dissolves to a

clear yellowish bead, colorless

when

cold.

With Co(N0 8
6.

)2

Chromium, Cr 2

3.

Before the Bp. on

Ch.

No

change.

GENERAL REACTIONS
Before the
Bp.

2/

on

Ch.

with

Nc^COg.
in

Cannot be reduced.

Soda sinks

Ch.

and a green colored mass remains.

In ignition tube with

Na CO3 and
2

Ch.

In flame on platinum wire

With borax

bead.

Dissolves slowly but

hot,

colors intensely.

Yellow while

green

when

cold.
salt bead.

With microcosmic
when
hot,

Colors red

green when cold.

With Co(NO3 ) 2
Before the

7.

Cobalt, CoO.

Bp. on Ch.
is

In O. F. unchanged.
to the metal

In R. F.

reduced

and

is

magnetic.

Before

the
to a

Bp.

on

Ch. with

Na^COg.

Reduced

gray magnetic mass.

In ignition tube with

Na^COa and Ch.

In flame on platinum wire

28

BLOWPIPE ANALYSIS

With borax

bead

on

platinum

wire.

In O. F. colors very intensely blue, both hot

and

cold.
2

With Co(NO 3 )
8.

Copper, CuO.

Before the Bp. on Ch.

Fuses to a black globule, which can be

reduced with some
Before
the Bp.
difficulty.

on

Ch. with

Na CO
2

3.

Readily reduced to metallic bead, which

red in color, hard, malleable.

is

In ignition tube with

Na CO and
2

Ch.

In flame on platinum wire.

Colors flame

emerald-green.

With borax bead on platinum O. F. green when hot, blue when

With Co(N0 3
9.
)2

wire.
cold.

In

Iron,

Fe 2

3.

Before the
In

Bp. on

Ch.

In

O. F.

unchanged.

R. F.

becomes

black and magnetic.

GENERAL REACTIONS
Before
the

29

Bp.

on

Ch. with

Na CO
2

Reduced

to a metallic powder, magnetic.

In ignition tube with

Na CO 3 and
2

Ch.

In flame on platinum wire

With borax

bead

on

platinum

wire.
cold.

In O. F. red while hot, yellow

when

With Co(NO 3 ) 2
10.

Lead, PbO.

Before the Bp. on

to

Ch.
very

Easily

reduced

the

metal,

bead

malleable.

Coating yellow, surrounded by

white ring.
Before the
Instantly

Bp.

on

Ch. with
the

Na^COg.
Ch.

reduced.

Coats

upon

further blowing.

In ignition tube with

Na CO3 and
2

Ch.

Reduced
In

to the metal.

flame

on

platinum

wire.

Tinges

flame blue.

With borax

bead

on

platinum

wire.

30

BLOWPIPE ANALYSIS

In O. F. dissolves easily, forming a limpid

glass.

With Co(N0 3 )2
11.

Manganese,

Mn

3.

Before

the

Bp.

on Ch.

At high temperature

turns red.

Before the Bp. on Ch. with not reduced.

Na CO
2

3.

Is

Before the Bp. in O. F. on platinum

foil

with

-NagCOg.
hot.

Transparent

green

mass
cold.

when
In

Opaque, bluish-green when

tube with

ignition

Na CO 3 and
2

Ch.

Not reduced.
In flame on platinum wire

With borax bead on platinum wire.

violet-red while hot, amethyst-red

In O. F.
cold.

when

With Co(N0 3 )2
12.

Mercury,

HgO.

Before the

Bp. on

Ch.

Instantly reduced.

Very

volatile.
2 3.

Before the Bp. on Ch. with

Na CO

Re-

duced and

volatilized.

GENERAL REACTIONS
In
ignition

31
3

tube with

Na.2

CO

and Ch.
of

Sublimes condensing in the upper part

the tube as a metallic ring which
is

seen

with the lens to consist of minute globules

of

mercury.
In flame on platinum wire

With borax bead on platinum wire

WithCo(N0
13.

3 ) 2 __

Nickel, NiO.

Before the Bp. on Ch.

In R. F. reduced to

In O. F. unchanged.

metal, slightly magnetic.

Before

the

Bp.

on

Ch.

with

Na CO
2

8.

Easily reduced to the metal. In ignition tube with

Na CO and
2

Ch.

In flame on platinum wire

With borax bead on platinum wire. In O.F.

violet while hot, reddish-brown

when

cold.

With Co(NO 3 ) 2 ._

32
14.

BLOWPIPE ANALYSIS
Silver,

AgO.

Before the Bp. on Ch.

Easily reduced to the metal.

leable,

White, mal-

hard bead.

Coats the coal dark red

near assay.
Before the Bp. on Ch. with

Na CO 3
2

In-

stantly reduced to metallic globule.

In

ignition

tube with

Na CO and
2

Ch.

Reduced

to the metal.

In flame on platinum wire

With borax bead on platinum

O. F.
partially

wire.

In

dissolved.

Bead

becomes

milk-white.

With Co(NO 3) 2
Sn0 2
Before the Bp. on Ch. yellow
while
hot,

15.

Tin,

Coats

the

coal

dirty

white when cool.

Not reduced.

Before the Bp. on Ch. with

Na CO 3
2

Re-

duced
leable
assay.

to

metallic

tin.

White, hard, mal-

bead.

Coating white and close to

GENERAL REACTION'S
In ignition tube with

33

Na CO 8 and
2

Ch.

In flame on platinum wire

With borax bead on platinum

O. F.
glass.

wire.
to

In

small

quantity

dissolves

limpid

With Co(NO3 )2
ZnO.

Greenish-blue color.

6.

Zinc,

Before the Bp. on Ch.

Upon

ignition

becomes

yellow.

Is

not

reduced.

Before the Bp. on Ch. with

Na CO
2

3.

Re-

duced

to metal.

Rapidly

volatilized, coating

the coal white.

In ignition tube with

Na CO and
2 3

Ch.

In flame on platinum wire

With borax bead on platinum

O.F. yellow while
cold.

wire.

In

hot,

limpid glass

when
*

With Co(NO 3)

Green mass.

34

BLOWPIPE ANALYSIS

Having now given the principal reactions for the most important metals, we will proceed to the examination of the alkali metals,
the alkaline earths, and

some

of

the acid

elements.

THE ALKALI METALS

17.

Ammonium,
is

NH

4.

This

hypotheti-

cal

compound

commonly
its

classed

among

the alkali metals from

to the

close resemblance

members

of this group.

To
cal

detect the presence of this hypotheti-

metal,

mix the assay with about four

2 3,

parts of

Na CO

place in an ignition tube,

and apply

heat.

The odor

of the evolved
if

gas will be recognized, and

a piece of

red litmus paper be moistened and held at

the

mouth

of

the tube,

it

will

be turned
gas.

blue by the escaping

ammonia

We

are not authorized to infer the pre-

existence of

ammonium, however, from

the

GENERAL REACTIONS

3$

appearance of this reaction, for the presence of nitrogenous organic matter in the
substance, which would be
this

decomposed by
a

treatment, would give rise to such

reaction.

8.

Potassium.

Potassium
its

is

recognized

by the color which

salts

impart to the

Bunsen

flame.

If

a portion of a salt of

potassium be held on a platinum wire in

the
flame,
it

imparts

blue-violet

tint

which rapidly disappears.

19.

Sodium.
is

Like potassium,

this alkali
its

metal

detected

by the color which

salts give to the flame.

If

a sodium salt be held on the platinum

in

wire

the

flame,

it

imparts

an intense

yellow color.

The extreme

delicacy

of

this

reaction

has been mentioned elsewhere.

The

value

36
of this test

BLOWPIPE ANALYSIS
is
it

really lessened
is

by

its

great

delicacy, for

possible to detect minute

in

quantities

of

sodium
it

almost

all

sub-

stances, although
cal

combination.
wire

may As an

not be in chemi-

example, draw the

the
fingers,

platinum

between

and

then place in flame, and note presence of

sodium.

20.

Lithium, Li 2 0.

In the Bunsen flame

it

on the platinum wire

red tinge.

imparts a carmine-

Hydrochloric

acid

on

the

sample aug-

ments the

coloration.

THE ALKALINE EARTHS

21.

Barium, BaO.

In the Bunsen flame

it

on the platinum wire

green coloration.
fied

imparts an appleis

This reaction

intensi-

by moistening the sample with hydro-

chloric acid.

GENERAL REACTIONS
22.

37

Calcium, CaO.

In the
it

Bunsen flame

on the platinum wire

red
color,

imparts an orange-

which appears gray when seen

glass.

through blue

Hydrochloric acid on the sample makes

the color

more

intense.

23.

Strontium,

SrO.

In

the
it

Bunsen

flame on the platinum wire

intensely red color, which
is

imparts an

increased

by

converting the substance into the chloride.

THE ACID ELEMENTS

24.

Borates.

If

the substance be finely

powdered, moistened
then
placed

with

glycerine,
in

and
the

on
it

platinum wire

Bunsen
color.
If

flame,

imparts a brilliant green

turmeric paper be dipped into a soluof

C.,

tion
1

a
it

borate,
is

and

then
to

be

dried

at

00

turned

peculiar

red

38
color.

BLOWPIPE ANALYSIS
These two reactions are extremely

delicate.

25.

Bromides.
salt

Bromides

treated
of

with

microcosmic

and oxide

copper on

platinum wire impart to the flame a greenishblue color, the edges being decidedly green.
26.

Chlorides.

Chlorides are treated in

as

the

same

way

bromides.
is

The

color

imparted to the flame

azure-blue.

To

discriminate

between bromides and

the

chlorides

more

clearly,

substance

is

mixed with anhydrous potassium bisulphate

and fused
in

an ignition tube.

Bromine and sulphur dioxide are evolved

(if

the substance be a
filled

bromide), the tube

being

with a yellow gas possessing

the characteristic odor of bromine.

27.

Fluorides.

small

portion of the
is

substance in a finely powdered condition

GENERAL REACTIONS

39

placed in one of the ignition tubes, a strip

of

moist
the

Brazil-wood paper

is

introduced
is

into

open end, and

is

heat

applied.

Hydrofluoric acid
color of the paper
yellow.

evolved, and the red

is

changed into a straw-

Mica, containing only 0.75% of fluorine,

shows the reaction

clearly.

28.

Iodides.

Iodides are treated, as the

bromides and chlorides, in a bead of microcosmic

flame
is

salt

with

oxide

of

copper.

The

colored green.
in

Fused with potassium bisulphate

ignition

an

tube

the violet vapors

of

iodine

and thus iodides may be distinguished from chlorides and bromides.

are evolved,

29.

Nitrates.

If

nitrate

be

heated

upon charcoal before the

gration occurs.
If

Bp., violent defla-

the substance contain-

40

BLOWPIPE ANALYSIS
a very

ing the nitric acid be mixed with

small quantity

of

finely

powdered potasis

sium cyanide, the

deflagration

accom-

panied with ignition and detonation.

If

the

substance
with

be

mixed

in

dry

condition

dry

potassium
in

bisulphate,
tube,

and

is

then

heated

an

ignition

red-brown nitrous fumes are evolved.

reaction takes place
if

This

there

is

but a small

quantity of nitrate present.

30.

Phosphates.

Phosphates impart to

the flame a bluish green color.

is

The

color

made more

intense

by moistening the
acid,

substance with

sulphuric

and
the

then
plati-

taking the paste so formed on

num
flame.

wire and

placing

it

in

the

Bunsen

31.

Silicates.

Silicates,
salt

when

treated
wire,

with microcosmic

on a platinum

GENERAL REACTIONS
suffer decomposition;

41

the bases unite with

the phosphoric acid to form a transparent

glass in

which the

silica

may be

seen

float-

ing as a cloudy mass.

The bead must

silica

only be examined
it

for

while hot, since on cooling

becomes

opaque.

32.

Sulphides.

Many

sulphides,

when

heated in an ignition tube, volatilize and

give

a sublimate of

sulphur in combina-

tion with the metallic portion of the sub-

stance.

very delicate test for sulphur in whatit

ever combination
stance,

may be found

in a sub-

and which may be performed with

is

great ease,

to

mix the
2

finely
,

powdered
fuse in

assay with four parts,

Na CO 3 and

an ignition tube.
the tube
is

When

thoroughly fused
is

broken, and the fused mass

placed on a bright silver coin, and a drop

42
of

BLOWPIPE ANALYSIS
water
is

added.

If

the substance con-

tains sulphur, a black spot will

be observed

on

the

coin

where the fused mass was

placed.

Before going on to the next chapter, the

student should assure himself of his familiarity

with the reactions just given, and he

should practise with various substances, the

nature of which
is

unknown

to him.

CHAPTER

IV

BEHAVIOR OF SOME OF THE PRINCIPAL ORES BEFORE THE BLOWPIPE

FOR

the sake of practice, and as a fitting

"

introduction to
this chapter is

Determinative Mineralogy,"
It is

appended.

not intended

to give a detailed account of the minerals,

but rather to set before

the

student the

most marked characters, such as hardness,

specific gravity, color, lustre, etc.

To
we

determine the hardness of a mineral,

to

try

scratch

it

with

the

minerals

forming an arbitrary "scale of hardness,"

proceeding successively from the softest to
the hardest.

When we

say that a certain

that the

mineral has hardness

= 4, we mean
43

mineral

is

scratched by 4 on the scale, and

44
that

BLOWPIPE ANALYSIS
4 on
the
scale
is

scratched

by the

mineral.

The

scale of

hardness chiefly in
is

use

is

the Mohs-Breithaupt scale, which

as follows:

1.

Talc,

common

laminated light green

variety.
2.

Gypsum,

crystallized.

3.

Calcareous spar, transparent variety.

4.
5.

Fluor spar, crystalline.

Apatite, transparent.

6.
7.

Orthoclase, white cleavable variety.

Quartz, transparent.

8.
9.

Topaz, transparent.
Sapphire, cleavable variety.

10.

Diamond.
seldom happens
in

It

determining the
its

hardness of a mineral that

actly
of

hardness ex-

conforms to that

of

some one member

the scale.

In such cases

we

generally

estimate the hardness.

For example, sup-

PRINCIPAL ORES BEFORE THE BLOWPIPE 45

pose
softer

mineral

was

harder
it

than

4,

but
5

than

5,

and that

was nearer

than
In

4,

then we would
to

call its

hardness 4^.
scale
file,

order

preserve
a

the

some
first

operators
cutting
until a

use

three-cornered

the

mineral
is

and

then

the
is

scale

number

found, which

abraded

to

about the same depth as the mineral

under examination.
Since a set of minerals forming a scale
of

hardness

is

not

always

at

hand,

the
is

following

scale
:

given

by

Chapman

appended

1.

Yields easily to the

nail.

2.

Yields with difficulty to the

nail

or

just receives

an impression from

it.

Does

not scratch a copper coin.

3.

Scratches a copper coin but

is

also

scratched

by

it,

being of about the same

degree of hardness.

46
4.

BLOWPIPE ANALYSIS
Not scratched by
a copper coin.

Does

not scratch glass.

5.

Scratches glass with

it.

difficulty,

leaving

its

powder on
6.

Yields readily to the knife.

glass
easily.

Scratches

Yields

with

difficulty to the knife.

7.

Does not
edge
10.

yield to the knife.

file,

Yields

to the
8.
9,

of a

though with
flint.

difficulty.

Harder than
gravity

Specific

cannot
aid
is

well

be

deter-

mined without the

hence
its

of

a balance, and

value here

not great.

As

in

the preceding chapter, alphabetic

will

arrangement

be employed.

ORES OF ANTIMONY
Stibnite,

Sb 2 S 3

Sb.;i, S.2 9

*H =
color

2,

= 4.524.62.
metallic lustre.
*

Of lead-gray

and

Consists of a large
Specific Gravity.

number

H = Hardness, G =

PRINCIPAL ORES BEFORE THE BLOWPIPE 47

of

needle-shaped crystals.

Brittle.

Fuses

in candle flame.

In an ignition tube yields

a sublimate of sulphur.

On

Ch. before the

Bp.

it is

volatilized, giving

antimony coating
blue.

and tinges the flame pale

ORES OF ARSENIC
Native Arsenic, As.
of Sb,

This contains traces

Ag, Fe, Co, and Ni.

3-5>

H=
color.
idly.

= 5.7-5.8.
before

Dark gray
the

in

Fracture tin-white, tarnishing rapVolatilizes

Bp. on

Ch.
of

without

melting,

giving white

coating

arsenious acid and characteristic garlic odor.

In ignition tube
ring.
it

sublimes, giving arsenical

Realgar,

AsS, As

70,

30.

H = 1.5

2,

3.56.

Bright red to orange-red color

lustre.

and resinous
it

In

an ignition tube

fuses

and

finally

sublimes.

The

sub-

48 limate

BLOWPIPE ANALYSIS

when

cool

is

red

and transparent.
Bp. on Ch. and

Fuses readily before the

-

burns with pale yellowish flame, emitting

gray-white fumes having garlic odor.

Orpiment,

As 2 S 3 As
,

61,

39.

H = 1.5 -2.0,
Lemon-yellow
pearly lustre.
in
Sectile.

0=3.4-3.5.
and
resinous

color

or

Before the Bp. on

Ch. behaves like realgar, but in an ignition

tube
is
it

gives a dark yellow sublimate which

transparent.

ORES OF BISMUTH
Native Bismuth, Bi.
of As, Te,

This contains traces

and

S.

H = 2.0 - 2.5, G = 9.7 - 9.83.

white,
lustre.

Color, silverred.

slightly
Brittle

tinged with

Metallic

when

cold, but

may

be lamiCh.

nated

when

hot.

Before the
Bi.

Bp. on

behaves like pure

PRINCIPAL ORES BEFORE THE BLOWPIPE 49

Bismuthite, Bi 2

90,

CO

7,

HO
2

3,

H = 4.0 -4.5,
and vitreous
tions.
lustre,

= 6.9-7.8.

Usually of a white or light greenish color

in

acicular crystalliza-

In

an

ignition

tube

decrepitates,

yielding water and

turning gray.
is

Before

the Bp. on Ch.

to

it

fuses easily and

reduced

metallic

globule,

coating the
it

Ch. with

Bi 2

3.

With Na2 CO 3

occasionally gives

the sulphur reaction.

ORES OF CHROMIUM
Chromic Iron Ore, FeO.32, Cr2 O 8 .68.

A1 2 O 3 Fe 2 O 3 MnO, and
,
,

MgO

are

commonly
Occurs

present.

H = 5.5,
In

= 4.32-4.57.

usually massive.
ish black.
netic.
tallic.

Color, iron-black to brownvarieties strongly

magand somewhat meLustre, shining

in

many

Heated

an ignition tube, remains

unchanged.

Infusible before the Bp.

on Ch.

50

BLOWPIPE ANALYSIS
the

Before

Bp. on

Ch. with

Na CO
2

and

KCN
it

yields metallic iron.

to

In borax bead

slowly dissolves

a clear transparent

glass,

which

is

a beautiful green

when

cool.

ORES OF COBALT
Smaltite, Co(Fe, Ni)

As

2,

Co

28,

As

72.

H = 5.5, G = 6.37 - 7.30.

or
steel-gray.

Color, tin-white
metallic.

Lustre,

When
it

heated

to

redness in an ignition tube

yields a sublimate of metallic arsenic.

Before

the Bp. on Ch.

it

fuses readily, with emis-

sion of arsenical fumes, to a grayish black

magnetic globule.

This globule may be

examined

for iron, cobalt,

and nickel with

the borax bead.

Cobaltite,

8.19.
white
Before

CoS 2 + Co As Co. 36, As. 45, H = 5.5, = 6.0-6.3. Color, silver2,

tinged
the

with

red.

Metallic

lustre.

Bp. on

Ch. fuses

easily,

with

PRINCIPAL ORES BEFORE THE BLOWPIPE

51

emission of copious arsenical fumes, to a

gray magnetic globule.

in the ignition

Remains unchanged

tube.

Linnaeite, (Co, Ni) 3 S 4 (Co, Ni)s8,

,

8.42.
steel-

H = 55,
Crystallizes

= 4.8-5.0.
in

Color, bright

gray, sometimes reddish.

Lustre,

metallic.

the

regular

octahedron.

Before the Bp. on Ch. fuses to a metallic

globule which
is

attracted by the magnet.

With borax bead

gives reaction for cobalt.

Erythrite,

Co3 O 8 As 2 + 8
2

O,

CoO.37.6,

O.24.o.

H= 1.5 -2.0,
Color, crimson
tallized, of

0=2.95.

to

peach-red.

When

crys-

pearly lustre, but frequently dull

and earthy.
off

Heated

in ignition tube gives

water,

and color changes

to

blue

or
it

green.

Before the Bp. on Ch. in

R. F.

52

BLOWPIPE ANALYSIS

emits arsenical fumes and melts to a dark

gray globule which with the

reacts for cobalt.

borax

bead

ORES OF COPPER
Native Copper, Cu.

H = 2.5- 3
Color,

= 8.5-8.9.
Lustre,
metallic.

copper-red.

Oc-

curs usually massive and very arborescent.

Before

the
is

Bp.

on

Ch.

it

fuses,
it

and

if

the heat

sufficiently

high
;

assumes a
it

bright bluish-green surface

is

on cooling

covered with a coat of black oxide.

it

In

the borax bead

reacts for copper.

Chalcopyrite,

CuFeS

2,

Cu

35,

Fe

30,

8.35.

H = 3.5 -4,
often

= 4.1-4.3.
golden-yellow.

Color,

brass-yellow,
metallic.
ally

Lustre,

Occurs

crystallized, but is generIs

found

massive.

easily

scratched

PRINCIPAL ORES BEFORE THE BLOWPIPE

with a knife.
decrepitates,

53

Heated

in

an ignition tube
faint

and occasionally yields a

Before the

sublimate of sulphur.

Bp. on

Ch.

it

blackens, but becomes red again on

cooling.

Before the Bp. on Ch. with

it

Na2 CO 3
with

and

KCN

is

reduced, and the metals are

It reacts

obtained in separate masses.

the borax bead for copper and iron.

Copper

Glance,

H=
blue

2.5

3.0,

Cu S, Cu .80, S 20. = 5.5 - 5.8. Color, dark

2
.

to

steel-gray.

Occurs

in

compact

masses, often very shining.

Before the Bp.

on

Ch.

fuses

to

globule

which

boils

and emits glowing drops.

Sulphur dioxide
is

escapes abundantly, and the outer flame

colored blue.

Before the Bp. on Ch. with

Na

CO

yielding a metallic globule.

Tetrahedrite, 4

CuS + Sb 2 S 3
iron,

Frequently

contains

silver,

mercury,

and

zinc.

54

BLOWPIPE ANALYSIS

H = 3.0 -4.0,
to iron-black.

= 4.5-5.
Heated
in

Color, steel-gray

an ignition tube
of

fuses
oxide.

and gives a sublimate

antimonious

When

mercury

is

present this con-

denses in the upper part of the tube, forming the characteristic mirror.
Bp. on

Before the
metallic
;

Ch.

it

fuses

readily to a

globule, emitting dense white fumes

zinc

and antimony coatings are deposited on the

Ch.
After long ignition before the Bp.,
is
if

the mineral

finely

powdered and mixed

the ore
is

with

Na CO 3 and KCN,
2

reduced

to the metal.

Cuprite,

Cu

O,

Cu

89,

1 1.

H = 3.5 -4.0,

= 5.5-6.15.
Before the Bp.
finally

Color, intense crimson-red.

on Ch. blackens and fuses quietly, and

yields a metallic globule of copper.

Before

the Bp. on Ch. with

is

Na CO 3 and
2

KCN

it

easily reduced.

PRINCIPAL ORES BEFORE THE BLOWPIPE

Malachite,
2

55
.

CuO + CO + H
2

O,

CuO

72,

CO

.20,

O.8.

H = 3.5 -4.0,
Color, bright

0=3.90-4.03.
Occurs generally
in

green.

mammillated concretions.
and
fracture, silky.

Lustre, shining
in

Heated

an ignition
Before the

tube yields water and blackens. Bp. on Ch.

it

fuses to a metallic globule.

Before the Bp. on

Ch. with
reduced.

Na CO 3 and
2

KCN

it

is

easily

With borax

bead gives characteristic coloration.

Azurite,

3
2

CuO + 2 CO + H
2

O,

CuO

69,

C0

.26,

0.

5.

H = 3.5 -4.0,
Color, azure-blue.

0=3.77-3.83.
in crys-

Occurs usually

tallized or globular masses.

Lustre, earthy

or vitreous.

Before the Bp. and with other

reagents behaves like malachite.

56

BLOWPIPE ANALYSIS
Chrysocolla

CuO + SiO + 2 H
2 2

O,

CuO.45.3,

O.20.5.

H = 2.0- 3.0, G=2.

Color, bluish-green, closely resembling malachite.

its

Occurs usually as an incrustation,

surface being very smooth, like enamel.

it

In an ignition tube
water.

blackens and yields

it

Before the Bp. on Ch. in O. F.

blackens, coloring the flame bright green;

in the

R. F.

it

turns red.

Before the Bp.

on Ch. with Na-jCO 3 yields metallic copper.

In borax bead
it

reacts for copper.

Atacamite,
.

CuCl 2 +
50. i
,

3
.

CuO H 2 2
1

Cl

16.6,

20.3,

Cu

HO
2

3.0.

H = 3.0 -3.5, G= 3.75 -3.77.

Color,

green

to

blackish
vitreous.

green.

Lustre,
ignition

adamantine

to

In

an

tube yields water.

colors flame blue.

Before the Bp. on Ch.

Before the Bp. on Ch.

with

Na2 CO 3 and

KCN
it

is

reduced to the

metal.

In borax bead

reacts for copper.

PRINCIPAL ORES BEFORE THE BLOWPIPE

S7

ORES OF IRON
Limonite,
2

Fe2 O 3 +

O,

Fe2 O 8
3.6

86,
4.0.

HO
2

14.

H =
to in

5.0-5.5,

G=
In

Color,

brown

ochre-yellow.

Earthy or
an
the
igni-

semi-metallic
tion

appearance.
water.

tube

yields

Before

Bp.

on Ch.
iron.

infusible.

In borax bead reacts for

Hematite,

Fe,O3 Fe
,

70,

30.

H = 5-5 -6-5,
metallic.

= 4.9-5.3.
Lustre,

Color, dark steel-gray to iron-black.

When

pulverized

yields

red

powder.

Before the Bp. on

Ch. infusible.
In

After long roasting becomes magnetic.

borax bead gives usual indications of iron.

Magnetite,

Fe 3 O 4 FeO
,

.31,

Fe 2 O 3

69.

H = 5-5 -6.5,

0=5.17-5.18.

58

BLOWPIPE ANALYSIS
Lustre, shining and meits

Color, iron-black.
tallic.
is

Pulverized,

powder

is

black.

It

strongly magnetic.

Fuses with

difficulty

before the Bp. on Ch.

for iron.

In borax bead reacts

Pyrites,

FeS 2 Fe
,

47,

53.

H = 6.0 - 6.5, G = 4.95 - 5.20.

Color, brass-yellow.

Lustre, metallic.
cubes.
It

Occon-

curs
tains

commonly
Mn.

in

often

small quantities of

Au, Ag, Cu, As,

an ignition tube
residue

Co, and
gives

Heated

in

a sublimate of sulphur, the

becoming
Ch.
in

magnetic.

Before
is

the

Bp.
off

on

O. F. sulphur

burned

and

the red oxide remains.

This residue
etc.

may

then be examined for iron,

Marcasite (White Iron Pyrites).

the

Having

same general composition

lighter in color.

as pyrite, but

much

Crystals, prismatic.

Before the Bp. on Ch. behaves like pyrite.

PRINCIPAL ORES BEFORE THE BLOWPIPE

Pyrrhotite,

59

Fe 7 S 8 Fe.6o.5, 8.39.5.
,

H = 3.5 -4.5,
Color,
pyrite,

= 4.58-4.64.
Closely

bronze-yellow.

resembles
it

but

may be

distinguished from

by being feebly magnetic.

ignition tube yields

Heated

in

an

no sublimate.

Before

the Bp. on Ch. fuses to a magnetic globule,

which exhibits a yellowish

ture

crystalline struc-

when

fractured.

Mispickel,

FeAsS, Fe.34, As. 46, 8.20.

Color,
silver-

H = 5.5~6.o, G = 6.0 -6.2.

white.

Lustre, metallic; very brittle.

it

Often

associated with
of

we

find small quantities

Co, Ag, and

it

Au.

Heated

in

an

igni-

tion tube

first

yields a red sublimate of

sulphide

of

arsenic,

and

then

afterward

a crystalline sublimate of metallic arsenic.

Before the Bp. on Ch. emits dense fumes

of

arsenic and deposits

a coating on

the

60
coal;
it

BLOWPIPE ANALYSIS
then
fuses
to

globule

which

behaves like pyrrhotite.

Siderite,

FeCO

3,

FeO.6 2

CO

.38.

H = 3.5 -4.5, 0=3.7-3.9.

yellow to reddish brown.
Crystallizes in

Color,

grayish

Lustre, pearly.

rhombohedrons with curved

faces

these crystals are distinctly cleavable

and massive.
it

Heated
with

in an ignition tube

decrepitates

evolution

of

carbon

dioxide.

Before the

Bp. on

Ch. infusible.
2

Before the Bp. on Ch. with

to a

Na CO 3
for

it

fuses
it

magnetic mass.

With borax bead

re-

acts for iron

and sometimes

manganese.

ORES OF LEAD
Galena, PbS,

Pb

87,

3.

H = 2.5,
tre, metallic.

0=7.4-7.6.
Lus-

Color, bluish gray, slowly tarnishing.

Crystals in the form of cubes.

PRINCIPAL ORES BEFORE THE BLOWPIPE 6 1

Heated

in

an ignition tube

it

sometimes

decrepitates and yields a sublimate of sul-

phur.
to

Before the Bp. on Ch. easily reduced

metallic
state,

the

the

Ch.

becoming
of
lead.

coated

with

sulphate

and oxide
usually
this,

The
little

metallic
silver.

globule

contains

To

separate
is

the process

known
is

as "cupellation"

employed.
i

A hole

bored into the Ch. about

cm. in diameInto this hole

finely

ter
is

and about 6 mm. deep.

stiff

placed a

paste

made by mixing
little

pulverized bone-ash with a

water.

soda and

This paste
is

is

pressed in hard, and

off,

then the surface

centre
is

smoothed

and the
rounded

slightly depressed with the

end

of a glass rod.
is

The

charcoal so pre-

pared
paste

set in a

warm

place to allow the

to

dry.

When

the paste
is

is

quite

dry the small globule of lead

placed in

the depression in the centre of the bone-

ash "cupel," and

is

there exposed

to

the

62

BLOWPIPE ANALYSIS

O. F. from the Bp.

The

lead

is

oxidized

and

is

absorbed by the bone-ash, while any

present will

silver

remain

in

the

central

depression as a bright shining bead.

Cerusite,

PbCO

3,

PbO

84,

CO

.i6.

H = 3.0 -3.5,
gray, or yellow.
tallizes in

= 6.46-6.57.

Color, white,

Lustre, adamantine.

Crys-

prismatic needles

When
is

heated
evolved

in

an ignition tube carbon dioxide

and the residue turns yellow. Bp. on Ch. readily reduced

lead.

Before the
to

metallic

Anglesite,

H = 2.03.0,
low, gray,

PbSO PbO 74, SO .26. = 6.12 6.39. Color, yel4,

.

and brown.

Lustre, adamantine,

resinous.
decrepitates,

Heated

in

an

ignition
yields

tube
little

and sometimes
the

water.

Before
bead,

Bp. on

Ch. fuses

to

clear

which on cooling becomes

PRINCIPAL ORES BEFORE THE BLOWPIPE 63

opaque.
Before
is

the

Bp.

on

Ch.

with

Na CO 3
2

reduced to the metal giving a

yellow coating.

The Na^Og absorbed by

the coal reacts for S.

ORES OF MANGANESE
Pyrolusite,

MnO
Lustre,

2,

Mn

63.2,

36.8.

H = 2.02.5,
steel-gray.

= 4.82.

Color, iron-black to

non-metallic.

Heated
little

in

an ignition tube yields generally a

water,

and

if

the
is

temperature
evolved.

be

high
the

enough,

oxygen

Before

Bp. on Ch. infusible.

characteristic color.

In borax bead gives

Psilomelane,

Mn O + H
2

O.

H = 5.5 -6.0,
Color,

0=3.7-4.7.
steel-gray.

iron-black

to

Generally

resembles pyrolusite,

but

is

distinguished
It

from

it

by

its

superior hardness.

fre-

64

BLOWPIPE ANALYSIS

quently contains

BaO and

Li 2 O.

It

behaves

before the Bp. like pyrolusite.

Wad (Bog
essentially

Manganese).
2,

This mineral

is

MnO

MnO, and
,
,

O,

with
,

small quantities of
etc.,

Fe 2 O 3 A1 2 O 3 BaO, SiO 2
it.

associated with

H = 0.5 -6.0,
black.

= 3.0-4.2.
in

Color,

dull

Heated

an ignition tube yields

it

water in abundance, otherwise

like pyrolusite.

behaves

ORES OF MERCURY
Native

Mercury,

Hg.
Is

G=
liquid
in

13.5

13.6.

Color, silver-white.

at

all

ordi-

nary temperatures.
tube
is

Heated

an ignition
condensing

volatilized,

the vapors

in the

upper end

of tube to small metallic

globules of Hg.
is

Before the Bp. on Ch.

it

volatilized.

Frequently contains Ag.

PRINCIPAL ORES BEFORE THE BLOWPIPE 65

Cinnabar,

HgS Hg.86,
2,

S.

14.

H = 2.0 -2.5, G = 8.0 -8.2.

Color, scarlet-red to brick-red.
metallic.
of

Lustre, non-

When
it

pulverized yields a powder

vermilion-red color.

Heated

in

an

ig-

nition tube

volatilizes, yielding

black
red.

sublimate, which

by

friction

becomes

Before the
tilized.

Bp. on
in

Ch.

it

is

wholly vola-

Heated
3

an ignition tube with

sublimes,

Na CO
2

metallic

mercury

con-

densing in the upper portion of the tube

in

minute globules.

ORES OF NICKEL
Millerite,

NiS, Ni.644, $.35.6.

H = 3.0 -3.5,
Color,
brass-yellow.
it

0=5.2-5.6.
Brittle.

Before

the

Bp. on Ch.
globule.

fuses to a magnetic, metallic

The

roasted mineral gives in the

borax bead the color reaction characteristic

66
of

BLOWPIPE ANALYSIS
nickel,
is

and sometimes that

it.

of

cobalt,

which

often associated with

Niccolite,

NiAs, Ni

44,

As

56.

H = 5.0 -5.5, G= 7.35 -7.67.

Color,

pale
brittle.

copper-red.

Lustre,

metallic.

Very
yields

Heated

in

an ignition tube
of to

a
the

copious
residue

sublimate
falling

arsenious

oxide,

greenish

powder.
white
fumes.
istic

Before the Bp. on Ch. fuses to a

brittle

globule

emitting

arsenical

In borax bead gives color character-

of nickel.

Frequently in this mineral

the
arsenic
is

portion

of

replaced

by

antimony.

ORES OF SILVER
Native Silver, Ag.

H = 2.5
tile

3.0,

G=IO.I

n.o.

Color, silver-white.

Lustre, metallic.

Ducasso-

and malleable.

Usually occurs

PRINCIPAL ORES BEFORE THE BLOWPIPE 6/

ciated

with

Au,
Bp. on
is

As,

Sb,

Cu,

Fe,

etc.

Before the

Ch.

easily fuses

to

globule which

surrounded with a dark

red coating on the coal.

^
Argentite, Ag.2 S,

Ag.S/.i, S.

12.9.

H = 2.0
Very
sectile.

2.5,

0=7.20-7.36.
Lustre, metallic.

Color, blackish lead-gray.

Before the

Bp. on

Ch. in

O. F. intumesces with evolution of sulphur

dioxide, finally yielding a metallic globule
of

Ag.

Pyrargyrite,

Ag SbS
3

3,

Ag.59.8, Sb.22.5,
Color,

8.17.7.

H = 2.5, 0=5.77-5.86.
In

black to dark cochineal-red.

lic,

Lustre, metal-

adamantine.

an

ignition

tube

it

yields

on continued heating a sublimate

of

antimony sulphide.
it

Before the Bp. on Ch.

of

gives

coating

antimony

trioxide.

68

BLOWPIPE ANALYSIS
the

Before

Bp. on

Ch. with
silver.

Na CO 3
2

is

reduced to metallic

Proustite,

Ag S
3

As,

Ag.65.5,

As.

15.1,

S. 194.

H=

2.0 -2.5,

0=5.57-5.64.
behaves like

Color, light red.

tine.

Lustre, splendent, adamanit

Before the Bp. on Ch.

it

pyrargyrite, save that

gives off arsenical

fumes instead

of

antimonious oxide.

Stephanite,

Ag S
5

Sb,

Ag.68.5, Sb.is.3,

16.2.

H = 2.0
to

2.5,

G = 6.2
gray.
fragile.

6.3.

Color,

iron-black
tallic.

blackish
brittle

Lustre,

meig-

Very
it

and

In an

nition tube
yields a

decrepitates, fuses,

and

finally
tri-

slight

sublimate of antimony

sulphide.

Before the Bp. on Ch. gives a Before the

globule
of

coating of antimonious oxide.

Bp.

on

Ch.

with
is

Na CO 3
2

metallic

silver

obtained.

The

mineral

frequently contains copper and iron.

PRINCIPAL ORES BEFORE THE BLOWPIPE 69

Kerargyrite,

AgCl, Ag.753, 0.24.7.

H =1.01.5,
ous,

0=5.52.

Color, white, gray,

yellowish, greenish to blue.

Lustre, resin-

adamantine.
in
it

Soft

like

wax.

Fuses
Bp.

easily

candle-flame.
is

Before the
to

on Ch.
silver.

readily

reduced

metallic

ORES OF TIN
Cassiterite,

SnO

2,

Sn.79, O.2i.

H = 6.0 -7.0,
Color, brown,
brilliant.

= 6.8-7.0.
Lustre,

black.

adamantine,
in

Occurs
Reentrant

crystallized

square

prisms.

angles

characteristic.

Before the

Bp. on Ch. with

Na CO 3 and
2

KCN
action.

reduced to a metallic globule of

tin.

In the borax bead gives characteristic re-

Stannite,

Cu S
2

Sn S 2
.

4.0,

SnS 2 + G = 4.3
.

(FeS
4.5.

ZnS)
Color,

70
steel-gray

BLOWPIPE ANALYSIS
to

iron-black.

Lustre,

metallic.

Occurs usually massive and disseminated.

Heated

in

an ignition tube
Before the
dioxide
tin.

it

yields sul-

phur dioxide.
emits

Bp. on

Ch.

it

sulphur

and becomes covBefore the Bp. on

it

ered with oxide of

Ch. with

Na CO 3 and
2

impure globule

of

KCN A copper.

gives

an

very

difficult

mineral to determine.

ORES OF ZINC
Calamine,
67.5,
2

H Zn O Si, SiO H O.7.5. H = 4.5 -5.0,

2 2

.25.o,

ZnO.

0=34-3.5.
Lustre,

Color, white, gray, bluish, or brown.

vitreous.
Brittle.

In

an

ignition

tube

yields

water

when heated and

With Co(NO 3 ) 2

becomes

milky white.

Before the Bp. on Ch. pracit

tically infusible.

assumes

a green color which passes into a fine blue

when

the heat

is

increased.

PRINCIPAL ORES BEFORE THE BLOWPIPE

Smithsonite,

71

Zn

CO ZnO
3,

64.8,

CO

35.2.

H = 5,
Heated

= 4.30-445.
in

Color, gray, yellow,

brown, and green.

Lustre, vitreous, pearly.

an ignition tube
It

CO

is

evolved,

residue appearing white.

impurities of Cd, Pb, Fe,

often contains

Mn, Ca, and Mg.

dark

When

these are present the residue in the

ignition

tube

becomes

on
2

cooling.
3

Before the

Bp. on Ch. with

it

Na CO and
It

exposed to the R. F.
gives
the

is

decomposed.
for

characteristic
)2
.

reaction

zinc

with

Co(NO 3

Zincite,

ZnO, Zn

80.3,

19.7.

H = 4.0 -4.5,
Color,

= 5.43-5.70.
Lustre,
brilliant,

blood-red.

sub-

adamantine.

Before the Bp. on Ch. infusible.

Before the Bp. on Ch. with

coating of zinc oxide.

Na

CO

gives

Oives characteristic

72

BLOWPIPE ANALYSIS

reaction with

Co(NO 3

)2

It

frequently con2

tains a small quantity of

Mn O

3,

which may

be detected in the borax bead.

Sphalerite,

ZnS, Zn

67,

33.

H = 3-5-4-0,
Color, yellow to black.
iant,

0=3.9-4.1.
Lustre, resinous,
brill-

and sometimes submetallic.

Heated

in

an ignition tube sometimes decrepitates.

Before the
reduced.

Before the Bp. on Ch. infusible.

Bp. on

Ch. with
)2

Na CO 3
2

easily

With Co(NO 8
action.
tities of

gives the characteristic re-

It

frequently contains small quanetc.

Cd, Hg, Sn, Pb, Au, Ag,

PRINCIPAL ORES BEFORE THE BLOWPIPE 73

TABLE OF COLORS OF COATINGS ON CHARCOAL

ELEMENT

74

BLOWPIPE ANALYSIS

III

TABLE OF COLORS OF BORAX BEADS

IN OXIDIZING

FLAME

ELEMENT

PRINCIPAL ORES BEFORE THE BLOWPIPE

?$

IV
TABLE OF COLORS OF BORAX BEADS IN REDUCING FLAME

ELEMENT

BLOWPIPE ANALYSIS

TABLE OF COLORS OF MICROCOSMIC SALT BEADS

OXIDIZING FLAME

IN

ELEMENT

PRINCIPAL ORES BEFORE THE BLOWPIPE 77

VI
TABLE OF COLORS OF MICROCOSMIC SALT BEADS
REDUCING FLAME
IN

ELEMENT

THE PRACTICAL METHODS

OF

ORGANIC CHEMISTRY
AUTHORIZED TRANSLATION
1

2 mo.
BY

Cloth.

Price, $1.60, net

TRANSLATED BY

LUDWIG GATTERMANN,

Ph.D.,

WILLIAM SHAFER,
Instructor in Organic

Ph.D.,

Professor in University of Heidelberg.

Chemistry

in Lehigh University.

THE GUARDIAN.
"
is

The

selection

a most useful,

and judgment throughout is excellent. The book practical adjunct to any good text-book on organic

chemistry."

PHARrtACEUTICAL REVIEW.
is a book that should be in the library of every teacher of organic chemistry, and one which will no doubt be of great value to students in their second year of organic chemistry. Its chief peculiarity and merit is in the great stress laid on practical laboratory work.

" This

...

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NATURE.
" Since the advance of organic chemistry in this country must, in a measure, depend on the nature of the available text-books, both the author and the translator deserve our thanks for providing us with a work such as the present one."

PUBLISHED BY

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FIFTH AVENUE,

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OUTLINES
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INDUSTRIAL CHEMISTRY
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By FRANK HALL THORP,
of Technology.

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Instructor in Industrial Chemistry in the Massachusetts Institute

Cloth.

8vo.

Price, $3.50 net

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is brought thoroughly up to date, and in some cases the probable development are nicely foreshadowed. The descrip-

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and the

illustrations well selected.

The general arrangement and make-up

.
. .

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felt

altogether the

book

fills

well a need long

is excellent, and by teachers of Indus-

trial

Chemistry.

I shall

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it."

my

class

and

shall take pleasure in

recommending

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I have examined it carefully and think it a most excellent book, meeting a want I have long felt in my higher classes. I have introduced it in this year's classes."

"

W.
"

A. NOYES,

in

Science.

The

and

descriptions of processes, while necessarily concise, are clear The author has evidently made a careful study of interesting.

recent methods of manufacture as well as of older, standard processes. The frequent reference to American practice is an important feature

which distinguishes the book from other works on chemical technology. A select bibliography follows each subject, and will be found very
useful."

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