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REESE LIBRARY
UNIVERSITY OF CALIFORNIA.
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EXPERIMENTS
ARRANGED FOR

STUDENTS

IN

GENERAL CHEMISTRY

BY

EDGAR

F.

SMITH

AND

HARRY

F.

KELLER,

it

PROFESSOR OF CHEMISTRY, UNIVERSITY OF


PENNSYLVANIA, PHILADELPHIA.

PROFESSOR OF CHEMISTRY, MICHIGAN MINING


SCHOOL, HOUGHTON.

SECOND EDITION, ENLARGED, WITH 37 ILLUSTRATIONS.

PHILADELPHIA:
P.

BLAKISTON, SON & CO


1012 WALNUT STREET.

|)Q$
COPYRIGHT, 1891, BY

PRESS or WM F. FELL & Co.,


I22O-24 SANSOM ST.,
PHILADELPHIA.

P.

BLAKISTON, SON

&

Co.

PREFACE.
This

little

work

is

The arrangement of

designed as a guide for beginners in chemistry.


the course

is

such as the authors have used with

success in the instruction of their classes

its

object

with the supervision of an instructor, but rather to


reference

is

made

to Richter's

is

assist

not to dispense

him.

book on the subject can be employed

in

its

stead.

text-

The experiments

have been collected from various sources, and no claim


originality.

Although

"Inorganic Chemistry," any other

is

made

for

CONTENTS.
PART

I.

CHAPTER
I.

II.

III.

PAGE

APPARATUS, MANIPULATIONS AND OPERATIONS,

9-10

GENERAL PRINCIPLES
HYDROGEN,

10-11

12-14

IV.

CHLORINE, BROMINE, IODINE, FLUORINE,


V. OXYGEN, SULPHUR,
VI. NITROGEN, PHOSPHORUS, ARSENIC, ANTIMONY,
VII. CARBON AND SILICON, BORON,

PART

14-19
.

."

19-25

25-32

32-34

II.

VIII. POTASSIUM, SODIUM [AMMONIUM],


IX. CALCIUM, STRONTIUM, BARIUM,

X. MAGNESIUM, ZINC,
MERCURY, COPPER, SILVER, GOLD,
XII. ALUMINIUM, TIN, LEAD, BISMUTH,

XL

XIII. CHROMIUM, MANGANESE, IRON, NICKEL, COBALT,

35-38
39-41

41-42

43-46
46-50
50-56

NON-METALS.

CHAPTER

I.

APPARATUS, MANIPULATIONS AND OPERATIONS.


The Bunsen burner and

1i)

Make

i.

ganese dioxide in
reducing flame (?).
flame.

(2)

it.

5.

the blowpipe.

Dissolve a very minute quantity of manin the oxidizing flame (?).


Heat
4. In the
3.
Heat oxide of lead on charcoal in the reducing

a borax bead.

2.

In the oxidizing flame.


Working with glass tubing and rods.
6.

i. Cut various lengths of rods and


tubing.
by softening and turning the ends in the lamp.

(3)

Construct a wash-bottle (Fig.

2.

Round

the sharp edges

i).

FIG.

i.

Soften a sound cork by rolling it under your foot on


a clean floor.
2. Bore two parallel holes through it by
i.

means of a cork-borer. These perforations should be cylindrical and of less diameter than the glass tubes they are
Use a rat-tail file in enlarging them. 3. Cut
to receive.
suitable lengths of glass tubing.
4. Draw the longer one
to a fine point after softening in the flame.

5.

Bend

the

tubes in an ordinary fish-tail burner, and round the sharp


6. Fit the different pieces together.
edges.

Arrange some other form of apparatus for practice.


The balance.
i. Weigh an object by placing it on the left-hand pan of the balance,
and a weight judged about equal on the right-hand pan. Should the
latter be found too heavy, replace it by the next smaller one
if too light,
next
the
heavier
one.
Then
the
smaller
add
by
weights,
systematically
(4)
(5)

middle of the scale. The final adjustment


In adding or removing weights, the supports

until the needle points to the


is

made with

the rider.

must always be
(6)
i.

raised.

Measuring vessels.
Measure off 10 cc. of water (a]
9

in a cylinder,

()

in a burette, (c)

EXPERIMENTS IN GENERAL CHEMISTRY.

10
in a pipette.

Always read the lower meniscus.

2.

Measure

off similarly

3. Measure
50, 100 and 200 cc. of water, and determine their weight.
the volume of 50 grms. of oil of vitriol, and of 65 grms. of muriatic acid.
What are the specific gravities of these substances ? Note the relation

between weight and volume in the metric system.


(7) Chemical operations Solution, evaporation, crystallization, precipitation, filtration, washing and drying.
i. Place into a test-tube pure sodium carbonate, into another cobalt
Stir.
What occurs ? 2. To
chloride, and add distilled water to each.
:

any change ? Now add a little


3. Pour 5 cc. of strong hydrochloric acid upon powdered manganese dioxide ; observe appearance and
odor.
Note, too, in each case, whether heat has any effect. Distinguish
calcium carbonate, add water.
hydrochloric acid.

What

Is there

action has

it ?

between chemical and mechanical solution.


and the calcium carbonate solutions, each

4.

Heat the cobalt chloride


on an iron

in a separate dish,

completely driven off (?).


5. Dissolve potassium chlorate in hot water, and allow to stand and cool (?).
6. To a
plate, until the liquids are

portion of the cobalt chloride solution, add a solution of soda; boil. 7.


8. Wash the precipitate "until pure water runs
to settle and filter.

Allow

through the

filter (?).

9.

Heat the

filter until

CHAPTER

perfectly dry.

II.

GENERAL PRINCIPLES.
Changes in matter.
a glass rod with a piece of cloth, then touch particles of paper
2. Through an insulated spiral of stout copper wire pass a
with it (?).
(i)

Rub

i.

current from two Bunsen

cells.

Place a piece of wrought-iron

a nail

inside the spiral, and bring iron filings in contact with it.
What happens? Interrupt the current and note the result ; repeat. 3.
Heat a platinum wire in the non-luminous flame ; is there any change ?
will

answer

What

is

the effect of removing

it ?

Are the

original properties of the substances in the above experiments


altered, after the action of the forces of electricity, magnetism and heat
has been stopped ?
4. Mix intimately four parts, by weight, of finely powdered sulphur
with seven parts of very finely divided iron (filings). Pass a magnet over
a portion of the mixture.
Another portion treat with carbon disulphide in

GENERAL PRINCIPLES.

II

Then heat the remaining portion in a tube over a gas flame.


Note carefully what occurs in each case. Powder the mass
FIG a
Can you
resulting from the last operation in a dry mortar.
extract from it any iron with a magnet, or dissolve out any
sulphur with carbon disulphide? What inference do you draw
a test-tube.

from the

facts

observed

Decompose water

5.

in

Hofmann's

The water should be acidapparatus by an electric current.


ulated with sulphuric acid to make it a conductor of elec-

current from four to six Bunsen cells is required.


the gas, of which a larger volume has collected, apply a flame, and to
6. Heat oxide of mercury in a tube of
the other a glowing spark (?)

tricity.

To

hard glass (Fig. 2). Apply the spark test (?).


7. Rub some sulphur
and mercury together in a mortar (?) 8. Heat sugar in a dry test-tube,
at first gently, and then more strongly.
Note color and odor. 9. Mix
Is there any action ?
What
dry soda and tartaric acid in a mortar.
occurs when you add water ? Point out in what respect the changes
involved in experiments 1-3 differ essentially from those in 4-9.
By
what general names can you distinguish the two different kinds? With
which does chemisty concern itself? Define chemistry.

Through what agencies have the results been obtained in experiments


4-9 ? Has any gain or loss of matter occurred in any of them ?
(2) The products resulting from 5 and 6 cannot be further simplified,
*.

e.,

decomposed into dissimilar substances.


and red oxide of mercury ?

They

are elements*

What

are water
i.

Dissolve in a

little nitric

acid, the black

powder obtained by heating

an intimate mixture of powdered sulphur and copper

filings. f
Evaporate the solution nearly to dryness, take up in water
and filter. What remains on the filter ? Place the filtrate in

a beaker, dip the platinum electrodes of a battery (one or two


Bunsen cells) into it (Fig. 3), and allow the current to act for
ten minutes.

What do you

observe upon the platinum

FIG. 3 .

~*"

foil,

forming the negative pole ? What changes have the copper


and the sulphur undergone in this experiment ?
(Study pp. 18-27, i n Richter's Chemistry.)
(3) Metals and non-metals.
(See Richter, p. 20.)
* The

instructor should here develop the idea of element

more

fully.

f A better substitute would be finely divided copper such as may be obtained by the
reduction of black cupric oxide in a current of hydrogen gas (see page 14).
;

EXPERIMENTS IN GENERAL CHEMISTRY.

12

CHAPTER

III.

HYDROGEN.

H.

and pour

(i) Put several pieces of granulated zinc into a test-tube


What occurs?
dilute sulphuric acid upon them.
FlG

(2)

The

Arrange the apparatus shown

in

Fig.

4.

should contain about 15 grms. of Zn,


and dilute
is poured
2 SO 4
through the funnel
flask

tube.

When

all

the air in the apparatus has been

displaced (ask for precautions /) collect six


tubes full of the gas over water.
(3)

What

are

its

properties

Will

it

test-

burn

Support combustion? Is it lighter than air?


i. To learn what becomes of
hydrogen when it burns in air,
(4)
The gas is led from the evolution flask
arrange apparatus as in Fig. 5.
A, into a bottle containing concentrated 2 SO 4 and then passes through
a tube filled with pieces of CaCl 2
The gas which escapes is free from
moisture. Burn it under a cold glass jar. What do you obtain ? 2. Fill a
small flask with a mixture of one vol. of H and five vols. of air ; cork
invert the flask several times to mix the gases; wrap a towel around it and

bring

its

mouth

to a flame.

FIG. 5

Result

(5) Hydrogen
the action of Jf2

not the only product of

is

SO

itpo?i

Zn.

Pour some of the liquid remaining in


the flask, in which H was generated, into
a porcelain dish.
Evaporate to about
one-third of the original bulk ; allow to

You

stand several hours.

cover that the solution


crystals.

These are zinc sulphate or white

vitriol

will

is full

salt,

now

dis-

of colorless

ZnSO

-j-

7H

O.

Write the equation of the reaction.


(6) Determine the weight of
generated by a given weight of Zn.
FIG. 6.
A piece of Zn (not more than .02 grm.) is accurately
weighed, and placed under a funnel in a beaker (Fig. 6).

The
tire

latter is

H,SO 4

is

then nearly

filled

with water, so that the en-

under the surface. A test-tube containing dilute


lowered over the stem of the funnel.
Hydrogen

funnel

is

When
appears and collects in the tube.
appeared,* transfer the tube containing the
holding water.
This

may

all

the

Zn has

dis-

H to a larger vessel,

Measure the volume of the gas by marking

be hastened by bringing a spiral of platinum wire in contact with the Zn.

HYDROGEN.

the tube where the inner and outer levels of water are even, and then
weighing or measuring the quantity of water that it will hold to that
mark.
Note the temperature of the water, and the height of the barometer.

The weight of

found by multiplying the vol. by the wt. of


Before
this can be done, however, it is necessary
cc., /.<?., .0000896 gr.
to reduce the volume of the gas to o C. and 760 mm., as the above value
the

is

has been determined under these conditions.

temperature, and p

and

To

If v

= pressure, then
+

(i

.000x5896

calculate the quantity of

Zn

=r volume observed,

X p
X

at)

= .003665.*

necessary to generate a

FIG.

7.

H, we say

unit of

Wt

of

H Wt of
:

Zn

x.

x here stands for the equivalent weight of Zn.


The equivalent weights of some other metals, such

as

Fe, Cd, Mg, can be determined in the same manner. Magnesium gives the most satisfactory results.
(7) Decompose water by electrolysis and test the products.
(8)

Take

a small piece of sodium, wrap


under the mouth of a test-tube
with water, and inverted in water

it

in

paper and place

it,

with

forceps,
filled

(Fig. 7) contained in a dish. Repeat this


until the test-tube is filled with the gas.

Test

it

for

H.

What becomes

of the metal

Write

the reaction.
(9) Construct the apparatus
Fig.

shown

in

8.

Water is heated to boiling in the flask


A, and the steam led over iron filings or
of hard

glass.

wire, heated to redness in a tube


Care must be taken to prevent steam from condensing in

any part of the tube.


for H.

Collect the escaping gas over water.

* Tension of
aqueous vapor

is

here neglected.

Test

it

EXPERIMENTS IN GENERAL CHEMISTRY.


Is

the iron changed

Equation

(10) Into a weighed tube


of hard glass (6-8 inches in

FIG

length) place a weighed quantity

oxide

(1-2 grams) of cupric


connect the tube with
;

a CaCl 2 -tube of

known weight

Pass a current of dry


over the CuO and heat.

(Fig. 9).

After the change is complete, cool and determine the loss in weight of
tube -)- CuO, and the gain in the CaCL2 tube.
Explain the reaction.
Problems.
i. How much
can be obtained from Zn and 299 grms.

of

H SO
2

2.

How much Zn

and H-jSO^ are necessary

to furnish

100

H ? 3. Suppose you have found that .015 grm. of Mg yield


H at 20 C. and 750 mm., what the equivalent weight of
cc.
of
15.2
that metal ?
4. How many cc. of H can be obtained from 2 grms. of
Na and water? 5. How many grms. of H O can be decomposed by
grms. of

is

grms. of Fe; by how much is the weight of the latter increased


10 grms. of CuO will yield how much Cu upon heating in H?
Give a brief summary of what you have learned about H.

6.

(Study Richter, pp. 39-47-)

CHAPTER
FIRST

IV.

NATURAL GROUP OF ELEMENTS CHLORINE, BROMINE,

IODINE,

FLUORINE.

CHLORINE.
(i) Into a test-tube put

happens both before and

MnO

Cl.

Note what

and concentrated HC1.

after heating.

(2) Use apparatus (shown in Fig. 10) for preparing


be in the
The
2 should
larger quantities of Cl.
form of small lumps (not powder.) Heat the mix-

FIG.

MnO

ture gently, pass the Cl through a small quantity of


it either
by downward displace-

water and collect

ment or over warm water.


Write the reaction.
liberated ?
(3)

ment?
ble?

4.

Does

it

i.

How many

What
2.

is

molecules

atoms of Cl are

the normal condition of this ele-

Is it lighter

support combustion?

How many

than air?

3.

Is

it

inflamma-

NATURAL GROUP OF ELEMENTS

FIRST

To

obtain answers to these questions,


as

proceed

5 bottles

fill

throw a

15

5 test-tubes with

dry Cl, and

Cover them with

glass plates.

under H.

(4) Again

Into

fill

CHLORINE.

with the dry gas.

little

pulverized antimony.
Into 2 carefully introduce a piece of phosphorus.
Into 3 insert tissue paper moistened with oil of turpentine. *
Into 4 introduce colored flowers.

Into 5 pour a little litmus solution.


What are the results ?
(5) Fill a small-sized flask one-half with chlorine, the other half with

Wrap

hydrogen.

mouth

a towel about the flask and apply a flame to

its

open

Care.

(?).

(6) Invert a bottle filled with Cl over water saturated with the same
What follows in the course of a few hours' exposure to sunlight ?
gas.

Can you account

for results in

the gas be collected over

experiments (4), (5) and (6)


water ?

(7) Determine the weight of a litre of chlorine.

shown

as

In the evolution-flask

place

Arrange apparatus

a mixture of equal

Add

and manganese dioxide.

salt

Why should

n.

in Fig.

weights of

warm

sul-

phuric acid, previously diluted with its own volume


of water (pour the acid into the water ).
Heat
!

evolved, and dried by passing


through concentrated sulphuric acid, after which it
led into the perfectly dry flask c.
When this is

Chlorine

gently.
it

is

is

which you ascertain by the color of the gas in


slowly withdraw the tube and cork the

filled,

the neck,
flask

at

meter.

once.

Weigh

Determine,

the

flask.

Read

the

barometer and thermo-

also, the weights of the flask filled with air and with

water.

Calculation

Capacity of

flask,

Temperature,

Pressure,

Flask

filled

with

air,

Cl,

Wt. of a

litre

of

"

It is well,

paper.

when

*- 2 93

air,

w
w'

grm.

....'.'.....

Cl,

the turpentine

is

old, to gently

warm

it,

and then saturate the

tissue

EXPERIMENTS IN GENERAL CHEMISTRY.

The weight of

the air filling the flask

(i

ence between
this

from

and

this

is

The remainder

w'.

C. and 760

of the Cl to o

11
^
r
and the weight of
i

How much

T^
litre,

heavier

is

is

WX

= -

one

litre

Write the reaction involved


Problems.

MnO

litres

i.

and HC1?

of Cl

3.

How many

The

the weight of the vacuous flask.


Subtract
the weight of the Cl, (W). Reduce the vol.

mm. (see under H)


x

xP x OOI2 93
+ .00367 t) 760

a
is

it is

ax

IOOO

of Cl than an equal vol. of

in the
litres

+ .003671)760

above method

H?

for preparing Cl.

of Cl can be obtained from

What weight of salt is


How many pounds of sodium
2.

required

kilo of

to prepare

100

sulphate and manganese

sulphate will be formed in the preparation of 100 litres of chlorine gas?


4. Calculate the number of grams of Cl that 2 litres of water will abthe latter takes up twice its volume of Cl
your deductions from the above experiments on Cl.
sorb, provided

Write out

(Read Richter, pp. 49-52.)

HYDROGEN CHLORIDE.

HC1.

Quickly cover
(1) Repeat the explosion of equal vols. of Cl and H.
Does the latter rise ?
the mouth of the flask, and immerse it under water.
Put a drop of the liquid on the tongue and note the

any change?
(2) The product of the union of H and Cl

called hydrogen chloride.


acid upon salt, thus:

It is usually

Add some

2NaCl
NaCl +

SO 4

The apparatus employed here

is

a colorless gas.

Na2 SO 4

= HC1 -f NaHSO

It is

the same as that used for making Cl

(Fig. 10).

(3) Determine the properties of

is

prepared by the action of sulphuric

+ H S0 = 2HC1 +

or, better,

taste.

Is there

blue litmus solution.

HCl as

under

H and CL

What new property

Fill a long dry glass tube with the


appears here ?
it
into
a
basin
containing water colored blue with
gas, and quickly bring
What happens? What does HCl gas yield on dissolving in
litmus.

water

by the action of Na upon water, it was


(4) In the preparation of
observed that the liquid became soapy to the touch, and acquired the
To it add
Prepare such a solution.
property of turning red litmus blue.
a few drops of litmus, and then an

HCl

solution

(gradually) from a

NATURAL GROUP OF ELEMENTS

FIRST

HYDROGEN CHLORIDE.

17

burette, until the blue color just begins to turn.


Evaporate the resulting
and
to
Dissolve
It
recrystallize the product.
crystallization.
liquid

appears in cubes, and has the taste of common salt.


We say
does not affect either red or blue litmus.

It
FIG. 12.
it is

The substance is chloride of sodium


What is a salt? An acid? A base ?
How can you obtain HC1 and Cl from NaCl ?
(5) Burn Hin an atmosphere of Cl, and Clin hydrogen.
neutral in reaction.

or

common

salt.

(p. 14) and


Into this introduce a burn-

Generate chlorine as already described


collect

in a large cylinder.

it

Does it continue burning jet of hydrogen (Fig. 12).


What
is
the
?
of
the flame ?
To show the combustion of
ing
appearance

Cl in

arrange apparatus as in Fig. 13.


determine the weight of a litre of

To

(6)
exactly as under chlorine.

HCl, proceed

FIG.

13.

HCl

(7) Determine the composition of


by volume.
i. Fill a perfectly dry and graduated tube with

HCL

Close

the open end with

the thumb, and opening the tube for a


moment, quickly pour in about 10 cc. of sodium amalgam
Close the tube at once with the thumb,
(see sodium, p. 36).

and shake

slightly moist,

well.

Invert the tube in a large

beaker of water, and remove the thumb.

The amalgam

will

and the latter will rush up into the tube,


drop
it
half
full.
Immerse the tube so that the water
filling
nearly
in it and that in the beaker are on the same level.
This is
done to measure the hydrogen under atmospheric pressure.
into the water,

Read

the residual volume of the gas and measure the volume

of the mercury.
Calculation

Capacity of tube,
Vol. of mercury,
Vol. of

(8) Add a solution of HCl to solutions of silver nitrate ; of mercurous


nitrate ; and of lead acetate.
What do you observe in each case? Boil

the precipitate formed in the lead solution with water.


result.
3

Cool, and note

EXPERIMENTS IN GENERAL CHEMISTRY.

i8

BROMINE.
(1) Allow a drop of bromine

to

fall

Br.

upon a heated watch

glass

cover

What is the color of the vapor ? Dissolve one


quickly with a beaker.
in
of
bromine
each
of
the following solvents contained in test-tubes
drop
it

alcohol,

water,

ether, carbon

relative solubilities,

(2)

disulphide, and chloroform.

and the color of each

Note the

solution.

Pass Cl through an

i.

What happens?

2.

aqueous solution of potassium bromide.


one portion of the product add a few drops of

To

CS 2 and agitate the mixture what is


3. To another portion of the solution,
;

FIG. 14.

free

Br,

Result

the result ?

containing

add a few drops of a starch solution.*

(4) Devise

a method

for

preparing bromine

from KBr.
(5)

Prepare hydrobromic

In a small

acid.

flask

grams of amorphous phosphorus with 4


of
from a funnel, provided with
2 O, and
grams
a stop-cock, gradually allow 20 grams of Br to run- in.f
The gas is purified by conducting it through a U-tube, containing moistened pieces of phosphorus and glass (Fig. 14), and led into water to
cover

obtain the aqueous solution.


(6)

Add

do the

aqueous

resulting

HBr

to solutions of

bromide precipitates

AgNO HgNO
3,

differ

much from

and Pb(NO 3 ) 2

the corresponding

chlorides ?

IODINE.
(1)

i.

I.

Place an iodine crystal upon a warm plate, and note color of


2. Test the solubility of iodine in the same solvents as were used

vapor.
with bromine

what are the colors of the resulting solutions?

Test the resulting liquid


Pass Cl through a solution of KI.
(2)
2. Repeat
with ether, carbon disulphide and starch solution (as with Br).
Avoid excess of Cl as
this experiment, substituting Br- water for the Cl.
i.

Br

well as

(?).

What

conclusion do you draw from these experiments relative to the


affinity of the halogens for potassium ?
* The starch

One gram
solution necessary for this purpose can be prepared as follows
It is
well ground in a mortar, with very little water, to creamy consistence.
then poured into 200 cc. of boiling water. Allow to subside, decant the clear supernaof starch

tant liquid

f As

and use

it is

ponding

is

it

for the test.

upon a balance, calculate the volume corresand measure out the same in a cylinder.

rather difficult to weigh bromine

to the weight given

SECOND NATURAL GROUP OF ELEMENTS

OXYGEN.

19

(3) Pass hydrogen sulphide gas (H 2 S) into 50 cc. of water, and add
powdered iodine till the brown color no longer disappears. Warm, filter
The product is what ?
(?) and distil the filtrate.

How

is

gaseous

HI

prepared

(4) Precipitate solutions of silver nitrate (AgNO 3 ), mercurous nitrate


(HgNO 3 ), lead nitrate (Pb(NO 3 ) 2 ), and mercuric chloride (HgCl 2 ) with

Note

KI.

result in

each case.

FLUORINE.

Fl.

(1) In a lead dish (or platinum crucible) place i gram of pulverized


fluor spar (CaFl 2 ).
Add cone. 2 SO 4 ; cover the dish or crucible with a

watch-glass coated with paraffin, through which some characters have been
drawn with a fine point. Heat gently for a few minutes.

What do you observe on removing the paraffin ?


(2) Can you liberate Fl from a fluoride?
i. How much NaBr, H SO 4 and MnO
Problems.
duce i cu. metre of Br vapor at 20 C and 745 mm. ?
2

HI

are necessary to pro2. What per cent, of

does a liquid contain, which represents a solution of 50 litres of the


i litre of
2 O?
3. 10 grms. of CaFl 2 will give what weight of

gas in

HF1 ?

How much

salt and sulphuric acid will be required to prepare


6 litres of muriatic acid of sp. gr. 1.17?
What volume would the HC1
in these six litres occupy at 735 mm. pressure and
5. What is
the percentage of hydrochloric acid in a solution of which 17 cc. dis4.

22C?

solve exactly 2 grams of metallic magnesium ?


hydrogen liberated at 760 mm. and o ?

CHAPTER

What

is

the

volume of

V.

SECOND NATURAL GROUP OF ELEMENTS OXYGEN, SULPHUR,


SELENIUM, TELLURIUM.

OXYGEN.

O.

Weigh the hard glass tube a (Fig. 15), and intro(1) Preparation.
duce a weighed quantity (about .5 grm.) of red oxide of mercury. Ignite
strongly; collect the liberated gas, and measure it.
Weigh the tube
i.

with the residue.


(2)

What

are the products of the ignition ?


Mix equal parts of KC1O 3
gas, as follows
heat in a tube of hard glass or small retort.

Prepare more of the

and pulverized

MnO

Collect the gas in bottles over water (Fig. 15).

EXPERIMENTS IN GENERAL CHEMISTRY.

20
Into No.
result.

Add

lower a piece of ignited sulphur on an iron spoon.


water after the combustion (?).
Into No.

FIG. 15.

Note

introduce a small piece of burn-

ing phosphorus (care !). Proceed as in No. i.


Into No. 3 introduce ignited charcoal. Treat

Add now a few

as before.

drops of blue litmus

to the contents of each bottle.

Any change?

bottle No.

4 introduce a fine watch


spring, previously heated at one end and
dipped into powdered S. Result ?
Has
Is oxygen heavier or lighter than air?
Into

odor

color, taste, or

it

Will

support combustion ?
other methods can be used for preparing O

burn

it

Does

it

What

(3) Determine

the weight of a litre of O.

Arrange apparatus shown in Fig. 16; a


tube of hard glass, whose weight is known

FIG.

contains a weighed amount of

The

grm.).

bottle

is

filled

The

and d a beaker.

clip

KC1O

is
;

a
it

(about 0.3

with water, b is a
con-

exit tube should

tain water as far as clip b at the

beginning of the

the clip, heat a to bright


redness, and receive the water displaced by the
When no more gas is evolved, cool ; allowing the rubber tube
in d.
Some of the water will be drawn back
to dip under the water of the jar.

experiment.

Open

into the bottle (?).


Measure the volume of the water in d. Note the
the
of
air, and the height of the barometer.
Weigh a, contemperature

taining residue (KC1).


Calculation

Weight of the tube,


Weight of KC1O 3 and tube,
Weight of KC1O3
Volume of H 2 O collected,

b
b

Barometric pressure,

Temperature,

Aqueous tension at t, ...


Weight of KC1 and tube
V
Vo_. X(P
"(I

(b

KC1
KC1O

Dissolve the residual


silver (?).

How

does

P')

+ .003670x760

c)

iooo

and

in water,

.Vo

and

behave under

to

its

like

solution

add

conditions?

nitrate of

SECOND NATURAL GROUP OF ELEMENTS


(4)

Give a summary

54
4.

21

your work upon O.

How much O, by wt. and vol., can be obtained from


of
HgO? 2. Heat will expel what vol. of O from 2.45 grms.
grms.
KC1O ? 3. How much HgO is necessary to yield i cu. d. m. of O ?
How many times is O heavier than H ?

Problems.
of

of"

WATER.

i.

OZONE.

O3

(i) Pour water on clean pieces of phosphorus to half cover them ;


invert a large, clean jar over this and allow to stand for several hours'.

For this purpose use paper impregTest the air under the jar for ozone.
nated with a mixture of starch paste and potassium iodide. What occurs ?

(Read Richter,

p.

85-89:)

COMPOUNDS OF OXYGEN AND HYDROGEN.

WATER. H
(1)

Arrange the

AgNO

Does

3.

Apply

all

it

Note

its

taste

and odor.

leave a residue

What

upon evaporation
it on litmus?

O.

distillation apparatus (Fig. 17)

cc. of distilled water.

with

and prepare about 100


Test

it

FlG I7
.

for chlorides

action has

these tests to a natural

water (except rain).


i.

(2)
ter in a

meat

Heat a

dry

in the

little

test-tube.

vegetable mat2.

same manner.

fully heat crystals

Heat
3.

fresh

Care-

of zinc or copper

sulphate in a test-tube. What happens in these experiments? 4. Expose


clear crystals of sodium phosphate, on a watch-crystal to the air.
5. Do
Results ?
the same with pieces of calcium chloride.

Determine the quantitative composition of water.


follows from the experiment of
under
of
described
oxide
H.
reducing
copper
(3)
1.

The composition of water by weight

2.

The

relative

volumes with which

and

determined either by analysis or synthesis.


formed in electrolyzing water.
3.

Fill a

unite to form water, are

The former

has been per-

eudiometer (Fig. 18) with water. Through a rubber tube


cc. of O and then a like volume of H.
(If the eudiome-

admit about 50

Close the open


not graduated, mark these with rubber bands.)
end with your thumb, leaving some air to serve as a cushion beneath it,
and pass the spark. Remove the thumb, and pour in enough water to
ter is

EXPERIMENTS IN GENERAL CHEMISTRY.

22

make
tion

What
the levels equal in both limbs.
What is the residual gas ? Test it.

the amount of the contrac-

Determine the weight of a

(4)

FIG. 18.

is

struct apparatus

shown

C is

with a cork.

in Fig. 19.

litre

Conof steam,
flask a is closed

The

a vessel containing melted paraffin.

small glass tube is weighed and filled with water (not


more than .02 grm.). Heat the vessel Cwith a Bunsen

burner until the temperature of a is constant (?).


Now
drop the tube containing the water through the mouth
flask (the bottom of which should be protected
with a layer of asbestos) and quickly re-cork. When
of water in the graduated tube ceases, read the volume of gas,

of the

the

fall

FIG.

(1)

and note the temperature and pressure of the air.


The calculation is analogous to that used under O.
(5) Perform experiment 2, p. 100 in Richter.
How many volumes of steam result from the combination of 2 vols. of H and i vol. of O?
How would you deduce the molecular formula of
water from the preceding experiments ?

19.

Add

What does

moist hydrated barium peroxide to cold dilute


the filtrate contain

H SO
2

4.

Filter.

(2) i. Add a solution of KI, containing starch, to a portion of this


Ferrous sulphate hastens the reaction.
2. Cautiously add a
liquid (?).
dilute solution of potassium permanganate to another portion (?).

COMPOUNDS OF OXYGEN AND CHLORINE.


(1)
it

Make

a dilute solution of caustic potash, and conduct chlorine into


is no longer absorbed.
Treat one portion of the product

until the latter

with HC1, and another with


What results ?
2 SO 4
After the slaking
2 O.
(2) Mix 10 grms. of quicklime with 25 cc of
FIG. 20.
is finished, conduct Cl into the mixture until it is no
.

longer absorbed.

Add HC1

to

one portion and H-jSO*

to a

second

portion.

What

is set

free ?

Does

it

bleach

(3) Pass Cl into a hot concentrated solution of

KOH

ceases to be absorbed (Fig. 20). What separates


Will it give off
Recrystallize the product from water.
till it

upon cooling?

SECOND NATURAL GROUP OF ELEMENTS

SULPHUR.

23

Try the action of HC1 upon a crystal. Allow a drop of


upon a small crystal and warm gently (?). Care
Observe carefully the behavior of KC1O 3 upon heating (?).

upon heating?

cone. H-jSOi to

fall

SULPHUR.

S.

(i) Place a few grams of powdered S in a dry test-tube, and heat


Observe and describe the changes which occur.
gradually.

(3) Dissolve a

(4)

little

CS and

S in

allow to stand

till

the liquid has

What remains?

evaporated.

Determine the

introduced into a

sp. gr.

of S (Fig. 21).

Water, previously boiled is


neck of the flask should

that the

It is essential

flask.

the flask, then place an additional 10 grm.


the
right-hand pan of the balance and small pieces
weight upon
of S upon the left-hand pan, until the pointer is again in the
Now introduce the S into the flask. Carefully remove
middle.

be narrow.

Weigh

FIG. 21.

water above the mark and re-weigh the flask with its contents.
The loss in weight will represent the weight of a volume of water

The latter divided by the former


equal to that of 10 grms of S.
is the specific
gravity of the sulphur.
(5) Prepare the monoclinic modification of S by melting about 10 grms.
of the ordinary variety in a covered Hessian crucible.
Cool and as
soon as a solid crust has formed upon the surface, pierce it and allow the
;

Note the shape of the

liquid portion of the contents to run out.


crystals upon the sides of the crucible.
still

(6)

To

above 230

obtain the plastic variety, heat 10 grams of S in a test-tube


C., and pour the mass into cold water.

Test the solubility of the product in


several days.
Does it change ?
(7)

To

CS

a strong solution of yellow

Preserve a portion of

potassium sulphide, add

What

are the properties of the separated sulphur


Give a brief outline of the element sulphur ;

it

for

HC1.

compare

it

with the pre-

viously studied elements.

SULPHUR AND HYDROGEN.


Hydrogen sulphide is formed with difficulty from its elements, but
readily obtained by the action of acids upon sulphides, thus
(8)

is

FeS

+H

SO 4

The apparatus

= FeSO + H
4

to be used

is

S or Sb 2 S 3

6HC1

2SbCl 3

3H 2 S.

the same as that employed in preparing

hydrogen.
(9)

What

are the properties of

Is it soluble in

water

Does

it

EXPERIMENTS IN GENERAL CHEMISTRY.

24

What

?
Hold a porcelain plate in
Pass the gas into solutions of chromic acid, permanganic acid, and ferric chloride. What changes are observed ? How
do these last-named reactions show its reducing power? What happens.

burn

are

its

products of combustion

the flame; what results

to the aqueous solution of the gas when exposed to the air ?


What action
has the aqueous solution upon litmus? To what class of compounds does
it,

therefore,

(10) Pass

SbCl 3 Pb
,

Can

belong?

HS

through solutions of the following

(NO

3) 2 ,

AsCl 3 and Zn (C 2 H 3 O 2 ) 2
,

Note

salts, viz.

CuSO

4,

results carefully.

manner? (See Chap. II,


i.)
Determine
the
(n)
composition of hydrogen sulphide.
Into a bent tube of hard glass, filled with mercury,
sulphides be prepared in another

Place a
(Fig. 22), introduce dry hydrogen sulphide.*
in
of
tin
the
bent
and
heat
it.
Is the
portion,
piece
volume of the gas changed after the experiment, and

what becomes of the piece of

tin ?

Test the gas re-

maining in the tube. Do your results enable you to


deduce the molecular formula of H 2 S ? (See Richter,
Write a
2 O.
3d ed., p. in.) Trace the similarity between H 2 S and
summary of your experiments on H 2 S.

SULPHUR AND CHLORINE.


(12)
FIG. 23.

Prepare this compound by conducting


Sulphur Monochloride.
dry chlorine over molten sulphur. The product which distils
over is collected in a dry test-tube, kept cold by immersion
in ice water.
2. Redistil the product.
Determine its boiling
point in an apparatus similar to that pictured in Fig. 23.
Note the color and odor of the product. Expose some of it
to the air on a watch-glass.
Add water to another portion
in a test-tube.
Note carefully what happens.
Write the reaction, and examine for all the products.

contained

SULPHUR AND OXYGEN.


(13) Burn sulphur in the

air.

Result?

Burn FeS 2

are the properties of the resulting compound ?


It
(14) Fit a small flask, as indicated in Fig. 24.

is

in the air.

sulphur dioxide

What

SO

Place copper turnings

Warm. Is the
2 SO 4 (strong) through the funnel tube.
the
same
as
that
in
water? Has
obtained
in
Is
it
soluble
product
13?
the aqueous solution the same properties as the gas?
2. Pass some of
in

it,

then add

The

instructor should perform this experiment.

NITROGEN GROUP

NITROGEN.

25

the gas into solutions of potassium dichroraate and potassium permanganate acidulated with
2 SO 4
Fir 24
Repeat these experiments

,.

What
with the aqueous solution instead of the gas.
happens in each case? 3. Test the aqueous solution of
SO 2 with litmus. What is this solution commonly called ?
4.

Fill a

Note the
(15)

many

dry

jar

with

SO

What

is

Na SO
2

introduce colored flowers.

can

it

3.

What

form

How

would you desig-

Add HC1

salts ?

follows?

How

acid?

the formula of sulphurous

series of salts

nate the different sodium

of

gas

result.

to a solution

the

Evaporate

solution

to

What is it? Write the reaction.


dryness and examine the residue.
SULPHUR TRIOXIDE SO 3 and SULPHURIC ACID H 2 SO 4 (Read Rich.

ter, p. 189).

(16) i. Prepare sulphuric acid as described in Richter, p. 191. Study


the product carefully. 2. Dilute a portion of it with water ; what happens ?
2. Test a portion of this diluted solution with litmus (?).
4. Another
and evaporate. What is the residue ?
portion neutralize with
Does it contain any S? Prove this. 5. Add BaCl 2 to a third portion of

NaOH

the solution.

chloric acid

How many

(17)

(NH

What is the precipitate ?


6. What is the action

Is

it

soluble in water or in hydro2 SO 4


upon wood or

of strong

Explain the cause of this action.

paper?

4) 2

SO

4,

series of salts

can sulphuric acid

Na SO 4 NaHSO 4 and CuSO 4


2

CHAPTER

form.

Prepare

(Read Richter, pp. 189-200).

VI.

NITROGEN GROUP NITROGEN, PHOSPHORUS, ARSENIC, ANTIMONY

AND BISMUTH.

NITROGEN.
(i) Preparation.

i.

phosphorus and ignite


FIG

25.

FIG 26

it

N.

In a dish swimming on water place a piece of


invert a beaker glass over it (Fig. 25).
What
;

becomes of the P ?

When

the latter has ceased

burning, restore the level of the water,


the decrease in the volume of the air.

and note
Test the

residual gas with a burn ing taper.


2. Heat gently
in a small flask or retort a mixture of i part
2,
i

pt.

NH C1,
4

pt.

K Cr O
2

collect the gas over water.

7,

and 3

KNO
H O;

of

pts.

Fill five bottles

with

this gas.

(2)

Has

it

color, taste,

odor?

Does

it

burn or

EXPERIMENTS IN GENERAL CHEMISTRY.

26

support combustion ?
with other elements?

heavier than air

Determine the weight of a

(3)
flask

Is the gas

is

fitted, as

shown in Fig.
and insert

litre

Does

of nitrogen.

Pour about 30

26.

it

unite readily

round-bottomed

cc. of

water into

the rubber cork to the mark.

it,

Boil the

FIG.

water, while the clip is open, until all the air has been
Steam should be allowed to
expelled from the flask.

Now close the tube


escape for about five minutes.
with the clip, and remove the flame.
Cool and
flask.
Read the temperature and barometric pressure in the balance-room.
Connect the flask with the tube, b, of the aspirator,

weigh the

clip

is

The
containing N, and arranged as in Fig. 27.
rubber tube, a, is made to dip under water, and the
Now raise the
gradually opened, allowing N to enter the flask.
vessel containing the water into which the rubber tube

FIG. 28.

dips, so that the water in

in the aspirator.

and open the

it is

Close the

at a higher level than that

clip.

Disconnect the

flask

clip for a

moment, to establish atmospheric


Weigh. The calculation is identical

pressure in the flask.

with that given for O.

Wnat
of

is

and

the ratio between the weights of equal volumes

H?

(4) Is air a chemical

compound ?

How

would you determine the weight of a litre of air ?


Determination
i.
of the Oxygen in Air by the Pyrogallate Method,
(5)
At
the atmospheric temperature and pressure
FIG. 29.
measure off 50 cc. of air in the Hempel burette,
shown in Fig. 28. Connect this at c with the
capillary of a

Hempel's compound pipette (Fig.

29) containing an alkaline solution of pyrogallate


of potash.
Open the clips and transfer the air to
the pipette

by

raising the tube, a.

When

this is

capillary of the pipette is filled with water from b,


close the clips again. Disconnect the apparatus. Shake

accomplished, and the

and
Reconnect pipette and

the pipette for several minutes so as to bring gas

absorbent in intimate contact.


burette,

and

force

the

residual

gas into the latter.


read the volume.

Restore atmospheric pressure and


What does the loss represent ?
2.

Explosion Method.

To 40

cc. of air

contained in

NITROGEN GROUP

AMMONIA.

27

Pass this mixture into the Hempel


the burette add 40 cc. of pure H.
explosion pipette shown in Fig. 30. Close the stop-cock, d, and the clip,
c, then connect the platinum electrodes with an inductor and pass a spark

What
much

Measure the volume of the gas remaining. How


takes place ?
of the contraction was due to O ? What is the composition of the

gas after the explosion

(Study Richter, pp. 116-125.)

NITROGEN AND HYDROGEN.


AMMONIA.

Heat an intimate mixture of finely powdered ammo(6) Preparation.


nium chloride and caustic lime in a flask conduct the evolved gas
through a tube filled with small pieces of lime, and collect it in jars or
;

test-tubes over mercury.

What is the object of the lime in the tube?


the gas by passing it through
CaCl 2 ?
2 SO 4 or
lected over mercury ?

ammonia

(7) Is

Does

combustible?

gas

it

Why can you not dry


Why should it be colFIG. 3 i.

FIG. 32.

NH

i. Conduct
3 through
support combustion ?
a glass tube, and insert this into a wider tube

filled

with oxygen (Fig. 31).

The ammonia

will ignite

gas

Apply a flame.
and continue to

Heat concentrated ammonia water in


a beaker until there is an abundant disengagement of gas, then conduct a rapid current of
oxygen through the liquid, and lower a glowing
burn.

2.

spiral of

platinum into the beaker (as in Fig. 32).

What happens

Note the odor of


water

NH

(caution

?).

Is

it

lighter than air?

Soluble in

(8) Prepare

What are
Add red

an aqueous

its

solution of

ammonia.

properties
litmus to some of the solution (?), and then neutralize carefully with dilute HC1.
Evaporate to dryness.
Compare the product
with the ordinary
Test it for Cl (?).
Heat a little of it with
4 C1.

NH

sodium hydroxide (?). Heat another portion on a platinum


(9) Determine the weight of a litre of NH^

foil (?).

Fill a dry flask with the gas by upward displacement, and proceed
What is the density of
S ?
exactly as under chlorine.
To determine the quantitative composition of
3
perform experi-

NH
NH

ments T and 2 on pp. 130 and 131, in Richter.


Write out summary.
(Read Richter, pp. 125-131.)

EXPERIMENTS IN GENERAL CHEMISTRY.

28

NITROGEN AND THE HALOGENS.


(n) Pour a saturated alcoholic solution of iodine into strong ammonia
Collect the precipitate on a filter and wash it with water.
Weuer.
Open
the moist filter; tear it into small pieces and spread these on a board.
After they have become dry, touch them with the end of a rod (?).
Ask

for instructions

(Read Richter, pp. 132-133.)

NITROGEN AND OXYGEN.

N O.

(12) Hyponitrous oxide

i.

add a

Place about 5 grms. of

ammonium

and apply heat. Collect the


2. Test it with a
product over warm water.
glimmering chip 3. with
with
burning phosphorus 4.
burning sulphur. 5. Mix equal volumes of
this gas and of H, and apply a flame.
What other gas does it resemble
nitrate in a small retort

little

water,

in

its properties?
(Read Richter, pp. 212-213.)
i.
Pour dilute
(13) Nitric oxide NO.
copper turnings contained in an evolution flask.

HN0

(sp.

gr.

1.2)

upon

Cool, and allow the

red fumes, which form at first, to escape ; then collect the colorless pro2. What occurs when this
duct over water.
gas comes in contact with
the air?
Is it the O or the N of the air that acts upon the
gas? 3.

NO

How can
be disgiven under (12) to this gas (?).
tinguished from oxygen ? 4. Fill a cylinder with NO, and add a few
drops of CS 2 shake well and bring a flame to the mouth of the vessel (?).
into a strong solution of ferrous sulphate. What
5. Pass a current of
Apply the

tests

NO

boiling

become saturated with the gas heat it to


Pass the gas into a solution of potassium permanganate (?).

After the solution has

occurs?

(?).

6.

NO

(14) Nitrogen trioxide

Nitrous

Add HNO

(Read Richter, pp. 205-206.)

8.

(Richter, p. 206.)

i. Heat 10 grams
2
(15) Nitrogen tetroxide, N 2 O 4 and dioxide,
of dry lead nitrate in a test tube ; condense the escaping vapors in a
well-cooled receiver.
What are the vapors, and what is the condensed

NO

liquid

Note the

color.

What

2.

is

the action of cold water,

NO

and of

What do

these reactions

indicate in respect to the composition of this compound ?


207-208.) 3. What is its action upon potassium iodide?

(Richter, pp.

aqueous solutions of the alkalies upon

(16) Nitrogen pentoxide,

NO
2

5.

(Richter, p. 205.)

NITRIC ACID.
i.

HNO

In a retort heat a mixture of sodium nitrate and sul-

Preparation.
phuric acid in proportions corresponding to the equation (?)

NaNO,

+ H SO
2

= N*aHSO

-f HNO

3.

PHOSPHORUS AND HYDROGEN.

NITROGEN GROUP

29

Collect the product in a cold receiver.


Color ? Odor ?
are the physical properties of
2. What
3 ?
Action on litmus (dilute with
2 O) ?
3. What action has it on indigo ?
Upon the skin ? 4. Notice the effect of the acid upon the following

HNO

Write the reaction for each one. 5.


Fe, Pb, Zn, Sn.
Cover powdered sulphur with the acid, and warm (?). Dilute with water,
6. Add a few drops of HNO 3 to
filter, and test the liquid with BaCl 2 (?).
metals: Cu,

a solution of ferrous sulphate (?)

Problems.

i.

Required

prived of O ; and
with 80 pts. of O ?

cu.

warm

the solution (?).

How much

m. of N.

how much P must be burned,

HNO

if

62

air is to
pts.

of

be de-

unite

2. How much
3
containing 46 per cent, of water, may be obtained from 1,700 grms. of NaNO 3 and how much water must be taken ?
3 will be absorbed
2 O, if
by 5 litres of
3. How many grams of
,

NH

the latter absorbs 500 times its volume of the gas ?


4. Ten litres of
water having absorbed 700 times their volume of ammonia, what are the
least

amounts of

NH

C1 and

(1)

i.

necessary for producing this solution

PHOSPHORUS.

varieties.

CaO

P.

Determine the physical properties of the active and the red


2. Allow a small piece of the active variety to ignite in the air.

Will the red variety do this? 3. Throw a small piece of the yellow
Repeat with the red variety (?).
variety into a jar of dry Cl (?).
4. Bring a small dry piece of active P in contact with iodine (?).
5.
a flask containing a small piece of P and water until the former is
melted, then pass a current of oxygen through a delivery tube into the

Heat

melted phosphorus

(?).

Care

(Study Richter, pp. 133-136.)

PHOSPHORUS AND HYDROGEN.

PH
i.
Fill a flask almost
(2) Phosphine
concentrated NaOH solution.
Add a few pieces
3.

When

full

with a moderately

of P, and heat carefully.

the air in the neck of the flask has been expelled by the escaping
cork with a delivery tube the other end of which dips under

gas, insert a

warm

water.

What becomes

of the gas as

it

escapes into the air

the reaction involved.

(Richter, pp. 136-139.)


there any similarity between

Is

PH

and

NH

Write

EXPERIMENTS IN GENERAL CHEMISTRY.

30

i.

(3)

PHOSPHORUS AND THE HALOGENS.


Pass a current of dry CO gas into a retort, the bottom

of which

covered with dry sand. When all the air has been expelled, introduce
some well-dried pieces of P, and replace the CO 2 by a stream of dry Cl.
Connect the neck of the retort with a Liebig's condenser, and collect

is

the product in a receiver.

It

What

phosphorus trichloride.

is

are

its

properties? Pour some of it into water (?).


2. Place a little PC1 3 in a dry test-tube, and pass a stream of dry Cl
upon its surface. What is the result ?

PHOSPHORUS AND OXYGEN.


(Richter, pp. 214-219.)
i. Prepare phosphorus pentoxifte, P 2 O 5 by burning a carefully dried
P under a dry bell -jar. 2. Drop a portion of the product into
of
piece
water (?).

(4)

pyrophosphoric acid,
series of salts are

P2 O

derived from them

HPO

and FeCl 3

4 ;

guish the different salts ?


i. Dissolve some Na 2

Na

H PO metaphosphoric acid, HPO and


How are these acids obtained ? How many

Orthophosphoric acid,

(5)

What do you

By what names would

and

in water

test che solution

observe in each case

2.

y<Ju distin-

with

AgNO

Dissolve fused

HPO

4 in water, and perform the same tests with its solution.


3. Heat
it no
of phosphorus (NaNH 4
4 ) until
cool,
longer effervesces
crush the residue in a mortar, and dissolve it in water.
How does this
2

HPO

salt

upon treating with the above reagents? 4. Acidify a


of
the
last-named
solution with acetic acid, and add a solution of
portion
albumen to it. Result?
solution behave

P2 O 3 and phosphorous acid H 3 PO 3


(6) Phosphorus trioxide
Pour PC1 3 into water. Evaporate the solution to syrupy consistency
.

(Study Richter,

(7) Hypophosphorous acid

H PO

Heat pieces of phosphorus

2.

in a

porcelain

dish

strong baryta solution (see p. 29).

When- no more

CO

it

filter,

and pass

(?).

p. 216.)

into the solution until

with a moderately

PH

3 is formed, cool,
shows a neutral reaction to

Filter and
Toward the end, the solution should be warmed.
evaporate to suitable concentration.
Hypophosphite of barium will

litmus.

crystallize.

How may

the free acid be obtained from this salt ?

NITROGEN GROUP

ANTIMONY.

ARSENIC.
(1) Study

the

physical

31

As.

and chemical

of

properties

this

element.

Are they analogous to those of phosphorus


(Richter, pp. 142 and 143.)
Result
i. In a tube of hard glass heat a small piece of As to redness.

Heat As with the oxidizing flame upon charcoal


powdered As in strong HNO 3 (?).
2.

3.

(?).

To

33.

the mixture of

Zn and

Dissolve

ARSENIC AND HYDROGEN.


(2) Perform Marsh' s test for As*
Arrange the apparatus shown in Fig.

dilute

in a, add a small por2 SO 4 contained


tion of the solution to be tested for As.

The

liberated gas contains


It

and

AsH

passed through c, filled


with CaCl 2 (?), and then through d, a
After all the air has
tube of hard glass, contracted at several places.
been expelled from the apparatus, ignite the hydrogen. If As is present
it will burn with a bluish white flame, and white vapors will be given off.
(arsine).

Hold

is

a cold porcelain plate in the flame

(?).

Heat the tube

d, as

shown

in the figure (?).

Great care must be exercised


extremely poisonous

in performing this test, as the arsine

ANTIMONY.
(i) Study

this

SbH and AsH


3

gas

is

Sb.

element in the same manner as As. Distinguish between

3.

Treat the metallic mirrors obtained in Marsh's apparatus, with a


As dissolves readily,
freshly prepared solution of hypochlorite of sodium
i.

2. Heat a piece of the tube in which a


scarcely acted upon.
mirror has formed, in the flame of the Bunsen burner.
Dissolve the pro-

while Sb

is

warm HCI, and add H 2 S water (?). 3. Treat the spot


formed upon a cold porcelain plate with yellow ammonium sulphide, and
duct in dilute,

evaporate the solution at a gentle heat (?).


Problems.
(i) How much P can be obtained from

bones?
phine

vol. phos(2) 10 grms. of


the weight of the product remaining, after evapor-

(See Richter, p. 134.)


(3)

What

is

250 grms. of

give what

ating a solution of 10 grms. of

As

* Ask

in

HNO

for instructions.

EXPERIMENTS IN GENERAL CHEMISTRY.

32

CHAPTER

VI.

CARBON GROUP-CARBON AND


CARBON.

SILICON.

C.

How many

allotropic modifications of this element are known?


(i)
What are their principal properties? i. Boil a dilute litmus solution

with powdered animal charcoal;


for the litmus in the preceding
3.
i.

Result?

filter.

experiment

2.

Substitute indigo

(?).

Determination of the composition of coal.


Volatile matter and coke.
Weigh out 2 grms. of powdered coal in
a platinum crucible provided with a well-fitting

Heat with a

cover.

gases cease
crucible.

to

large flame, until the escaping


lid and the

burn between the

lamp flame is applied for a


Cool and weigh. Loss in weight

blast

minute longer.
represents the
called coke.

volatile

matter.

The

residue

is

A second portion of coat (i grm.) is


over the Bunsen flame, until the
heated
gently
2.

Ash.

volatile constituents

then raised and the


Fig. 34.

The

residue

The

are expelled.

heat

is

of the crucible placed in the position indicated in

lid

is

the ash.

(Read Richter, pp. 150-152.)

CARBON AND HYDROGEN.


(2)

Methane (Marsh gas)

CH

4.

Heat a dried mixture of sodium acetate and sodium


Preparation.
hydroxide in an iron tube.* Collect the gas over water. Note its color,
i.

odor and
times

its

structions

Does

taste.

vol.

it

burn?

2.

Mix

vol.

of

it

with

of air and explode by applying a flame.

(Ask

to

for

8
in-

!)

How

would you determine the molecular weight of this compound ?


Make
a eudiometric combustion of i vol. of CH 4 with 2 vols. of
(3)

as described in Richter, p. 121.

(4)

Ethane

(5) Acetylene

6.

(Richter, p. 153.)
Light a Bunsen burner at the base

*A

hard glass tube will answer.

and turn

it

CARBON GROUP
down, so that the flame

is

SILICON.

33

Acetylene can be recognized, among

small.

by its characteristic odor.


CARBON AND THE HALOGENS. (Richter, p. 160.)

the products of combustion,


(6)

CARBON AND OXYGEN.


(

CQ

Carbon dioxide

7)

2.

Upon pieces of marble, contained in an evolution


1-2 H O).
Conduct the resulting gas
flask, pour dilute HC1 (i HC1
It may be collected either by
through water and through cone. H.jSO 4
i.

Preparation.

2
.

downward displacement of
and odor of

taste

the
Is it

this gas.

or over mercury.
2. Note color,
How does its weight
soluble in water ?
air,

Does it burn
compare
a
Conduct
current
of
CO
2 into a solution
3.
the
Na 2 CO 3 (?). 4.
and
test
residue
for
liquid,
Na 2 CO 3 solution, add solutions of MgSO BaCl
with that

of air

4i

or support combustion ?
of NaOH, evaporate the

To
2>

different portions ,of

Pb (NO 3 ) ZnSO 4
2,

(?).

(Study Richter, pp. 228-232.)


(8)

Carbon monoxide

CO.

i. In a tube of hard glass heat zinc dust to faint redness,


Preparation.
while conducting a slow current of CO 2 over it.
In what respect does

the

differ

product

cone.

H SO
2

Write the reaction.


(9)

from

in a flask,

CO 2 2. Heat crystals of
and wash the product with a
.

Study the properties of

Carbon disulphide

CS

this gas.

oxalic

2.

(10) CARBON AND NITROGEN.


i. In a dry test-tube heat a
nitrogenous carbon

rating with

Cool and add water.


.

2.

(NH

solution.

(Richter, p. 233.)

Perform some of the experiments indicated in Richter,

piece of K.
with AgNO 3

acid with

NaOH

KCN

is

p. 234.

compound with

a small

formed and can be tested

Convert a portion of the KCN into KCNS by evapoTest with FeCl 3


3. To a solution of FeSO 4 add

4 ) 2 S.

potassium ferrocyanide.

What

results ?

ferrocyanide upon solutions of ferric


(n) Study the nature of flame.

4.

What

is

the action of the

salts ?

Make

the experiments described'in

Richter, pp. 155-160.

SILICON.

Si.

Make an intimate mixture of i grm. magnesium


Heat this to
powder and 4 grms. of finely powdered quartz-sand.
It is best to use the blast
bright redness in a wide tube of hard glass.
1

(i) Preparation.

for this purpose.


The part of the tube containing the mixture
should be rotated in the flame. The residue, after a few minutes' heating,

lamp
is

allowed to cool, and treated with water containing HC1.


5

The product

EXPERIMENTS IN GENERAL CHEMISTRY.

34
consists of

amorphous

silicon

and undecomposed

action of the following reagents upon Si


fluoric acids, potash solution and chlorine.

SILICON

2.

quartz.

(Read Richter,

Test the

and hydro-

sulphuric, nitric

p. 161.)

AND OXYGEN.

SiO 2
(2) Silicon dioxide (Silica, Quartz)
i. Test its solubility in the various acids and alkalies.
.

ture of

2. Fuse a mixgrm. of finely powdered quartz with 4 grms. of Na.2 CO 3 in a


,

platinum crucible.

Dissolve the product in water.

3.

To

a portion of
Take up the

add HC1, and evaporate to complete dryness.


and filter off the insoluble portion. 4. To another
the
of
aqueous solution of the fusion add NH 4 C1. (?). Make a
portion
bead of salt of phosphorus ; bring a fragment of a silicate or of quartz into
it, and heat in the blow-pipe flame for a few minutes (?).
this solution

residue with water

BORON.
it

B.

(1) Preparation similar to that of Si.


Is
unite directly with other elements ?

modifications

What

is

What are its properties? Does


it known in several
allotropic

the valency of this element

(Read Richter, pp. 240 and 241.)

BORON AND OXYGEN.


(2) Boric Acid -BO 3
i. Dissolve borax in 5 parts of boiling water, add HC1 to acid reaction,
and allow to cool. What crystallizes out of the solution ? Dry some of
.

Test its solubility in


the product by pressing it between filter paper.
What do you observe on igniting the alcoholic
water and in alcohol.
Moisten a piece of turmeric paper with an aqueous solution of
solution ?
boric acid, and dry at a gentle heat.

Problems.

(i)

grms. of carbon

CaCO

give,

What happens?

How much CO results from


(2) How much CO will an
2

the combustion of 12
indefinite

when acted upon by 4.666 grms. of muriatic

quantity of

acid, contain-

CO

ing 30 per cent, of pure HC1 ?


(3) How many cubic decimeters of
can be obtained from 90 grms. of oxalic acid ? (4) What amount of SiO.2
2 grms. of Wollastonite (CaSiO 3 ) ?
(5) What is
the theoretical quantity of boric acid obtainable from 15 grms. of borax

can be obtained from

(Na 2 B 4 O 7 -f ioH 2 O)?

METALS OF THE ALKALIES

POTASSIUM AND OXYGEN.

35

METALS.
CHAPTER

VII.

METALS OF THE ALKALIES POTASSIUM, SODIUM, [AMMONIUM].


POTASSIUM. K.
(1) Preparation.
Arrange apparatus as shown in Fig. 35.
of hard glass, c, introduce a porcelain boat containing about
mixture of 138 pts. (i
FJG

Into a tube
i

grm. of a

35

mol.)

of dry (?)K 2 CO 3
pts.
(3 at.) of

and 72

Mg powder.

Pass a cur-

rent of dry

over

and after all the


been displaced
apparatus

it,

air

has

in

the

light the

(?),

escaping gas ; heat the


part of the tube surrounding the boat to incipient redness.

which

is

formed, and drive

temperature

and the
residue

it

is

potassium.

the boat

it

(2) i. Cut a piece of


the fresh surface. Care !

(3)

i.

it

in this

What

is

the

method of preparation.

K with a knife, and observe the color and lustre of


2.

To ascertain whether the

in a stream of

Expose a thin

brilliant metallic mirror

away from the boat by increasing the


Note also the green color of the vapor

Formulate the reaction involved

a small piece of

Observe the

imparts to the burning hydrogen.


Test its reaction with litmus (?).

violet coloration
left in

it

slice

H.

of

K
H

metal

is

fusible, heat

heavier or lighter than water ?


to the air.
What takes place? 2.
3.

Is

it

a small piece of it upon


In this experiment it is ad2O
(?).
visable to use a tall beaker and to cover the same with a glass plate.
3.
What is the action of the halogens upon K? Ask for instructions.

Throw

POTASSIUM AND OXYGEN.


Potassium
In an iron vessel dissolve
Hydroxide.
(4) Preparation of
in
of
water.
of
160
cc.
Cautiously add
crystallized Ba(OH) 2
50 grms.
a hot concentrated solution of 20 grms. of

K SO
2

until a

sample of the

no longer precipitated by either K 2 SO 4 or Ba(OH) 2


supernatant liquid
Filter rapidly through a plaited filter, and evaporate the solution in an
is

Continue heating the residue till it


During this operation protect the eyes
appears in a state of quiet fusion.
with a glass plate. Now pour the product upon a clean iron surface, and

iron or silver dish over a large flame.

EXPERIMENTS IN GENERAL CHEMISTRY.

36
while

still

Examine

warm

it

put

fracture

its

into a bottle provided with a well-fitting stopper.


color.
Try its solubility in water and in alcohol.

and

What is the reaction of the aqueous solution with litmus ? What

is

an alkali

Salts.

(5) Potassium Chlorate.


(6) Potassium Nitrate.

grms. of
rates

NaNO

from the

KC1O

KNO

3.

3.

(See p. 22).
a hot concentrated solution of 20

To

add a solution of 18 grms. of KC1. Boil. What sepamixture ? What crystallizes from the mother liquor

warm

on cooling ? Recrystallize the latter product. Examine its crystalline form.


Is it more soluble in hot than in cold water ?
Explain the method of
preparation.
(7) Into a red-hot platinum crucible throw small portions of an intimate
mixture of 10 grms. of
What
3 and i^ grms. of charcoal powder.
takes place?
Write the reaction. What is gunpowder ?

KNO

Reactions.
(8)
i.

Use

KNO

Place a

introduce

for the following tests.

little

of the

salt

upon the end of a clean platinum wire and


What color do you observe?

into a non-luminous flame.

it

View

the flame through a cobalt glass (?).


2. To the aqueous solution
of the potassium salt add HCland boil.
Concentrate by evaporation and
add PtCl 4
What is the composition of the resulting precipitate ? Try
.

its

solubility in hot

and

in cold water, also in alcohol.

3.

To

the con-

centrated solution of the salt add a saturated solution of tartaric acid

on shaking, a white

either at once, or

SODIUM.
(1)

How

Na.

metal usually prepared ?


physical and chemical properties (Richter,

this

is

(2) Study

crystalline precipitate appears (?).

its

Wherein does
(3) Prepare

it

differ

from

p.

285).

K?

Sodium Amalgam.

To 500

grms. of dry mercury, contained in a Wedgewood mortar add


Perform this operation in a
gradually 5-10 grms. of Na in thin slices.
good draught chamber, as the union of the two metals is attended with
the evolution of light and heat, and poisonous vapors are given off. Stir
well with the pestle, allow to cool, and transfer the product to a wellWhat is its action on 2 or dilute 2 SO 4 ?
stoppered bottle.

HO

SODIUM AND OXYGEN.


(4) Preparation of Sodium Hydroxide solution.
Add a little water to 10 grms of fresh quicklime contained in an iron

Cover the latter, and in a second iron pot dis(or porcelain) vessel.
solve 25 grms. of soda ash (Na2
3 ),
using about 100 cc. of water.

CO

SODIUM AND OXYGEN.

METALS OF THE ALKALIES

Heat the solution

to boiling

stir

37

which should have

the quicklime

with enough water to form a thin paste


and
this
of
add
Stir well
gradually to the boiling liquid.
lime),
(milk
with an iron wire ; transfer the mixture to a bottle ; cork, and allow it to

broken up

to a

white powder

After the supernatant liquid has become perfectly clear, decant it


It should be preserved in
glass siphon filled with water.
a tightly corked bottle (?). Test a few drops of the solution with BaCl 2 (?).
stand.

by means of a

What
which

should the solution contain, and of what does the precipitate, from
Write the equation representing the reit was separated, consist?

action.

(5) Determine the

Measure

amount of

NaOH contained in the solution.

off accurately 20 cc. into a porcelain dish

add a drop or two

of phenolphthalein solution, and dilute with water.


From a burette carehas just disappeared.
until
the
color
dilute
red
add
acid
fully
hydrochloric

Read

off the

volume of the acid used

neutralize the alkali

it is

the exact quantity needed to

NaOH

-f

(i mol.) of

HC1

NaCl

+ H

O;

NaOH

require 36.5 pts. (i mol.) of HC1,


the weight of the HC1 contained in the volume of the
dilute acid consumed, a simple proportion will give the weight of the
that

is,

and

if

40

pts.

we know

The strength of the acid is determined


follows: In a porcelain dish, dissolve 1.06 grms. of pure Na 2
3,
previously ignited and accurately weighed; add a little phenolphthalein,
alkali in 20 cc. of the solution.

CO

as

heat to boiling and introduce acid from the burette until the liquid
remains colorless after continued boiling. The carbonate is then exactly
neutralized

Na 2 CO 3

2HC1

2NaCl

CO 2

+ H

2 O.

73 pts. of HC1 for 106 pts. of Na 2 CO 3


Suppose, now,
20 cc. of the acid had been used to decolorize the indicator, then i cc.

It takes, therefore,

would equal

iffi

= .53

grms. of

Na

CO

3,

or .365

number is the standard or strength of the


The phenolphthalein takes no part in these

latter

cates

by

its

grms. of HC1.

The

dilute acid.

it
reactions
merely indichange of color the complete neutralization of the alkali.
;

is it
necessary to boil the solution when the acid
with a carbonate ?

Why

is

standardized

Salts.

(6) Sodium

chloride.

NaCl.

Grind 50 grms. of salt in a mortar with 150 cc.


Purify common salt.
of water.
Filter into a beaker, and conduct HC1 gas into the solution,

EXPERIMENTS IN GENERAL CHEMISTRY.

38
as

shown

Pure NaCl separates out.

Collect it on a platinum
cone, remove the liquid with the aid of a filter
pump, and dry the salt by warming it in a porce-

in Fig. 36.

no.

3 6.

lain dish,

while stirring

it

with a glass rod.

Na 2 CO 3
(7) Sodium carbonate.
some
of
the
commercial carboRecrystallize
nate.
Heat a portion of the product in a porcelain dish.
What do you observe ?
.

Reactions.
(8)

Use the

purified chloride for the tests,

i.

What

color do sodium

2. Mix a drop of the aqueous solution with 10


give to the flame?
drops of a PtCl 4 solution on a watch-glass.
Evaporate very carefully to
a small volume.
On cooling, a red colored salt crystallizes out in long

salts

monoclinic needles

(?).

Is

it

soluble in water? in

alcohol?

there any salts of sodium which are not soluble in water


pounds of sodium be precipitated by any reagent ?

(1)

What

is

the

AMMONIUM.
composition of ammonium?

Can

it

3.

Are

Can com-

be obtained in a

free state?

(See Richter, p. 295.)


(2) Dissolve commercial sal ammoniac in a

in slight excess,

warm,

filter if

crystallization; stir constantly.


in the form of a fine powder.

a precipitate

is

Ammonium

little

water,

add ammonia

formed, and evaporate to


chloride is thus obtained

Reactions.

On

a piece of platinum foil heat successively small portions of


(3)
What occurs in each case ?
the chloride, the sulphate, and the nitrate.
Note the odor
in
small
mortar.
with
lime
a
C1
burnt
2. Mix a little
4
i.

NH

of the escaping gas and its reaction with litmus.


What
tion of
4 C1 with a caustic soda solution.

NH

Heat

3.
is

a small por-

given off? Explain


4. Add PtCl 4 to a

the action of strong bases upon ammonium salts.


Result? 5. To a concentrated solution
solution of
4 C1.

NH

ammonium salt add tartaric acid and shake the mixture


pounds of ammonium impart a color to the flame ?

Compare

the metals of the alkalies with each other.

(?).

How can the com-

pounds of potassium, sodium, and ammonium be distinguished


Problems.

i.

How much KNO

is

of the

Do com-

6.

theoretically obtainable from 2 kilos

METALS OF THE ALKALINE EARTHS


of Chili saltpetre of

KC1

97%, and what amount

CALCIUM.

39

of Sylvite containing

HNO

98%

of

were required
to saturate 50 cc. of a potash lye; further, that 10 cc. of the acid neuwould the lye contralized i. 06 grms. of Na 2 CO 3 what amount of
ash
In
a
the
valuation
of
CO
tain?
2
3 ), 29.1 cc. of a
(impure
pearl
3.
is

required?

2.

Suppose that 75

cc. of dilute

KOH

sulphuric acid were used to neutralize 5 grms. of the sample ; the acid
litre ; calculate the percentage of imcontained 98 grms. of
2 SO 4 per
4. Required the minimum amount of marble that
purities in the product.

should be burnt to liberate the

NH

from 50 grms. of

CHAPTER

NH NO
4

3.

VIII.

METALS OF THE ALKALINE EARTHS CALCIUM, STRONTIUM, BARIUM.


CALCIUM.

Ca.

CALCIUM AND OXYGEN.


(1) i. Ignite 2 grms. of powdered marble in a platinum crucible to
the highest temperature obtainable with the aid of the blast lamp.
Continue this for 15 minutes, occasionally stirring the mass with a platinum
wire ; what is the residue ? Explain the reaction.
2. Add about 5 cc.

of water to the product.


What do you observe?
the product with litmus paper.
(2)

i.

Prepare lime water.

To

the

slaked

Test the reaction of

lime obtained

from 20

transfer the mixture


p. 37) add i litre of water
to a bottle.
Cork tightly, shake and allow to stand. When the solution
has become clear, draw it off by means of a siphon ? What does it contain ?
Of what does the undissolved portion consist ? 2. Place a portion of the lime water on a watch glass and expose to the air(?).
3.
Through a second portion blow air from your lungs (?). 4. Conduct a
stream of CO 2 through a third portion and observe carefully the successive

grms. of quicklime (see

changes.
tion

Explain them. 5. What takes place upon boiling the clear soluis obtained as the final product in the preceding experiment ?

which

Salts.

(3)
i.

What
What

Calcium Chloride.

CaCl 2

Evaporate some of the spent acid of a


the residue?

CO

generator to dryness.

Expose a little of the salt to the air (?). 3.


use have you made of CaCl 2 previously? 4. Prepare porous CaC/^
is

2.

Dissolve the residue obtained in


(CaCl 2 -f- 2H 2 O).
filter, and neutralize exactly with HC1.
Evaporate the

in

lime water,

filtrate to

dryness

EXPERIMENTS IN GENERAL CHEMISTRY.

40

and heat the residue for some time on the sand-bath.


show a neutral reaction.

in a porcelain dish,

The

solution of the product must

Calcium Hypochlorite.C*(C\Q\.
(See p. 22.)
CaSO 4
(5) Calcium Sulphate.
i.
Carefully heat a few grms. of gypsum in a porcelain dish until the
water of crystallization is completely expelled.
Pulverize the residue.
(4)

What happens when


stand

it

is

made

and allowed

into a paste with water

to

Reactions.

Use

the pure

CaCl 2

for the following tests

Introduce a small portion of the salt into the Bunsen flame by


means of a platinum wire (?).
2. To the aqueous solution add (NH 4 2
)
i.

CO

Result

3.

To

3.

another portion add dilute


What is the
2 SO 4
Why does it not form in very dilute
.

composition of the precipitate?


solutions?

3.

Add (NH 4 ) C O
2

to the filtrate

from the

CaSO 4

(?).

STRONTIUM.

Sr.

Reactions.
i.

What

element

color
2.

imparted to the Bunsen flame by compounds of this


a CaSO 4 solution to the solution of a strontium salt (?).

is

Add

BARIUM.

Ba.

Reactions.

Observe what color Ba compounds give to the flame. Moisten the


2. To a portion of the aqueous
sample with HC1 before heating it (?).
i.

solution of the chloride

H SO
2

to a

add

second portion

(NH ) CO
4

3.

What

results?

Add

2.

dilute

(?).

Point out how the elements of this group may be distinguished (#)
from those of the preceding group ; (b} from each other.
Problems.
i. How much nitric acid of 20 per cent, will effect the soi grm. of Iceland spar
(CaCO 3 ) ? How much CO 2 is given off,
and what volume would it occupy at 20 C. under a pressure of 750 mm. ?
2. Suppose .5 grm. of sulphur were dissolved in HNO 3 what quantity
of BaCl 2 must be added until it ceases to produce a precipitate ? 3. One
grm. of a mineral consisting of the carbonates of Ca, Sr, and Ba, in the
proportion of their molecular weights, will leave what weight of the mixed

lution of

sulphates on treating

and evaporating with an excess of

H SO
2

MAGNESIUM GROUP

MAGNESIUM.

CHAPTER

IX.

MAGNESIUM GROUP MAGNESIUM,

MAGNESIUM.
Examine

41

ZINC,

CADMIUM.

Mg.

metal in the forms of ingot, ribbon and powder*


(1)
Note its color, lustre and specific gravity. 2. Introduce a piece of the ribbon into the flame with the forceps (?). What is the product ? 3. Treat
the

a piece of the ribbon with dilute

H SO
2

4.

Reaction

Salts.

Magnesium Chloride. MgCl 2


Prepare the ANHYDROUS salt. Dissolve about 50 grms. of the crystallized (?) chloride and 50 grms. of NH 4 C1 in as little water as possible.
Evaporate to dryness in a porcelain dish. Reduce the mass while hot to
small pieces in a mortar, dry it carefully, so as to remove every trace of
It is best to do this by heating small portions of the material
moisture.
in a porcelain crucible until it no longer sinters.
A small sample should
not give off moisture when heated in a dry test-tube.
Be careful also to
.

(2)

prevent re-absorption of moisture.


Quickly transfer the warm powder to
a platinum crucible provided with a well-fitting cover.
Heat, at first
4 Cl, then increase the temperature until the mass
gently, to expel the

NH

It is the anhydrous salt which,


of quiet fusion.
being
be
should
extremely hygroscopic,
preserved in a tightly stoppered bottle.
It should dissolve in water to a clear liquid.
is

in a state

Why

cannot the anhydrous chloride be obtained by evaporation of the

aqueous solution

Mg SO 4 -f yH 2 O.
(3) Magnesium Sulphate.
What
Recrystallize some of the commercial salt.
crystals ?

Taste

is

the form of the

(4) Reactions.

Heat a portion of the sulphate or chloride on a platinum wire


Bunsen flame moisten with Co(NO 3 ) 2 solution and heat again.

i.

the

Add some

2.
pink-colored mass results.
solution of the chloride (?).

dition of an

ammonium

solution with
is

NH

and

The

little

resulting precipitate dissolves

of the

on ad-

3. Mix a second portion of the chloride


add Na 2 HPO 4 and agitate the liquid. What

salt (?)

NH

C1,

the composition of the precipitate


6

caustic soda to a

in

Examine

it

with the aid of a lens.

EXPERIMENTS IN GENERAL CHEMISTRY.

42

ZINC.
(1)

How

is

this

Zn.

metal obtained from

its

ores?

(2) Study the physical and chemical properties of Zn (see Richter, p.


2. Rei. Treat a small piece of pure Zn with dilute
2 SO 4 (?).
316).
the
commercial
metal.
What
this
impure
experiment, substituting
peat

do you observe ? What causes it ?


Melt 100 grms. of the metal in a wellcommercial zinc.
Granulate
(3)
The blast lamp maybe used for this purpose,
covered Hessian crucible.
difference

The crucible
it is better to perform the operation in a wind furnace.
then removed from the source of heat, and allowed to cool until the

but
is

melted metal no longer takes

fire

when

the cover

is

Pour the
Drain the

lifted.

metal, in a thin stream, into a pail filled with cold water.


product and dry at a moderate heat.
Salts.

(4) Zinc sulphate.

of this

salt

and

Zn SO 4

recrystallize

-f
it

O. (See p. 12).
carefully from water.

7H

i.

Prepare some

2.

Examine the

What

other salt have you prepared that exhibits similar forms


crystals.
Is there any analogy in the composition of the two salts ?

Reactions.
i. Heat a small piece of Zn on charcoal in the oxidizing flame. (?)
Moisten the incrustation obtained with a drop of Co(NO 3 ) 2 and heat
What is the
of ZnSO 4 add (NH 4 ) 2 S.
Result ?
3. To a solution
again.
in
HC 2 H 3 O,
color of the precipitate ? Try its solubility in dilute HC1 and

(5)

2.

(acetic acid).

the

Zn

4.

Study the action of caustic

alkalies,

e.

g.,

NaOH

upon

solution.

How could you distinguish between Zn and


are there between this and the preceding groups

Mg ? What

differences

the strength of a sulphuric acid of which 20 cc.


2. Suppose it was found that i grm.
dissolve exactly .048 grm. of Mg?
C. and 755 mm., and,
at 16
cc.
of
of Zn gave with
2 SO 4
325

Problems.

i.

What

is

further, that .369 grm. of

Mg

Knowing the atomic weight of


two sulphates are isomorphous,

Zn from

the data given

produced the same amount of the gas.


Mg to be 24, and remembering that the
how is it possible to deduce the at. wt. of

MERCURY AND OXYGEN.

CHAPTER

43

X.

MERCURY, COPPER, SILVER, GOLD.

MERCURY.

Hg.

(i) Study the physical and chemical properties of the metal.


does it differ from the other metals?

Wherein

MERCURY AND OXYGEN.

Hg O

Mercuric oxide.

(2)

How

substance prepared? What is its behavior on heating?


Mix a little powdered S with dry Na.2 CO 3 and HgO. Ignite the mixture in a dry test-tube.
Extract the residue with water, filter, acidify

with
this

is

this

HC1 and add BaCl

What

has

become of

the oxide of mercury in

experiment?
Salts.

Mercurous Nitrate.

(3)

An

HgNO

3.

mercury (use 10-15 g rms O

excess of metallic

treated in the cold

HNO

with moderately strong


3 until the formation of crystals is no longer
noticeable.
Redissolve the crystals by warming, filter, and allow to
crystallize.

To

prepare a solution of the

HN0

salt

take

it

up with water acidulated with

(?).

(4) Mercuric chloride.

HgCl

Dissolve about 5 grms. of Hg in aqua regia.


Evaporate to dryness on
a water bath.
Place the residue into a small dry flask, cover the latter
with a watch-glass, and heat cautiously on a sand-bath.
What is the

sublimate formed in the upper part of the flask

Dissolve

it

in four parts

of boiling water and allow to crystallize.


Reactions.

Use the

(5) Mercurous compounds.

a few drops of
Filter,

and add

HC1

NH

solution of the nitrate,

to 2 or 3 cc. of the solution.


3

to the precipitate (?).

2.

to another portion of the nitrate solution (?).

immerse a

slip

when you hold


(6)

of
it

Cu

foil.

stain

Add
3.

Add

takes place ?
stannous chloride

In a third portion

on the metal

is it

changed

in the flame?

Mercuric compounds.

HS

Examine the

i.

What

The

chloride will answer for the

tests.

through a dilute solution and observe the gradation of


colors through which the precipitate passes.
What is the final product ?
i.

Pass

EXPERIMENTS IN GENERAL CHEMISTRY.

44

Add SnCl

2
drop by drop,
changes which occur.

2.

to the

COPPER.
i.

mercury solution.

Explain the

Cu.

Ignite the pure oxide in a current of dry


the color and the lustre of the product \ test

Preparation.

Examine

14).

bility in

H SO

HC1,

(both strong and

dilute),

and

HNO

(see p.

its

solu-

Write equa-

3.

tions representing the reactions.


Salts.

CuSO, -f sH 2 O.
Copper Sulphate.
10 grms. of Cu in a flask add 45 grms. of cone.
and heat.
2 SO 4
When the metal has completely disappeared and the gas (?) ceases to be
given off, allow to cool, place the white crystalline residue (?) into a
(2)

To

Now add a few drops of


porcelain dish, rinse the flask with hot water.
to
the
hot
water
and
filter.
From
the filtrate the sulphate
3
solution,
on
the
standing.
crystallizes
Recrystallize
product.

HNO

Does this salt suffer decomposition on exposure to the atmosphere?


Heat a small quantity in a porcelain crucible, first moderately, then more
strongly (?).

CuK2 (SOt) 2 -f- 6 2 O.


(3) Sulphate of Copper and Potassium.
2 SO 4
Prepare solutions of 10 grms. of blue vitriol and 7 grms. of
both saturated at 70. The latter should also contain a few drops of

H SO
2

4.

Mix

the

solutions

whitish-blue crystals.

on cooling the double

Examine

salt

separates

in

their form.

Reactions.

Use

(4)
i.

Mix

either of the salts

little

of the

salt

you have prepared.


with

Na 2 CO 3 and
,

heat on charcoal in the

2. Make a borax bead and dissolve a minute quanreducing flame (?).


What color does it give (a) in the oxidiztity of a Cu-compound in it.

ing flame? (<) in the reducing flame? (r) when the bead is reduced with
Is the
a small piece of tin ?
2 S.
3. Through a dilute Cu-solution pass

HNO

resulting precipitate soluble in HC1 or in


drop by drop, to the solution. What changes

3
4. Add ammonia,
do you observe? 5. To

a portion of the very dilute solution add potassium ferrocyanide (?).


(5) To a solution of copper sulphate in a porcelain dish add a small
Allow to stand over night. Note the result. Has the Zn
piece of Zn.

disappeared

form

Where

Does the
is

the

solution contain

any of

this

metal

In what

Cu ?

(6) Repeat the experiment, weighing the copper sulphate (.5 grm.)
Add.HCl in quantity sufficient to insure the
(.2 grm.).

and the Zn

SILVER.
entire solution of the Zn, collect the

dry, heat gently and weigh

be

it

45

Cu on

filter,

in a porcelain crucible.

wash with alcohol,

The

filtrate

should

colorless.

Compare
employed

the weight of the metallic Cu obtained with that of the Zn


How does the found Cu accord with the calculated amount

(?).

.5 grm. CuSO 4 .5H 2 O?


Repeat the experiment using Cd in place of Zn. Compare the weights
What deduction can you make ?
of the metals as before.

of that metal in

SILVER.

Ag.

(1) Prepare pure Silver from a coin.

Dissolve a 25-cent piece in nitric acid of sp. gr. 1.2, filter (?), and
Fuse the residue till it
evaporate the blue (?) solution to dryness.
Now add ammonia in
blackens, extract with 250 cc. of water ; filter.
large excess,

40

until

%)

and then, cautiously, a sodium bisulphite solution (of about


on boiling a small portion of the liquid, it is completely

decolorized.

The greater part of the Ag separates from the solution on standing in


The remainder may be precipitated by
the cold ; it is well crystallized.
the
to
70. Digest
product with strong ammonia (?), wash, dry
warming
and ignite it.
Examine the metal

carefully.

What

are

its

physical and chemical

characteristics?

SILVER

AND SULPHUR.

Ag.2 S.
(2) Silver Sulphide.
Into a dilute solution of AgNO 3

about
filter

(see next experiment), containing


grms. of the metal, pass H.2 S. When the liquid smells of the gas,
off the black precipitate, wash it with water and dry at 100.
2

Salts.

AgNO

3
(3) Silver Nitrate.
Dissolve the Ag obtained in (i) in dilute
S and evaporate to dryness on the water bath.
Dissolve the residue in 80 cc. of distilled water,
.

HNO

and preserve the solution

in a dark bottle (?).

What

is its

reaction with

litmus ?
Reactions.
(4) i. Compounds of Ag on charcoal before the blow-pipe give a
white metallic globule (?).
use the nitrate
add
2. To a silver solution
HC1. Collect the precipitate on a small filter, wash, dissolve it in amthe solution (?).
monia, and add an excess of
3 to
Explain these

HNO

EXPERIMENTS IN GENERAL CHEMISTRY.

46
reactions.

3.

Expose a small portion of the chloride

Any change ?

What

(Read Richter,

p.

is

practical application

to direct sunlight.

made of

this

reaction

340.)*
(5) Place strips of the metals Zn, Fe, Sn, Pb, and Cd in a solution of
What is the result in each case? Explain.
silver nitrate.

GOLD.
(1)

How

Au.

could you distinguish the metal

Au

from Hg, Ag, and Cu?

Reactions.

Dissolve a small piece of gold (or of a substance containing


in
aqua regia, concentrate the solution at a gentle heat and pour it
gold)
into a porcelain dish. Add a solution of FeCl 3 to an SnCl 2 solution until
(2)

i.

the latter

is

permanently yellow.

and then into the gold


formed.

Add

2.

solution.

After diluting, dip a glass rod into this


purple streak (purple of Cassius) is

ferrous sulphate to

some of the AuCl 3 solution

(?).

In what respects do the members of this group differ from each other,
and how can they be distinguished from the metals of the preceding

groups ?
Problems.

1.5 grms. of HgO gave on ignition with carbon 4.63 grms.


of metallic mercury; the specific gravity of the vapor of HgCl 2 referred
What is the atomic weight of Hg ? 2.
to H, was found to be 135.5.

Hg contains how many atoms, if the vapor density


TOO?
On
analysis a chalcocite was found to contain 20.15 per
equals3.
cent, of S and 79.85 per cent, of Cu.
Deduce the molecular formula
What
of
of the mineral.
4.
quantities
Ag, Au, and Hg can be precipiThe molecule of

tated from their respective solutions

by

CHAPTER
ALUMINIUM,

grm. of Cu

XI.

TIN, LEAD,

ALUMINIUM.

BISMUTH.

Al.

What
(i) By what methods is this metal obtained on a large scale?
the
of
are its properties?
the
action
following reagents upon Al
Try
the
Write
reactions.
HNO
and
NaOH
solution.
HC1,
3
:

* If
a
practicable, the instructor should here show and explain the preparation of
photographic negative.

TIN.

47

Sa/ts.

KA1(SO 4 ) 2 -j- i2H 2 O.


(2) Sulphate of Aluminium and Potassium.
mix these so that
2 SO 4 ;
Prepare saturated solutions of A1 2 (SO 4 ) 3 and
the resulting liquid contains the two sulphates approximately in the proThe double sulphate crystallizes on
portion of their molecular weights.

Why?

standing.

Recrystallize

it

from water.

What

is

the form of the

crystals ?

What

is

an alum!

(See Richter, p. 351.)

Reactions.
(3)

Use alum.

i.

Heat a

oxidizing flame, moisten with


(?) is the product.

(NH
To

4) 2

2.

little

of the salt on a platinum wire in the


and heat again. A blue mass
3) 2

Co(NO

To an aqueous

S to another portion of the solution.

the diluted solution

changes

add ammonia (?). Add


What do you observe ? 4.

solution

add NaOH, drop by drop.

Note the successive

(?).

TIN.

Examine

Sn.

emits on
i. Note the sound it
Etch a smooth surface with HC1 (?). 3. Try the solu4. What action have moderately dilute, and
bility of Sn in hot HC1.
concentrated, HNO 3 upon it? Write the reactions.
(2) Determine the specific heat of Tin.
A thin glass beaker of about 200 cc. capacity is carefully covered on
(1)

bending

(?).

a bar of this metal,

2.

the outside with a moderately thin layer of cotton wool.


This may' be
Pour 100 cc. of distilled water into the beaker.

called the calorimeter.

Suspend a thermometer

Introduce the test-tube with


boiling water.

Place 25 grms. of granulated tin


the latter with a plug of cotton.
contents into a beaker glass containing

in the water.

into a test-tube, close the

mouth of
its

stout copper wire will serve as a handle.

After ten or

minutes the tin will have acquired the temperature of the boiling
water
100. The tube is then rapidly removed from the latter and its

fifteen

outer surface freed from moisture by quickly passing a towel over it.
Remove the cotton from the mouth, and transfer the tin to the calori-

meter.

While the metal

is

being introduced raise the thermometer from

the water, and replace it as soon as all the metal has been added ; stir the
liquid well and observe, as accurately as possible, the highest point

EXPERIMENTS IN GENERAL CHEMISTRY.

48

reached by the mercury column.

from these data.

"
"

w
v
x

results

=
=
=

sp.

heat

can be obtained

temperature of water before introducing the


"
"
"
"
after
weight of the water.
"
of the metal.

Let y
"
"

Approximate

Calculate as follows

tin.

then

x __ loo(z-y)
"25 (loo-z)

Would

(Study Richter pp. 256-259.)

the specific heat found for tin,

when multiplied by

the constant 6.4 give the same value as that found in


experiment (3) for the equivalent of tin ? Explain.
many series
of tin compounds are there ?

How

(3) Determine the equivalent weight of Tin.


Place about 3 grms. of tin in a porcelain crucible that has been preCover the metal with 5-10 cc. of concentrated
3
viously weighed.

HNO

Then

by means of an

carefully apply heat

solved, while fumes of

NO

When

are set free.

The

iron plate.

tin is dis-

the acid has been entirely

expelled, heat the crucible with the white stannic oxide over a Bunsen
burner ; allow to cool and weigh.

=
of crucible and SnO
"
"
"
" metallic
= weight
_
Then w - v = weight of O,
" Sn.
"
andv - y =
8
Equiv. ofSn=i^-^
W V
Let w
" v
a.
v
y

tin.

(t

((

Softs.

SnCl 2
(4) Stannous Chloride.
Dissolve 10 grms. of granulated
.

of a few drops of PtCl 4

Sn

in

warm

cone.

HC1

with the addition

Put the solution into a well-stoppered bottle.

(?).

Reactions.

Use

(5) Stannous Compounds.


i.

is

precipitate (?)

What

is

1.

HS
2

Add

happens?

sulphide solution?

HgCl upon SnCl (see p. 44).


Compounds. Add a few drops of Br

solution,

Pass

precipitate?
2.

precipitate from the

the action of

(6) Stannic

SnCl 2

A brown
through a portion of the diluted liquid.
thrown down. Is it soluble in yellow ammonium sul-

What does HC1

phide?

the chloride solution.

HS

Conduct

and boil

(?).

Use the diluted

to a portion of the

liquid for the tests.

into a portion of the solution.


What
Is it soluble in HC1? in
4 ) 2 S?

is

the color of the

(NH

Cu-turnings, boil, decant the liquid, and add


Explain..

2.

HgCl

2.

What

BISMUTH.

LEAD.

49

Pb.

How

can this metal be obtained from the oxide?


(i)
cal properties can it be distinguished from other metals ?
the

By what
Is

it

physisoluble in

(2) In a solution of 5 grms. of lead nitrate in


of water, suspend a strip of metallic Zn and let stand for a

mineral acids?

about 50
few days

cc.
(?).

Salts.

of granulated lead (test-lead) by warming with


Concentrate by evaporation and allow to crystallize.

(3) Dissolve 5 grms.


dilute

HNO

3.

Reactions.
(4) i. Before the blowpipe, on charcoal, lead compounds are reduced
2. Add HC1 to a
to metallic beads, which are sectile with the knife.

Boil the precipitate with water. (?)


What takes
2 SO 4
4.
place on cooling?
3. To another portion add dilute
(?).
Pass
2 S into a third portion (?).

solution of the nitrate.

BISMUTH.

Bi.

Reactions.
i.

(i)

Mix

little

of the oxide or nitrate of Bi with

Na

CO

and heat

Does the resulting metallic globule


reducing flame on charcoal.
resemble lead ? Is it sectile? 2. Pass
2 S into a solution of the chloride
in the

HC1

Add

a large volume of water to a bismuth


What occurs? What reactions distinguish Al, Sn, Pb and Bi
solution.
from each other, and from the metals previously studied ?
i. What is the molecular formula of a mineral
Problems.
containing
or nitrate in

(?).

3.

SiO 2
A1 2

CaO

=
=
=

43.08
36.82
20.10
100.00

2.

of tin and chlorine yielded on analysis 29.42 parts of


its vapor density was ascertained to be
;
132.85.
the atomic weight of tin ?
3. Deduce the formula of Cosalite

compound

Sn and 35.40

What

is

parts of Cl

from the following analysis

S
Bi

Pb

Ag

=
=
=
=

15.27

41.76
40.32
2.65

IOO.OO

EXPERIMENTS IN GENERAL CHEMISTRY.

50

CHAPTER

XII.

CHROMIUM, MANGANESE, IRON, NICKEL/ COBALT.

CHROMIUM.

Cr.

CHROMIUM AND OXYGEN.


(1)

Chromic oxide.

Cr.2

3.

Mix intimately 20 grms. of potassium dichromate


Preparation.
and 4 grms. of sulphur. Heat the mixture in a porcelain crucible over
i.

the blast

for about

lamp

boiling water and dry


in dilute

HC1?

NaHSO

in a

2.

20 minutes.

at a gentle heat.

it

Fuse a portion of

Cool, extract the residue with


What is its color ; is it soluble

it

What

platinum crucible.

with six times


takes

experiment with some finely powdered chromite.

place?

its

3.

weight of

Repeat

this

(?)

Salts.

(2) Chromic Chloride.

CrCl 3

Prepare the anhydrous salt. Intimately mix 10 grams of Cr2 O 3 prepared as described, and 3 grms. of powdered charcoal, and convert this
into a dough with a little starch paste.
Form the product into balls of the
,

pea ; dry, and then ignite these (covered with charcoal powder)
in a Hessian crucible, provided with well-fitting lid.
Place the residue

size of a

into a tube of hard glass, and heat it in a current of CO.2 to expel every
With the aid of a blast lamp increase the temperatrace of moisture.
ture

and replace the

CO

by a current of

Cl.

The

excess of Cl should

be absorbed by conducting it into a bottle filled with caustic soda. (?)


The resulting CrCl 3 sublimes to the cooler portions of the tube. Describe
Is it soluble in water?
appearance.
other chlorides are prepared in a similar way

its

What

Write the equa-

tion, expressing the reaction.

(3) Chrome Alum.


Dissolve 10 grms. of

SO

Cr2 (SO 4) 3 .K2 SO 4 + 24 H 2 O.


K2 Cr2 O in a little water acidify with
7

into the liquid until the latter


stand ; the double salt crystallizes.
2

solve

warm

some of

it

What

it.

in cold water

H SO
2

is

4,

pass

Allow to
form ? Dis-

saturated with the gas.

What

is

its

crystalline

and note the color of the solution

now

takes place (see Richter, p. 374)?

How is it
2 Cr 2 O 7
crystals of potassium dichromate,
Dissolve 10 grms. of this salt in water, and from a burette
carefully add a caustic soda solution until the color is changed to yellow (?).
(4)

i.

Examine

obtained?

2.

MANGANESE AND OXYGEN.


What crystallizes from the solution on evaporation
convert the product into the dichromate ?

51
?

How

can you

re-

Reactions.

Dissolve a minute quantity of a chromium compound in a borax


(5)
bead.
Heat in the oxidizing and in the reducing flame. Results?
2. Heat a little of the compound with
3 on a platinum foil (?)
i.

KNO

(6) Chromic compounds.


caustic soda, drop by drop,

Use chrome alum

for the tests.

to a little of the solution. (?)

i.

Add

Continue the

addition of the reagent till the precipitate is redissolved.


What takes
2. What is the action of ammonia on the
place on boiling the solution ?
solution of the

chromium salt ?
Use a solution of potassium chromate.

(7) Chromates.
acetate solution.

i.

Add

lead

Note the color of the precipitate. Is it soluble in


2. Substitute BaCl 2 for the lead salt in the preceding exacetic acid?
add
2 SO 4 and
periment. (?)
3. Acidify the chromate solution with
H O 2 to the liquid. What happens? 4. To some of the chromate
solution add a few drops of HC1 and about i cc. of alcohol.
What occurs

when the mixture

is

heated to boiling

MANGANESE.

Mn.

MANGANESE AND OXYGEN.


(1) In what proportions do these two elements unite with each other?
Enumerate the oxides which occur in nature. What is formed when the

oxides of manganese are heated in

H?

When

they are ignited in the

air?
Salts.

(2)

Manganous

Chloride.

MnCl

-f-

4H

O.

Evaporate in a porcelain dish the solution obtained in the preparation


of Cl from MnO 2 and HC1.
Heat the dry residue over a small flame for

some time. Add much water and boil. Filter, and to


of the filtrate
add a solution of Na 2 CO 3 in excess. Allow the precipitate (?) to settle,
draw off the supernatant liquid with a siphon, and wash the remaining

Add the precipitate


precipitate several times with water by decantation.
then to the principal solution and digest at a gentle heat until a small
sample mixed with (NH 4 ) 2 S gives a flesh-colored precipitate which
Now filter and evaporate
completely dissolved by dilute acetic acid.

filtered
is

to crystallization.

(3) Potassium

Manganate

K MnO
2

and

Potassium Permanganate

K Mn O
2

8.

EXPERIMENTS IN GENERAL CHEMISTRY.

52

KOH

and 2.5 grms.


Maintain a
2
gradually add 5 grms. finely powdered
moderate red heat for 15 minutes. Dissolve the dark-green residue in a
In a porcelain crucible fuse a mixture of 5 grms.

KC1O

little

MnO

Observe the color of the solution. What does it contain?


much water and conduct CO 2 into the liquid. Is there

water.

Then

dilute with

any change

K Mn O
2

little

If so, write the equation expressing

as well as

of the alkaline

K MnO
K MnO
2

it.

are powerful oxidizing agents.


Warm a
solution with a few drops of alcohol (?).

of the permanganate solution, acidified with


add sul2 SO 4
phurous acid (?). Treat the acidified solution also with solutions of ferrous
sulphate and oxalic acid (?).

To

little

Reactions.

What

color do

Mn-compounds impart to a borax bead in the


What
is the effect of the reducing flame?
2. Heat a
flame?
oxidizing
little of an Mn-compound with Na 2 CO 3 and
3 on a platinum foil.
i.

(4)

KNO

What does

the resulting mass contain ?


3.
the chloride in water add (NH 4 ) 2 S. What

To

little

of the solution of

the color of the precipitate.


Test its solubility in acids (including acetic acid).
4. Add caustic soda
Is the precipitate soluble in
to another portion of the chloride solution.
an excess of the reagent ? Is its color affected by exposure to the air ?
is

Explain.

IRON.
(1) Preparation.

boat

filled

Into a tube of

Fe.

Bohemian

with the finely powdered oxide.

through the tube, and when

glass place a porcelain


Pass a current of dry

expelled (how could you test


What
it?), apply heat to that part of the tube which contains the boat.
After a red heat has been
is formed in the anterior portion of the tube ?
all

the air

is

maintained for 10 minutes allow the boat to cool in H, and examine


contents.

Are they attracted by the magnet ?

Expose the product

its

to

air (?).

How

is

properties? (see
iron, steel,

on a
and
Richter, pp. 393
394).

iron obtained from

its

ores

large scale ?

What

are

Distinguish between

its

cast-

and wrought-iron.
Salts.

(2) Ferrous Sulphate.

SO

4 -f 7H 2 O.
Fe
in
of
the
form
nails or wire, free from rust, contained
of
25 grms.
When the evoluin a flask, add 200 cc. of dilute (i
4) sulphuric acid.

-Fe

To

tion of the gas (? Note its odor !) is no longer violent, warm, and finally
boil until the liberation of gas ceases.
sample of the solution poured

IRON.

53

on cooling, give a copious separation of crystals.


Filter into a casserole containing 2-3 cc. of cone,
2 SO 4 , and let stand
for 8 hours.
Collect the crystallized product in a funnel the stem of
into a test-tube should,

which

is

closed with a loose plug

liquor to drain off,

wash with very

of glass wool,* allow the mother


cold water (?), and dry between

little

sheets of filter paper.


Examine the product carefully. Note its color,
in
water
and crystal form. What other salts of analotaste, solubility

gous composition are isomorphous with it


What is observed when some of the salt

?
is

heated,

first

moderately, then

strongly, in a tube of hard glass ?


Expose the aqueous solution of the salt to the air for several hours (?).

Ammonium

(3) Ferrous

Sulphate.

Fe

(NH ) (SO
4

4)2

6H

-f-

O.

In 100 cc. of dilute sulphuric acid dissolve clean iron wire till no more
hydrogen is given off; neutralize a like quantity of the acid exactly with
ammonia water, and add to it a few drops of dilute sulphuric acid. Filter
the iron solution into that of the

ammonium

salt.

Let the

salt crystallize,

on a funnel provided with a perforated platinum cone, wash and


as
described
under (2). Preserve in a well-stoppered bottle. What
dry
metals can replace the iron in this salt without altering its crystalline
drain

it

form?

Fe 2 (SO 4 ) 3 .(NH 4 ) 2 SO 4 -f 24H 2 O.


(4) Ferric Ammonium Sulphate.
Place 20 grms. of crystallized ferrous sulphate into a porcelain dish
Warm
together with a few cc. of water and 3.5 grms. of oil of vitriol.
on an asbestos plate, adding nitric acid, drop by drop, until no further
dissolve
3
change of color (?) is observed. Evaporate the excess of

HNO

the residue in hot water and add 3.5 grms. of (NH 4 ) 2 SO 4 ; filter, and set
the solution aside for crystallization. Separate the crystals from the mother
liquor,

and wash and dry them

does this

salt

belong

Why

as

under

(2).

To what

class of substances

Reactions.
(5) In a borax bead dissolve a small quantity of an iron compound,
and treat it successively in the oxidizing and reducing flames. What
changes do you observe ?

Use a freshly prepared solution of ferrous


(6) Ferrous Compounds.
sulphate for the following tests: i. To a few drops of it, diluted with
water, add ammonia. Note the color of the precipitate, and the changes
which occur on exposure
portion

(?).

to the air (?).

2.

Add (NH
HC1 ?

4) 2

S to another

3.

In a porce-

Is the resulting precipitate soluble in

lain capsule bring together a little of the ferrous solution

It is better to

with the aid of a

and a drop of

use a perforated platinum cone, and to remove the adhering solution

filter

pump.

EXPERIMENTS IN GENERAL CHEMISTRY.

54

a potassium ferrocyanide solution. Result ? 4. In a similar


drop of the iron solution with ferricyanide of potassium.

manner

test

In the presence of free acids, oxidizing agents


(7) Ferric compounds.
convert iron compounds from the ferrous into the ferric condition,
i.
Acidify the ferrous sulphate solution with sulphuric acid, warm, and add
cone.

HNO

until

to produce a

it fails

change

in color

the iron

is

then

Dilute a few drops of the yellow liquid with


several cc. of water and add ammonia (?).
3. Test a drop of the ferric
in the ferric state.

2.

solution with potassium ferrocyanide (?).

ferricyanide of potassium (?).

potassium sulphocyanate

5.
6.

(?).

Treat

4.

a.

second drop with

Mix another drop with


Conduct

HS
2

into

a solution of

some of the

ferric

What do you observe? Explain the reaction, and


sulphate solution.
write the equation expressing it.
7. Place a piece of metallic Zn in a
test-tube containing a solution of the ferric salt.
What takes place ?
Under manganese

it was observed
an oxidizing agent. To show
lower form of oxidation, fill a burette

(8) Quantitative estimation of iron.


that the salt potassium permanganate

how

this salt acts

with iron in

its

is

with an aqueous solution of it ; allow it to drop slowly into the solution


The pink color of the permanof a ferrous salt acidulated with
2 SO 4
on
This constirring with a glass rod.
ganate immediately disappears

tinues until the ferrous salt

is

completely oxidized to the

ferric state.

drop of permanganate added in excess will then impart a faint pink color
This indicates that the reaction is ended. Write the
to the liquid.
equation.

may be utilized for determining the quantity of iron in a


may be done, it is first necessary to standardize the

This behavior

That

solution.
FIG. 37-

this

permanganate solution.

Proceed

as

follows: Dissolve about 2

Fill a burette
2 O.
grms. of the permanganate in 1000 cc. of
clean
this
out
.2
of
'with
solution.
piano wire.
Weigh
grm.

Place this into a small flask (Fig. 37) provided with a cork
Cover the iron wire with dilute sulphuric acid.

and valve.*

When

Warm.

the iron

cork, add cold water

manganate
the

until the final

K Mn O
2

required to

consumed, then

is

completely dissolved, remove the


and slowly admit the per-

produce

this effect.

Suppose 30

cc.

"

K Mn O8
2

= .2000 grm. metallic


"
= .00666 "

iron.

then the standard of the permanganate in iron units.

* With a
sharp knife make a longitudinal incision of about
and close one end by means of a glass rod.

tube,

Note the volume of


cc. had been

pink coloration appears.

30

This

is

to the solution,

cm. length, in a rubber

COBALT AND NICKEL.

55

grm. of ferrous ammonium sulphate in 100 cc. distilled


and then introduce the permanganate until the
2
4

Next, dissolve
water, add 5 cc.

final reaction is

observed.

H SO

Calculate the percentage of iron in this salt

and compare the experimental result with the theoretical value.


How much oxygen will each molecule of K Mn. O 8 give up in oxidizing ?
How many molecules of FeO can be changed to Fe 2 O 3 by a molecule of
2

K Mn
2

COBALT.

AND NICKEL.

Co

Ni.

Reactions.

Dissolve a minute quantity of a cobalt compound in a borax bead.


in the oxidizing, then in the reducing flame (?).
2. What is the

i.

Heat

first

behavior of nickel compounds under like conditions? 3.


to a solution of Co(NO 3 ) 2 warm the mixture (?).

alkali

have caustic alkalies on solutions of nickel salts?


tion

cautiously add
the reagent.

ammonia.

more of

What

5.

To

Add

caustic

What

action

the cobalt solu-

After a precipitate (?) has formed, add


Expose the resulting solution

takes place ?

to the air in a shallow dish (?).


6. Treat a nickel solution in an analomanner
To
the
solutions
of Co and Ni, each in a separate
7.
gous
(?).
Filter and wash the precipitated sulphides, and
test-tube, add (NH 4 ) 2 S.
test their solubility in acids (?).

Note the colors of cobalt and nickel

salts, in

the anhydrous state.


Is there any marked difference between

the hydrated as well as in

Co and Ni

in respect to their

chemical deportment?

Point out the differences in the reactions of Cr, Mn, Fe, Co, and Ni.
How may ferrous compounds be distinguished from ferric ? What conditions are favorable to the conversion of the former into the latter?

The

latter into the

former

By what means may chromic salts be changed into compounds of


chromic acid? How may the reverse change be effected?
Devise a method for separating the elements treated in

this chapter.

i. How much K 2 Cr 2 O T can be obtained theoretically from


Problems.
100 kilos of a chromite containing 58.6 per cent, of Cr 2 O 3 ? 2. 100
grms. of a pyrolusite which was found to contain 4 per cent, of impuri-

EXPERIMENTS IN GENERAL CHEMISTRY.

56

C and 745 mm., when


ties, will give what volume of O, measured at 20
strongly ignited ? What is the weight of the residue, assuming that onehalf of the impurities was moisture, the other half quartz ?
3. How
3 are required to oxidize 12 grms. of crystallized ferrous
many grms. of

HNO

sulphate

which

.7

What percentage of metallic iron is contained in a salt, of


grm. are exactly oxidized by 17.8 cc. of permanganate solu4.

tion (standard

cc.

= .0056 grm.

Fe)

APPENDIX.
TABLE OF METRIC WEIGHTS AND MEASURES,
MEASURES OF LENGTH.
I

metre

metre

= 1000 millimetres,
= 39.3709 inches.

100 centimetres

10 decimetres

1.09363 yards = 3.2809

feet

MEASURES OF CAPACITY.
i

cubic metre

1000

litres

1,000,000 cubic centimetres

1,000,000,000 cubic

millimetres.
i

litre

= 61.02705 cubic inches = .035317 cubic

foot 3= 1.76077 pints

= .22097 gallon.

MEASURES OF WEIGHT.
I

I
I

= weight of
of water
4 C.
Kilogram = 1000 grams = 100.000 centigrams = 1,000,000 milligrams.
= 35-2739 ounces = 15432.35 grains.
Kilogram = 2.20462
gram

cc.

at

Ibs.

TABLE OF ATOMIC WEIGHTS OF ELEMENTS.


Aluminium

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