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^Tutorial
ANALYSIS Of
A SIMPLE SALT
<9
^f
ANALYSIS OF
A SIMPLE
SALT.
Price 6d.
In Active Preparation.
A QUALITATIVE
THnf\>.
Corr.
Coll. tutorial
Series.
BY
WILLIAM BRIGGS,
F.C.S,
AND
R.
W. STEWART,
B.Sc. LOND.,
AND PHYSICS
SCIENCE DIRECTOR OF UNIVERSITY TUTORIAL COLLEGE.
',
PRESS WAREHOUSE,
Row, STRAND, W.C.
/'<
CONTENTS.
PAGE
LISTS OF REAGENTS AND APPARATUS PROVIDED BY VARIOUS
EXAMINING BODIES
PREFACE AND DIRECTIONS
7
9
INTRODUCTION
11
CHAPTER
I.
PRELIMINARY EXPERIMENTS
CHAPTER
15
II.
GROUP
GROUP
I.
II.
Silver
30
Lead
Mercury (ous)
Mercury (ic)
Lead
Bismuth
Copper
Antimony
31
32
35
36
36
37
38
39
40
Arsenic
Iron
40
43
Chromium
Aluminium
45
46
47
48
49
50
Cadmium
Tin
GROUP
GROUP
III.
IV.
Nickel
Cobalt
Manganese
Zinc
GROUP
V.
GROUP VI.
'.
Barium
51
Strontium
Calcium
52
53
54
55
56
56
Magnesium
Potassium
Sodium
Ammonium
CONTENTS.
CHAPTER
III.
PAGE
57
57
58
58
59
59
60
Sulphuric
Sulphurous
Hyposulphurous
Hydrosulphuric
Hydrochloric
Chloric
Hypochlorous
Hydrobromic
60'
61
61
62
63
63
64
Hydriodic
Hydrofluoric
Hydrocyanic
Hydroferrocyanic
Hydroferricyanic
Nitric
64
Nitrons
Carbonic
Boric
65
65
66
66
67
Silicic
Phosphoric
Arsenic
Arsenious
67
68
Chromic
CHAPTER
IV.
SYSTEMATIC ANALYSIS.
PRELIMINARY EXAMINATION IN THE DRY WAY
EXAMINATION FOR A BASE Preparation of Solution
Table A., General.
Group I.
Group II.
III., Group III.
IV., Group IV.
V., Group V.
VI., Group VI.
EXAMINATION FOR ACID
69
76
I.,
II.,
APPENDIX
84
I.
MODEL ANALYSES
87
APPENDIX
II.
96
TABLE OF SOLUBILITIES
APPENDIX
III.
97
LIST OF REAGENTS
AND APPARATUS
Fluid Reagents.
IN 6
oz.
STOPPERED BOTTLES.
Ammonium
Ammonium
Ammonium
Chloride.
Sulphide.
IN 4
oz.
Sodium Phosphate.
Oxalate.
IN 2
oz.
Carbonate.
Sodium Hydrate
Sodium Carbonate.
Barium Chloride.
STOPPERED BOTTLES.
Ferric Chloride.
Lead Acetate.
Mercuric Chloride.
Stannous Chloride.
Alcohol.
STOPPERED BOTTLES.
Silver Nitrate.
Platinic Chloride.
In 4
Ammonium
Calcium Sulphate.
Potassium Ferrocyanide.
Potassium Ferricyanide.
Potassium Chromate.
Ammonium
oz.
Cobalt Nitrate.
STOPPERED BOTTLES.
Potassium Nitrate.
Potassium Cyanide.
Sodium Acetate.
of the pure
testa.
Chloride of Soda.
Magnesium Sulphate.
Calcium Chloride.
Molybdate.
Ammonium
Ammonium
Sulphate.
Chlorine Water.
Carbon Bisulphide.
Acetic Acid.
Dry Reagents.
IN 2
oz.
Fusion Mixture.
Sodium Carbonate.
Borax.
Potassium Nitrate.
Potassium Cyanide.
Ferrous Sulphate.
Calcium Hydrate (slaked lime).
Black Oxide of Manganese.
Apparatus.
Wash-bottle (page 21).
Sulphuretted Hydrogen apparatus (page 28).
(Ferrous Sulphide will be required for this apparatus).
2 doz. test tubes, 6 x f in.
2 boiling tubes, 8x1^ in.
Test-tube brush.
Test-tube stand to hold 12 at least.
Piece of wire gauze.
Piece of platinum-foil, 2 in. x 1 in.
3 inches platinum wire.
Black's blowpipe.
6 bulb-tubes.
3 watch-glasses.
2 porcelain evaporating basins, 2 oz. and 4 oz.
3 funnels, two 2-in. and one 3-in.
Filtering papers.
pestle,
oz. at least.
may
be useful.
PEE F AC E.
EVERY ONE who has
tried to do practical
own knows
work
in
Science
diffi-
With very
rived from,
theless, there is
if
No
chapters and tables, should be no difficult task.
to
a
made
render
this
cram
has
been
book, on
attempt
the other
hand
its
is
somewhat
DIRECTIONS.
it is
10
PREFACE.
Most people
analysis
even
if
allowance, treasure
fall
way.
it
does not
in an examination.
Make
purissima.
clean.
Be exact
day
INTRODUCTION.
QUALITATIVE Analysis has for its object the determination of the number and nature of the constituents of
elements.
more important.
Usually, the
is
the formation
The
together.
due to the interaction of the substances in solution giving
rise to the production of
is
reagents.
12
INTRODUCTION.
following:
I.
insoluble in water,
by hydrochloric acid
They
Group
II.
(or, indeed,
Group
the
groop
reagents must be
commencing systematic
analysis.
perfectly
13
INTRODUCTION.
presence of
ammonium
chloride.
Group
They
and which,
ammonium
They
are
there
is
" of the
Special notice should be taken of the words
in
the
above
remaining metals," which appear so often
I.,
II.,
and
III.,
precipitated.
a,
special or confirmatory
14
test.
INTRODUCTION.
or special reactions.
It must be carefully borne in mind that analysis is
founded upon a knowledge of the properties of the metals
and acids, and is really an application of such chemical
to the question in hand.
The student should,
all cases endeavour to clearly understand the
changes which are produced in the various
knowledge
therefore, in
chemical
made use
of
l2
= BaS0 + 2NaCl.
4
Such
even in simple
basicity of acids.
CHAPTER
IXTROD VCTOR Y
I.
EX. PERIMENTS.
it
on a
table.
Take a
Taking hold
hand near the
file.
to bend it away
and at the same time trying to pull
it apart.
The cat ends must then have their sharp edges
rounded by holding the tube vertically in the Bunsen
flame, until the flame is coloured strongly yellow by the
sodium of the glass.
from the
file-scratch,
to make a jet.
Take a short piece of tubing and heat the middle portion
in a small blowpipe flame, supporting each end of the
tube with the fingers, and continually turning it round so
16
when
the tube
is
quite soft,
The
the
the
the
Use of Spatula.
quantity of
some
It is often necessary to
take a small
For
this
To
fix
Take
spiral.
Flame
17
fl)
heat
it
On now
described above.
tube or bottle.
Na B 4 O 7 = 2NaB0. B O
2
3,
18
pound
with
MnS0
e.g.,
tlie bead,
Bunsen
nisable.
19
different
centre.
the charcoal.
KNO
and, having
S
(2) Take some potassium nitrate,
placed it on charcoal as described in (1), bring the blowpipe flame to bear on it. It suddenly flares up, and burns
a portion of the charcoal with it. This is deflagration.
(3) Take weights of powdered sodium carbonate,
Na 2 C0 3 and potassium carbonate. 2 CO S proportionate
to their molecular weights, and mix them thoroughly.
This mixture is known as fusion mixture, and should
be kept ready for use. Take a small quantity of litharge
(lead oxide), mix it with three or four times its weight
of fusion mixture, and heat the mixture on charcoal
before the blowpipe. The mass fuses, and in a short
time small globules of lead appear and are readily
fused into one large globule.
The use of the fusion
mixture is twofold it prevents the fused litharge from,
being absorbed by the charcoal, aud the fusion and reduction are more easily effected than in experiment (1). The
fusion mixture here acts as a, flux.
,
Note.
When a substance is to be reduced, it should be
heated on charcoal, with some suitable flux, in the reducing
If oxidation is to be effected, it should be heated
flame.
on the platinum wire, or on a piece of platinum foil in the
oxidising flame.
20
yellow when hot and white when cold. Now moisten the
mass with a few drops of cobaltous nitrate, and again
heat in the outer flame. The mass now assumes a fine
green colour.
(5) Take a small quantity of tin oxide, and mix it with
place the mixture
powdered potassium cyanide, KCy
on charcoal, and cover it over with a little KCy, then
;
KCNO
or
KCNS.
Sublimation.
(1)
21
(2)
tube.
KCy
2'2
small quantity of
it
fill
to
wash
all
Bunsen flame
crystallizes out.
above.
treat as
is
The
car-
23
effervescence,
carbonic acid
One
"
Two
This law expresses the principle of testing by precipiFor example, take a solution of barium chloride
in a test tube and add to it a small quantity of a solution
tation.
of
magnesium
MgS0
sulphate,
decomposition is possible
BaCl.2 -f MgSO4
4.
The following
double-
= BaSO + MgCl
4
(soluble)
Now
and
acids,
Mg
Ba (N0
3) 2
+ Na
S0 = BaSO + 2NaNO
4
(soluble)
24
be used
The funnel and filtering paper are arranged as already
described, but, instead of allowing the filtrate to drop
n
directly from the funnel into the test tube or other
U
vessel, fit to the lower end of the funnel, by means
of a short length of indiarubber tubing, a piece of
narrow glass tube bent round upon itself, near its
upper extremity, as in the diagram
The bend insures that the liquid shall entirely fill the
:
25
tube,
and there
is
scription.
Take a
To fold a pleated or folded filter paper.
circular piece of filtering paper and fold it in half, then
again, and again in half, then open so that its outline is a
semicircle; the creases produced by the other foldings are
merely to serve as guides. Then, beginning at the straight
side (i.e., the diameter of the circle of which the paper now
forms half), fold the paper from the centre to the circumference as far as the first crease ; then turn the whole paper
over, and fold the folded portion back an equal amount on the
other side; and so on, uutil the whole paper is folded into
a.
Press the paper well so as to render
sector-shaped piece.
the creases distinct, and then open it.
conical, pleated
filter will thus be formed which, when supported by a
funnel, will allow a liquid to flow through with great
rapidity.
Filtration.
Take a
solution of
barium
chloride,
BaCl 2
26
water has
all
filtered
through.
soluble in
AmHO.
This
is
most ordinary
is
applicable only
to-
27
Sulphuretted Hydrogen.
form of
28
CHAPTER
II.
work of analysis is
for, by successive application of the
simplified
group tests, we readily determine the group to which the
given substance belongs. In this way the field of investigation is narrowed, and it only remains to determine, by
special tests, what particular member of the group we
have to deal with. For this reason it is important to
note in the following reactions the special tests which
serve to distinguish the different members of each group
from one another.
After going through all the tests for the members of
on page 78 may be followed, until
each group, Table
By
much
the group
is
oO
GROUP
I.
SILVER, Ag
LEAD, Pb
.
MERCURY,
'Hg'
(white).
SILVER, Ag.
Solution
1.
acid,
HC1, gives a
2. Potassium chromate,
2 Cr0 4 ,
gives, in neutral*
solutions, a dark red pp., which, on the addition of HC1,
becomes white on account of the formation of silver
chloride.
3. Potassium cyanide, KCy, gives a white curdy pp.,
very soluble in excess of KCy. Rubbed upon a bright
This
piece of copper, a white stain of silver is produced.
stain does not disappear on heating.
Silver nitrate
is
the only
common
In that
Pb.
LEAD,
Solution
31
Lead Nitrate,
Pb(MTO,).
[Distinction
from Bismuth.~\
tation.
5. Heat on charcoal with sodium carbonate, Na 2 C0 3
and potassium cyanide, KCy beads of lead are formed,
which are malleable, and mark paper.
Common
Pb(C 2H 3
soluble salts.
2 ) 2,
32
MERCURY
Solution
(mercurous') 'Hg'.
,
Mercurous Nitrate,
Hg (NO
2
3)2
chloride,
NH
AmHO
ammonium
chloride.
p. 35.]
metallic globules.
5.* Acidulate a portion of a solution of any mercurous compound in a tube with hydrochloric acid, and
film of
boil with a strip of pure electrolytic copper.
mercury is deposited on the copper. When dried between
blotting-paper and heated in a tube, the mercury sublimes
and the copper resumes its natural colour.
Mercurous
curous
nitrate,
Hg 2 (NO 3
) 2,
is
the only
common
soluble mer-
salt.
Compare Reinsch's
GROUP
33
II.
H S in presence of HC1.
2
DIVISION
I.
MERCURY, Hg"
LEAD,* Pb
BISMUTH, Bi
COPPER, Cu
CADMIUM,
HgS
(black).
Cd
DIVISION
(i/eMow).
II.
Sn iv
(Stannic)
ANTIMONY,
Sb.
ARSENIC, As
....,,
Antimony Sulphide, Sb 2 S3
(orange).
(yellow).
*
Lead, as PbCl 2 is slightly soluble in cold water, and therefore
occurs in Group II. as well as in Group I.
,
ANAL.
34
As 2 S s
As 2 S s + 3(NH 4 ) 2 S
in the case of
= 2(NH
4 ) 8 AsS,.
soluble in water,
is the
analogue of ammonium arsenite, (NH 4 ) 3 As0 3 sulphur
replacing oxygen, and is hence called ammonium sulph-
is
arnenite.
In the case of antimony sulphide, similar reactions occur but in the case of tin a slight difference is found. With
stannic sulphide the reactions are
and
and
35
DIVISION
MERCURY,
Solution
I.
Hg".
Mercuric Chloride,*
HgCl.,.
the reagent
and
is
added,
finally black.
first
becomes
The black
pp.
is
yellow,
then brawn,
HgS.
yellow,
potassium iodide.
4. Sodic hydrate, NaHO, when added in excess, gives a
insoluble in excess.
yellow pp. of mercuric oxide, HgO
salt or of
5. Repeat reactions
will be obtained.
Similar results
Mercuric chloride, HgCl 2 (corrosive sublimate) is the most important soluble mercuric salt. Mercuric nitrate, Hg (N03 ) 2 is alsosoluble, but the salt is unstable, and when in solution tends to form
,
*
Sulphuretted hydrogen may be used as a solution in water, or
the gas itself may be passed into the solution from a suitable apparatus (see p. 28) until the precipitation is complete. The latter
is
preferable.
36
LEAD,
Fb.
BISMUTH,
Bi.
Bismuth Nitrate,
Solution
1.
S gives a brmonish-black pp. of bisrnuthous sul2
phide, Bi.2 S s
2. Water added in large quantity to a solution of bismuth, to which HC1 or ammonium chloride, AmCl, has
first been added, produces a white pp. of a basic chloride
BiOCl, which is insoluble in tartaric acid. [Distinction
from the basic chloride of antimony, SbOCl, which is soluble
in tartaric acid.]
3. Potassium chromate,
2
4
gives a yellow pp. of
the basic chromate, Bi 2 (Cr0 4 ) 2 O, soluble in dilute nitric
acid, but insoluble in sodium
[Distinction
hydrate.
.
K O0
from
4.
leadJ]
tinction
from
H S0
2
4,
gives no pp.
\_Dis~
leadJ}
COPPER,
Solution
37
Cu.
-Cupric Sulphate,
CnSO
4.
of
in
copper salts.
4. Potassium cyanide, KCj, gives a greenish-yelloio pp.
of cupric cyanide, CnCy2 which is soluble in excess.
S produces no pp. from this solution.
2
5. Sodium hydrate, NaHO, gives a bulky light blue pp.
be added,
of cupric hydrate, Cu(HO) 2 if excess of
and the mixture boiled, the pp. becomes black, having been
converted into cupric oxide, CuO.
6. If a piece of bright iron be dipped into a cupric
solution acidulated with HC1, it becomes coated with
copper if clean iron filings be boiled in the solution, it
will lose its blue colour, the copper being wholly displaced
by the iron.
,
NaHO
7.
cyanide,
for
some time
salt
38
CADMIUM,
Cadmium
Solution.
Cd.
Chloride, CdCl,.
1.
S gives a, fine yellow pp. of cadmic sulphide, CdS,
2
soluble in dilute sulphuric acid; the precipitation is prevented by presence of much HC1.
[Distinction from
copper:]
2.
hydrate,
Cd(HO) 2
wltite pp. of
cadmic
insoluble in excess.
cyanide,
is
completely volatilized.)
nitrate,
39
DIVISION
TIN
II.
(Stannous), Sn".
Solution
HS
stannous
1.
Am CO,.
2AuCl s +3SnClj + 6H 2
is
pp.
a strip of zinc to a solution acidulated with
HC1 it becomes coated with a spongy mass of metallic
tin.
Platinum-foil, in contact with the strip of zinc, does
not becomes blackened. [Distinction from copper and anti-
Add
4.
mony.]
5.
cyanide,
TIN
Solution
1.
3.
SnS2
Mercuric chloride,
from stannous
Sn
iT
.
Sulphuretted hydrogen,
of stannic sulphide,
2.
(Stannic),
HgCl
2,
gives no pp.
[Distinction
salts.]
to stannic compounds.
salts of tin.
40
Solution
ARSENIC,* As.
Arsenious Oxide, As 4O 6
dissolved in
dilute HC1.
1. Sulphuretted hydrogen,
acid solutions)
2 S, gives (in
a lemon yellow pp. of arsenious sulphide, As 2 S 3 insoluble
in strong boiling HCl; readily soluble in a concentrated
solution of ammonium carbonate, Ain t COs
boiling if
:
necessary.
2. Add cupric
sulphate, CuS0 4 and then sodium
hydrate, NaHO, drop by drop, till in excess (to render the
a fine green pp. of arsenite of copper
solution alkaline)
(HCuAs0 3 ) is obtained.
,
antimony .]
If, while the gas is still escaping, the delivery tube be
heated by the flame of a Bunsen burner or spirit lamp, at
a point a short distance from the jet, a black ring will be
produced on the tube just beyond the flame. If the tube
be now cut off at this point, and held in a slanting position
over a flame so that the ring is gently heated, a sublimate
of octahedral crystals will be formed at the jet end of the
If the tube, with the sublimate, be dropped into a
tube.
test tube containing dilute HCl, the As 4 6 dissolves and a
T
* Arsenic, when
present as an arseniate, that is, as As is only precipitated as AsjS 3 by passing the solution through the gas for some time.
In this form arsenic will be detected as an acid, (see page 67).
,
41
from which
Hoffmann's Test.
will precipitate
As 2 S $
By
test,
in solution
more
ammonia
recognised by its blackening a piece of filter paper previously moistened with AgN0 3 and held over the mouth
of the test-tube.
[Distinction from antimony, the compounds of which are not reduced in alkaline solutions to
,
SbH,.]
6. Reinsch's Test.
The solution is mixed with HC1,
and boiled with a clean piece of copper-foil. A grey film
is deposited on the
The copper-foil, having been
copper.
washed and dried, is then heated in a narrow open tube
where the arsenic oxidises, and arsenious anhydride, As 4 O 6
,
is
crystals.
7. Mix with sodium carbonate, Na 3 C0 3 and
powdered
a black lustrous
charcoal, and heat in a small bulb-tube
metallic ring will be produced in the cool part of the tube.
This ring, when treated as in Test 3, gives exactly the
,
same
results.
in dilute
HC1
is
the only
common
arsenic compound.
42
ANTIMONY,
Sb.
Solution
dilute HC1.
1. Sulphuretted hydrogen, H 2 S, gives (in acid solutions)
inan orange-red pp. of antimonious sulphide, Sb 2 S s
:
soluble in
Am CO
2
s.
2.
of
acid.
Marsh's Test.
arsenic.
On
5.
Hoffman's Test.
Apply
is
solution
43
GROUP
III.
AmHO
IN
THE
IRON,
Fe'" (Ferric)
Ferrous salts are not completely precipitated in the presence of AmCl hence, before testing for iron in this
group, a few drops of nitric acid must be added and the solution
boiled in order to convert any ferrous salt present into a ferric salt.
If iron is found, the original solution must then be tested to discover
whether it was initially present as a ferrous or ferric salt.]
;
CHROMIUM, Cr
ALUMINIUM, Al
IRON
Solution
fi
(white).
(Ferric), Fe'".
AmHO
Ammonium
gives a reddish-brown
hydrate,
pp. of ferric hydrate, Fe 2 (HO) 6
2. Potassium ferrocyanide, K 4 FeCy 6 gives a dark blue
pp. of prussian blue, Fe 4 (FeCy a ) 3
1.
no pp., but
6 Fe 2 Cyi 2 , gives
green (very dilute xolutions) or brown coloration.
4. Potassium sulphocyanute, KCyS, gives the solution a
blood-red colour on account of the formation of Fes (CyS) 6
The colour of the solution is readily destroyed by a solu3.
Potassium ferricyanide,
a deep
is
HgCl 3
the
common
precipitation of hydrates
by the
to
is
AmHO.
44
IRON
(Ferrous), Pe".
Solution
AmHO gives
Fe(HO) which
2,
AmHO
pp.,
ammonium
salts.
ferric salts.^
4. Potassium snlphocyanate, KCys, produces neither a
pp. nor change of colour when the solution is free from a-
ferric salt.
5.
and
Ammonium
Ferrous sulphate,
salts of iron, Fe".
is
Am
ferric solution
common
FeS0 4
Ferrous
(green
vitriol),
ammonium
is
the
sulphate,
45
CHROMIUM,
Solution
1.
Cr.
.
ti
AmHO
Cr2 (HO) 6
Potassium hydrate,
in several
ways
By
(1)
NaHO
(i.)
Cr,Cl,+6KHO = Cr,(HO),+6KCl.
Soluble in excess of
(ii.)
KHO.
When
KHO.
the solution
is
= 2Na,Cr0
+ SNaCl + 5H
O.
PbCr0 4
Chromium compounds
yellow pp. of
4s.
46
ALUMINIUM,
Solution
Al.
AmHO
HPO
AmHO
AmCi.
Heat on charcoal before the blowpipe a white mass
obtained which is highly luminous while hot. Moisten
with cobaltous nitrate, and heat again in the inner name a
fine blue mass is obtained.
[Distinction from zincJ]
4.
is
aluminium
common
is
common
alum.
is
NH
GROUP
2
S, IN
AmHO
Group-reagent
NICKEL, Ni
COBALT, Co
...
.
NICKEL,
Solution
Am S.
2
MANGANESE, Mn
ZINC, Zn
IV.
METALS PRECIPITATED
Am
47
Ni.
Am
2.
pp. of
to sherry-red
present.
when
cold,
Ni(NO 3)A
less deliquescent.
48
COBALT,
Co.
Solution
All
[Note that the colour of the solution is a pale red.
aqueous solutions of cobalt salts are of a reddish colour.]
Am
1.
S gives a Hack pp.
2
insoluble in excess of Am.2 S.
of cobalt sulphide,
CoS
o.
AmHO
presence of
gives
AmCl.
bluish-green
pp.,
not
formed in
cold
with strong
sodium hypochlorite,
NaOCl, gives
no pp.
5. The borax bead is coloured blue in the outer and
inner flame by cobalt compounds.
49
MANGANESE, Mn.
Solution
1.
Am
Manganous Sulphate,
MnSO 4
S gives a
2
sulphide,
MnS
acetic acid.
and Zn.]
is
prevented.
AmHO
ganese
salt,
III., but the precipitation does not take place until after
Ferric hydrate is preexposure to the air for some time.
cipitated immediately.^
KN0
when
colourless.
MnSO
unstable.
ANAL.
50
ZINC, Zn.
Solution
1.
Am
ZnSO
Zinc Sulphate,
2. Sodium, hydrate,
Zn(HO) 2
from aluminium.^
[Distinction
3.
Potassium ferrocyanide,
Zn FeCy6
2
K FeCy
4
nitrate,
Co(N0
becomes
green.
3)2
it.
vitriol,
Zn(C 2 H 3
; ) 2.
ZnS0 4 7H 2 0),
,
51
GROUP
V.
AmHO.
AlUjjCOj,
Group-reagent
BARIUM, Ba
STRONTIUM, Sr
CALCIUM, Ca
IN
THE
1.
Ammonium
OF
AmCl
AND
(white).
BARIUM,
Solution
AMMONIUM CAR-
PRESENCE
Ba.
Barium Chloride,
Am C0
Carbonate,
barium carbonate.
Bad
baric
of
salts
insoluble
in
dilute
acids
and
alkalies.
barium.
of
dilute solutions.]
crystalline
nitrate
Ba(NO3
)2
are the
52
STRONTIUM,
Solution
Sr.
Strontium Chloride,
1. Ammonium Carbonate,
strontium carbonate, SrCO 3
Am CO
2
SrCl,.
acid,
4. Strontium
crimson.
intense
compounds
of strontium.
53
CALCIUM,
Solution
1.
Ammonium
Ca.
Am C0
Carbonate,
of calcium carbonate,
CaC0
Am
2. Ammonium, oxalate,
2C2
4 gives a white powdery
pp. of calcium oxalate even in largely diluted solutions.
The pp. is insoluble in acetic and oxalic acids, but is
readily soluble in nitric and hydrochloric acids.
,
concentrated
,
[CaS0 4
4.
acid,
5.
of calcium
most
54
GROUP
No
MAGNESIUM,
VI.
Group-reagent.
SODIUM, Na.
Mg.
AMMONIUM, NH
POTASSIUM, K.
(Am).
MAGNESIUM, Mg.
Solution
no
because of the formation of the soluble double chloride
In the
of ammonium and magnesium, 2AmCl MgCl 2
absence of &mCl, part of the magnesia is precipitated as
the hydrate Mg(HO) 2 the double chloride being also
formed at the same time, thus
1.
pp.,
2MgCl
[The double chloride formed in the presence of AmCl is not precipitated by AmCO 3 hence magnesium is not precipitated in Group
V., provided a sufficient quantity of AmCl be present.
;
2.
Hydrogen
AmHO
presence of
of ammonium
The
4
magnesium phosphate,
separation from a dilute solution of a salt of magnesium
is promoted by heating gently and stirring with a glass
rod.
Very dilute solutions give a precipitate only after
standing some hours in a warm place.
3.
MgAmPO
55
POTASSIUM, K.
Solution
1.*
and add
PtC) 4
violet.
Owing-
method is not very reliable, and, unless the potassiumflame is very distinct, its presence will need careful
confirmation in the wet way.
this
The
the most
* Potassic
iodide,
formation of a
soluble
KI,
is
double
56
SODIUM, Na.
and
1.
2.
Potassium metantimoniate,
KSb0
3,
crystalline
3s*
gives
a white
NaSbO s from
,
yellow.
[This test is the most reliable for sodium, but it must be remembered that traces of sodium are always present, so that a faint
yellow coloration of the flame may in general be neglected. When
sodium is present in quantity, the colour is characteristic and very
intense.]
AMMONIUM, NH (Am).
Ammonium Chloride, AmCl.
4
Solution
chloride, PtCl 4
2.
NH
2AmCl.
Add NaHO
or
KHO,
Ammonia,
S,
3.
test tube
white sublimate
All
ammonium
of the tube.
salts are volatilized or decomposed by heat.
pp. of
NHg I.OH
2
2,
sulphate, bromide,
chloride, carbonate,
CHAPTER
III.
THE
SULPHURIC ACID, H SO
2
4.
Solution
is
present.
2.
Lead
acetate,
Pb(C 2 H 3
PbS0
of lead sulphate,
2) 2,
ACID, H SO 3
Sodium Sulphite, Na SO
SULPHUROUS
Solution
3.
the smell of
1. Add HC1, and, if necessary, heat
burning sulphur is perceptible, S0.2 being evolved ivithout
:
To some
little
;
sulphide.
H SO +3H = H S + 3H 0.
2
3.
Barium
chloride,
pp. of
BaSO
s,
58
ANALYSIS OF A
SllIl'LE
HYPOSULPHUROUS ACID
HS
2
Solution
SALT.
(Thiosulphuric Acid},
8.
2. Silver nitrate,
added gradually, in excess,
3
The pp.
gives, after some time, a white pp., Ag 2 S 2 3
slowly decomposes, becoming yellowish brown and then
thus
black, forming silver sulphide,
2 S,
AgN0
Ag
Ag
S2
+H = Ag S + H S0
2
HYDROSULPHURIC
Solution
ACID,
4.
H S.
2
Sulphide, Am.S.
1.
off,
Ammonium
black stain
acetate
cadmium
sulphide^ CdS.
Heat a dry sulphide in a piece
of glass-tubing held
obliquely over a flame in general, sulphur dioxide gas,
which may be recognised by its odour, is given off.
Tests 2 4 are applicable to the detection of H 2 S as an aqueous
4.
given
off.
HYDROCHLORIC
Solution
59
ACID, HC1.
AgNO
s
gives a white curdy pp. of
insoluble in strong boiling nitric
acid (silver cyanide, AgCy, dissolves) soluble in solution
of ammonia.
1. Silver nitrate,
silver chloride, AgCl
is
fumes
of
HC1.
3.
Potassium Chlorate,
KC1O
.
;
Note.
in water
hence the
is
"needle"
60
HYPOCHLOROUS
ACID, HC1O.
filter off;
:
HYDROBROMIC
ACID, HBr.
Solution
AgN0
1. Silver nitrate,
3 gives a yellowish white pp. of
silver bromide, AgBr: insoluble in dilute nitric acid;
slightly soluble in ammonia.
,
Mix with
Mn0
and
H S0
is
ANALYSIS OF
SIMPLE SALT.
HYDRIODIC ACID,
Solution
61
HI.
AgNO
1. Silver nitrate,
s
gives a yellow pp. of silver
iodide, Agl insoluble in nitric acid, and nearly insoluble
in solution of ammonia.
,
\_If too
much
blue.
glass.
62
Silver nitrate,
cyanide,
AgN0
AgCy, which
is
3
gives a white pp. of silver
at first redissolved, but remains
,
Am
tests for
hydrocyanic acid.
63
H FeCy
Ferrocyaiiide, H FeCy
HYDROFERROCYANIC
Solution
Potassium
ACID,
6.
Ag FeCy6
4
insoluble
air.
3. Ferric chloride,
4.
Copper sulphate,
Fe
CuS0
4,
cupric ferrocyanide.
Potassium Ferricyanide,
is
the only
Ferrous sulphate,
(TurnbuWs
H Fe
common
FeS0 4
Cy
12 .
Fe,Cy u
ferri cyanide.)
gives a
blue).
2. Ferric chloride,
or greenish coloration.
Fe 2 Cl 6 gives no
pp.,
Ag8 Fe Cy
2
12 ,
64
NITRIC ACID,
Solution
1.
3.
KNO
FeS0 4
When
and dissolve in
of the nitrate,
it
HNO
Potassium Nitrate,
H S0
2
quite cold,
to
form a
brown-
tated as a carbonate.
2. Heat with concentrated sulphuric acid and copper
turnings: nitric oxide, NO, is given off, which becomes
O 4 in the upper part of the tube from
nitric peroxide,
2
absorption of oxygen.
3.
A nitrate heated
on charcoal deflagrates.
Note.
no
pi-ecipitation reactions.
gas,
mixed with
are
coloration
HN0
3.
with.
H S0
2
CARBONIC ACID, H CO
2
65
Note.
on
boiling,
C0 2
2KHC0 = KC
no pp. fs^
2. Add NaHC0 3 to a solution of MgS0 4
formed, but on boiling the solution a white pp. of MgC0 3
The normal carbonate, N"a 2 C0 3 gives
is quickly formed.
a pp. of MgC0 3 at once.
:
BORIC ACID,
Solution
Borax,
H BO
3
.
;
Na B .O
wet a piece of
1. Add HC1 to a solution of borax
turmeric paper with the solution. The paper when dried
becomes reddish brown, and, on treating with dilute
;
Dry
the paper by coiling round the exterior of a test-tube, parwith water, and boiling the water in the tube over the*
tially filled
Bunsen
flame.
dish,
66
SILICIC ACID,
Sodium
Solution
Si04
Silicate,
Na SiO
4
1.
ness
when
cold,
white flakes of
2.
salt
silica,
Si0 2
will
remain undissolved.
PHOSPHORIC ACID, H FO
8
Solution
1.
Silver nitrate,
AgNO
.
;
phosphate,
2.
and,
magnesium
sulphate,
MgS0 4
AmMgPO
Ba 3 (P0 4) s
67
1.
Solution
Silver nitrate,
arsenate,
Ag As0 4
3
AgN0
[Distinction
Ammonium
2.
magnesium
AmMgPCv
3.
Ammonium
on boiling, a
4.
Add
molybdate,
AmHMo0
in excess gives,
4,
yelloiv pp.
heat to boiling,
pnateJ]
if
H 2 S.
sulphurous acid be
Solution
Arsenious Oxide,
As,O,,, dissolved in
68
.
t
CrO,.
AgN0
Silver nitrate,
chromate,
Ag Cr0
2
On adding
solution
2H Cr0 4 + 3H S0 8
2
3.
Lead
PbCr0 4
4. On passing a current of
2S
gas through an acid
solution of a chromate, reduction takes place the solution
becomes green owing to formation of chromic chloride,
;
is
precipitated.
2K,Cr0 4 + 3H 2 S + 10HCl
Note.
Thus
fl
Group
II.
it is
CHAPTER
IV.
SYSTEMATIC ANALYSIS.
below, I.-VI.
I.
SUBSTANCE.
On
must be
his guide,
under
his notice.
subtances, as they
marked
characteristics
It is useless to
must be seen
to
all
sub-
which come
70
HEAT A SMALL
II.
IN A BULB-TUBE IN
INFERENCE.
OBSERVATION.
1.
and
solidifies
The
2.
substance
changes
colour
Yellow while
(a)
on
white
brown when
From white
(fc)
hot,
cooling.
to yellowish
ZnO.
>
SnO.
yellow on cooling.
(c)
hot, yel-
(d)
From
")
s.
white to orange
Fe 2
From
yellow to reddish
hot, yellow
cold, fusible at a red
Bi,0 s
brown while
when
PbO.
heat.
3.
The
substance
off
gives
shrinks.
rates.
71
continued.
II.
INFERENCE.
OBSERVATION.
5. The substance volatilizes
and condenses as a sublimate
(a) Reddish
when
drops,
yellow
S,
Sulphur or a sulphide.
cold.
which HgS.
becomes red on rubbing.
A Si S s
(c) Yellow sublimate.
As,0 s
(d) Sublimate of small white
(&) Black sublimate,
HgI 2
octahedral crystals.
6.
(a)
evolved
is
gas
(test
with
glowing
(6)
Brown fumes
(c)
NH
of
4.
CO, (lime-water
NH
4,
combined
reaction).
(e)
splinter).
test).
Iodides.
(/)
(0)
Cl (bleaching power,
smell and colour).
S0
(smell).
pounds.
(A)
(CX)
(smell,
coloured flame).
rose-
Cyanides
metals.
of
heavy
72
III.
HEAT A SMALL QUANTITY OF THE SUBSTANCE IN A
TEST-TUBE WITH A LITTLE DILUTE HC1.
INFERENCE.
OBSERVATION
A gas is evolved
(a) C0 (lime-water
1.
(6)
test).
HS
2
Carbonates.
Sulphides, except those
of the metals of Group
II.
(c)
S0
(smell of burning
2
sulphur)
H,SO S
(d)
S0 and
2
separation of
yellow sulphur.
(e) Cl (smell,
and bleaching
HCy
(smell
almonds)
HC10
or
oxidizing
test).
</)
H,S,0,.
of
bitter
Cyanides.
73
OBSERVATION.
It decrepitates.
1.
It fuses
charcoal.
2.
and sinks
into the
Alkaline
salts.
It deflagrates.
Chlorates, nitrates.
Alkaline earths, A1 2 O5
3.
Si0 2 ZnO.
,
Co(NOs \ and
strongly heated, is
coloured.
A1 2
Blue.
S,
phosphates
and
silicates.
6.
coloured residue
is
left
MgO.
ZnO, Sb.
Cu, Co, Ni, Mn, Fe, Cr.
on the charcoal.
7.
An
incrustation
is
formed
on the charcoal
(a) White incrustation.
Am, Hg.
(6)
(c)
Yellow
when
when cold.
hot,
Reddish brown.
white
As.
Zn.
Cd.
74
OBSERVATION.
1.
A white
(a)
which,
malleable bead
Pb.
marks
paper
(yellow incrustation on
charcoal).
white
Soft,
(b)
bead
malleable
Sn.
(slight yellowish
incrustation).
Hard white
(c)
bead (no
(d)
White
malleable
Ag.
incrustation).
brittle
bead
(yel-
Bi.
low incrustation).
(e)
Sb,
tion).
2.
Red
3.
Magnetic
Cu.
infusible scales.
metallic
parti-
cles.
produced.
Sulphur compounds.
VI. IP
THE
SUBSTANCE
IS
BEAD.
OBSERVATION.
COLOURED,
HEAT
75
ON
BORAX
76
If the
substance
is solid, it
then try
if it is
Note.
It
will
generally be
found
unnecessary to
employ aqua
2.
If
powder
the substance
it
for,
acid.
(6)
HC1
77
If the substance is
If the reaction is
may
KOH
,
be present.
(c) Neutral.
may
salts,
be present.
II.
PQ
*
in
o
-
fl
iBH,
'S
-C
rJ
rC
Jl
O 3-
O o O
o O
I
P<
PH
o
PH
P.
fa
"1 s
o)
""
t-T
Is Ji
8
t*>
V2
to
".s
.s
-
'O
03
I I
&
1^
aa
-^-^
co
co"
a?
"
co jg
co OQ
cq^
-(J
^
^
t^
P"C
K.
ai^js
^^^
s"
grS"S"S2o
.s
.
.2 tT
o3
HhHuuw n^u
03
03
P ,C J3
2 3
M^^
t_5
-~
,j?
.J
5-5
"
S
S 'S
B-
o o
*!
rt
*5<
TABLE
I.
I.
H
r-3
M
<1
EH
TABLE
VI.
84
way.
(6) The result of the examination for the lase. The base
being now known, and the properties and solubility of the
substance being determined, the field of search is often
considerably narrowed. If no acid is found, the substance
may be an oxide or hydrate, and here again a knowledge of the nature of the base helps to decide whether
such a compound is likely to occur.
Preparation of Solution.
The substance is in solution or soluble in water.
Groups I. or II. be present, remove them
by boiling with a slight excess of pure sodium carbonate,
filter, and use the filtrate for the examination for acids.
If Groups I. and II. be absent, use the original solution.
1.
If metals of
3.
The substance
is insoluble.
HN0
HN0
To
INTEREVCE.
solution
add
pp., insoluble in
HC1.
neutral
85
Bad.,.
White
White
(or
H PO H S0 H B0
H Si0 H SA (pp.
HC1.
pp., soluble in
H S0
Presence of
KiF 6 ).
2
4,
3,
3,
4,
but
dissolves,
is
H C0
2
(pp. dissolves
effervescence),
with
H,C,0,
H Cr0
Yellow pp.
2.
To
AgNO
(a)
another
add
portion,
HNO
pp. soluble in
soluble
i. White,
in
"Yellow.
Red.
iv.
Dark
4,
red.
HN0
pp. insoluble in
i.
White, soluble
4,
As0 4
CrO 4
Yellowish
Yellow,
in
iv.
v.
HC1,
white
HBr.
am-
vi.
insoluble
ditto,
Orange-red, soluble
in
HI.
H S.
H FeCy
2
ammonia,
White, insoluble in
ammonia.
HCN, HC10.
ammonia,
Black,
monia,
iii.
3.
in
in
soluble
ammonia.
ii.
H,C0
4,
iii.
ii.
HNO,,
H Si0 H B0
H P0 H As0
ammonia,
(6)
H FeCy
4
a.
3,
OBSERVATION.
If
no pp.
BaCl 2 or
is
AgNO
produced
by
3. To a portion of solution
add a solution of FeS0 4 and
then pour down the side of the
S0 4
See
test-tube strong
2
,
Note, p. 64.
brown
ring formed at
junction of fluids indicates
HNO
strong
H S0
2
HC10,
tonation indicates
If
no acid
is
detected by
1,
2, 3, or 4.
5.
To a fresh portion
add Fe 2 Cl 6
solution
of the
by
dicates
H Fe Cy
H FeCy
6
HCyS.
12 .
APPENDIX
I.
MODEL ANALYSES.
KJ
<
wi
APPENDIX
III.
1881.
Potassic Carbonate, Sodic Chloride, Calcium Chloride,
Ammonic Chloride, Manganous Sulphate, Barium
Chloride, Zinc Sulphate, Ferric Chloride, Lead Nitrate,
Ferrous Sulphate, Antimonious Chloride,
Magnesic
Chloride, Bismutii Nitrate, Boracic Acid, Mercurous
Nitrate, Nickel Sulphate, Alum, Stannous Chloride.
1882.
Potassic Carbonate, Sodic Chloride, Calcium Chloride,
Ammonic Chloride, Manganous Sulphate, Barium
Chloride, Zinc Sulphate, Ferrio Chloride, Lead Nitrate,
Ferrous
Antimonious Chloride, Magnesic
Sulphate,
Chloride, Bismuth Nitrate, Boracic Acid, Mercurons
Nitrate, Nickel Sulphate, Alum, Stannous Chloride.
1883.
Sulphate, Barium Nitrate, Bismuth Nitrate,
Sodium Phosphate, Ferrous Sulphate, Potassium Nitrate.
Cadmium
1884.
Nitrate,
Cadmium
1885.
Mercuric Chloride,
Iodide,
Ammonium
Chloride,
Potassium
Zinc Sulphate, Potassium Chlorate, Ammonium Phosphate, Sodium Carbonate, Barium Chloride, Manganese
Sulphate, Sodium Chloride, Nickel Sulphate, Silver
Nitrate, Calcium Chloride, Sodium Thiosulphate, Sodium
Arsenite, Bismuth Nitrate, Mercurous Nitrate, Cadmium
Nitrate.
ANAL.
APPENDIX.
98
1886.
Mercuric Chloride, Manganese Chloride, Ferrous Sulphate, Zinc Sulphate, Lead Nitrate, Barium Nitrate and
Chloride, Calcium Chloride, Sodium Phosphate and Thiosulphate, Potassium Chloride, Bromide, Iodide, Sulphate,
and Carbonate, Ammonium Chloride and Phosphate,
Magnesium Sulphate.
JAN. PREL. Sci.
Sodium Carbonate, Zinc Sulphate,
Ammonium Chloride, Manganese Sulphate, Sodium
Nitrate,
Manganese Chloride.
'
1888.
Nitrate,
ride,
Zinc Sulphate,
Ammonium
Phosphate.
1889.
Barium Chlorate.
lonfcon 3nter.
Sc
ant>
prelim.
Set,
BIOLOGY, CHEMISTRY,
AND
PHYSICS,
of
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H. DIBB,
J.
B.Sc.
Lond.,
Double
Physics.
0.
W.
J.
EVANS,
Honours.
B.Sc.
Teacher's Diploma.
J.
J.
Juris-
(Br. I. & IV.), Exhibitioner in Latin at Inter. Arts. Univ. Scholar in Classics at B.A.,
Gold Medallist at M.A. ; First Class, First Div., Classical Tripos
Assistant Examiner at London University; Author (with A.
H. Allcroft) of
History of the Early Pfincipate.
II.
Honours
at Inter. Arts.
Assistant
B.Sc., &c.
First Class
Honourman
in French.
and Honourman in
O.W
Classical Tripos.
ADVERTISEMENTS.
Successes
Cbief
t
.a-
r>"icfw2
I^iojqH TO!
t.
loJ/iT Laao
RECENTLY GAINED BY
"University Correspondence
Colleae.
*
JRI
-"*
wfl*
nni.iu'rT
.aajaO
AT MATRICULATION, JUNE,
~
189O,
'
1O5 U.
Students passed,
forming one-eighth of the entire list,
with lOth, 13th, and 17th places in Honours.
C. C.
In Jan., 1890,
78
In June, 1889,
'F
ni t>-ti5L
AT INTER. ARTS,
8O
2O
U. C. C. Students passed
and two with second
;
51
'
189O,
Inter. Sc.
2.
and Frel.
places.
Sci. Exams.,
Honours.
AT
also
'.
aoqhT
1889,
B.A.,
TO U. C. C. Students passed.
Of these 16 Students took Honours.
j
i
n x
v
i
a a it
v
passed at B.Sc., 2 of whom headed Honour lists.
-r
iBioM
ni
AT
M.A.. 1890.
'
......
Students of Univ. Corr. Coll. passed.
8o-moi.->,
5
g^
i.
I.,
and
in 1888
---
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