Professional Documents
Culture Documents
PREFACE.-
OCTOBER, 1895.
LABORATORY MANUAL
OF
INORGANIC PREPARATIONS,
WATER.
H 2 O.
2 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 3
FIG. l.
LABORATORY MANUAL OF
case the condenser " sweats " from the use of very cold
water, the drip from the outside can not contaminate the
distillate. The lower end of the tin tube is cut aslant for
the more certain delivery of the distillate.
INORGANIC PREPARATIONS. 5
/X ^SE r UB^>
(UNIVERSITY;
Vc^?w.V
ETHYL ALCOHOL.
C 2 H 5 .OH.
6 LABORATORY MANUAL OF
INORGANIC PREPARATIONS.
OXYGEN.
O.
FIG. 3.
8 LABORATORY MANUAL OF
Na 2 O 2 + 2H.C1 = O + 2NaCl + H 3 O,
INORGANIC PREPARATIONS.
HYDROGEN.
H.
Hydrogen is best prepared from granulated zinc
and dilute sulphuric acid (i litre acid, 5 litres water) in
Kipp's Apparatus ; the zinc should not be too pure or the
supply of gas will be slow and feeble. In any case it is well
to add a small amount of copper sulphate solution, just
sufficient to produce a thin coat of copper on the zinc, 01
a piece of platinum foil may be used in place of the copper
sulphate ; in this latter case it is better to amalgamate the
zinc, by first treating with dilute sulphuric acid and then
adding mercury and shaking, or by simply treating the
zinc with a strong solution of mercuric nitrate containing
free nitric acid.
(tri
ID LABORATORY MANUAL OF
NITROGEN.
N.
NH 4 Cl + KNO 2 = N 3 + KC1 + 2H 2 O.
Cl.
INORGANIC PREPARATIONS. II
12 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 13
14 LABORATORY MANUAL OF
INORGANIC PREPARATIONS.
HYDROCHLORIC ACID, OR
HYDROGEN CHLORIDE.
HC1.
l6 LABORATORY MANUAL OF
FIG. 4.
NITRIC ACID.
HNO 3 OR NO 3 OH.
I 8 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 19
NITROUS OXIDE.
N 2 O.
20 LABORATORY MANUAL OF
NITRIC OXIDE.
NO.
INORGANIC PREPARATIONS. 21
NITROGEN TETRAOXIDE.
N34.
22 LABORATORY MANUAL OF
SULPHURIC ACID.
H 3 SO 4 OR SO 2 (OH) 2 .
a. Concentrated pure sulphuric acid.
INORGANIC PREPARATIONS. 23
4 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 25
HYDROGEN SULPHIDE. HYDROSULPHURIC
ACID. SULPHURETTED HYDROGEN.
H 3 S.
FIG. 6.
26 LABORATORY MANUAL OF
(trwivr.. SITY X
SULPHUR DIOXIDE.
S0 3 .
Cu + 2H 2 SO 4 = SO 2 + 2H 3 O + CuSO 4 .
It can be absorbed in water and used as a solution of sul-
phurous acid or absorbed in caustic alkalies forming
28 LABORATORY MANUAL OF
CARBON MONOXIDE.
CO.
INORGANIC PREPARATIONS. 29
30 LABORATORY MANUAL OF
AMMONIA,
NH 3 .
AMMONIUM HYDRATE.
NH 4 OH.
INORGANIC PREPARATIONS. 31
KOH,
32 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 33
IO 1.11$ 21 1-236
II I.I26 22 1-247
12 1.137 2 3 T - 2 5 8
13 1.148 24 1.269
i4-- --1-159 2 5 J - 2 79
15 1.170 26 1.290
16 1.181 27 1-300
17 1.192 28 1.310
1 8 i. 202 29 1-321
20 1.225
34 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 35
S " OF THE A
UNIVERSITY)
36 LABORATORY MANUAL OF
LEAD DIOXIDE.
Pb0 2 .
INORGANIC PREPARATIONS.
37
38 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 39
LEAD CARBONATE.
PbCO;{.
40 LABORATORY MANUAL OF
LEAD TETRACHLORIDE.
Pb.Cl 4 .
INORGANIC PREPARATIONS. 41
BISMUTH HYDROXIDE.
BiOOH.
AMMONIUM SULPHIDE.
INORGANIC PREPARATIONS. 4$
SODIUM SULPHIDE.
Na 2 S.
POTASSIUM SULPHIDE.
K 3 S.
AMMONIUM OXALATE.
(NH 4 ) 3 C 2 4 , 2Aq.
44 LABORATORY MANUAL OF
SODIUM ACETATE.
NaC 2 H 3 O 2 3Aq.
* STOLBA.
INORGANIC PREPARATIONS. 45
46 LABORATORY MANUAL OF
SODIUM.
OF THE
{ UNIVER
INORGANIC PREPARATIONS. 47
SODIUM AMALGAM.
(10%).
48 LABORATORY MANUAL OF
SOD'IUM CARBONATE.
(Na 2 CO 3 10Aq.)
INORGANIC PREPARATIONS. 49
* J. LAWRENCE SMITH.
50 LABORATORY MANUAL OF
POTASSIUM CYANIDE.'
KCN.
INORGANIC PREPARATIONS. 51
must contain neither silica nor potassium sulphide ; the
precipitate which lead salts produce in its solution must
accordingly be of a white color, and the residue which
its solution leaves upon evaporation, after previous super-
saturation with hydrochloric acid, must completely dissolve
in water to a clear fluid.
POTASSIUM SULPHOCYANIDE.,
KCNS.
52 LABORATORY MANUAL OF
POTASSIUM NITRITE,
KN0 2 .
INORGANIC PREPARATIONS. 53
54 LABORATORY MANUAL OF
POTASSIUM PYROANTIMONATE.
AMMONIUM MOLYBDATE.
CNH 4 ) 2 Mo0 4 ,
DISSOLVED IN NITRIC ACID.
MOLYBDIC SOLUTION.
INORGANIC PREPARATIONS. 55
AMMONIUM CHLORIDE.
NH 4 C1.
Select sublimed white sal ammoniac of commerce.
If it contains iron it must be purified by slowly pass-
ing chlorine gas into the nearly saturated solution for a
short time or until potassium ferricyanide gives no blue
color with a few drops of the liquid. Ammonia is then
added in slight excess, the whole is warmed, filtered from
the separated ferric oxide and evaporated to crystallization.
56 LABORATORY MANUAL OF
SODIUM NITRATE.
NaNO 3 .
2NaHP0 3 + 5H 3 0.
INORGANIC PREPARATIONS. 57
POTASSIUM CHLORATE.
KC1O 3 .
POTASSIUM BISULPHATE.
KHSO 4 .
INORGANIC PREPARATIONS. 59
POTASSIUM FERRICYANIDE.
60 LABORATORY MANUAL OF
POTASSIUM IODIDE.
K.I.
POTASSIUM CYANATE.
KCNO.
INORGANIC PREPARATIONS. 6 1
62 LABORATORY MANUAL OF
POTASSIUM METANTIMONATE.
K 4 Sb 2 O 7 .
INORGANIC PREPARATIONS. 63
64 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 65
TITANIUM TRIOXIDE.
Ti0 8 .
5
66 LABORATORY MANUAL OF
TiO 3 + 3H 2 O.*
INORGANIC PREPARATIONS. 67
X^C^^X
VANADYL CHLORH^iC^
AMMONIUM BICARBONATE.
(NH 4 )HC0 3 .
68 LABORATORY MANUAL OF
AMMONIUM BROMIDE.
NH 4 Br.
AND
POTASSIUM BROMIDE.
KBr.
4NH3+3Br=3NH 4 Br+N.
INORGANIC PREPARATIONS. 69
genes depends on the fact that ferric salts will set free
iodine from neutral solutions of the iodides :
70 LABORATORY MANUAL OF
AMMONIUM BICHROMATE,
(NH 4 ) 3 Cr 2 7 .
INORGANIC PREPARATIONS. 71
AMMONIUM NITRATE.
NH 4 NO 3 .
72 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 73
CUPROUS CHLORIDE.
CuoCte.
lBft^px.
. THOMAS, Be,, 2 o, 743.
W-.^^S
74 LABORATORY MANUAL oP
CuCl 3 + Cu = Cu 2 Cl 2 .*
CUPROUS CYANIDE.
(CugCN).,.
INORGANIC PREPARATIONS. 75
2Cu(CN) 3 = Cu 3 (CN) 3 + CN 3 .
(NH 3 ) 4 CuS0 4 .
CuK 3 (SO) 3 + 6H 3 O.
/6 LABORATORY MANUAL OF
CUPRIC SULPHATE.
CuSO 4 ,5H 2 O.
CUPROUS OXIDE.
CuoO.
INORGANIC PREPARATIONS*^; 77
78 LABORATORY MANUAL OF
CUPROAMMONIUM TETRA IODIDE.
4NH 3 CuI 2 ,I 2 .
CUPROUS PHOSPHIDE.
CugPg.
INORGANIC PREPARATIONS. 79
PURE SILVER. .
Ag.
80 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 8 I
AgKCO 3 .
82 LABORATORY MANUAL OF
PURE GOLD.
Au.
INORGANIC PREPARATIONS. 8$
AuCl 3 .
84 LABORATORY MANUAL OF
INORGANIC PREPARATIONS. 8/
Mg(OH) 2 ,MgC0 3 .
o /^*
100 C.
CaCl 2 .
88 LABORATORY MANUAL OF
* In place of this you can also proceed from the residue of ammonia
production, consisting of a mixture of calcium chloride and surplus lime.
Boil the same with water until the last traces of ammonia have passed away,
then filter and continue as stated above.
INORGANIC PREPARATIONS. 89
CALCIUM CHLORIDE.
CaCl 2 , crystallized +6H 2 O.
CALCIUM CARBONATE.
CaCo 3 .
90 LABORATORY MANUAL OF
CALCIUM CHROMATE.
CaCr 2 O 4 .
INORGANIC PREPARATIONS. 91
Zn.
by heat.
92 LABORATORY MANUAL OF
ZINC EISEN.
STRONTIUM HYDROXIDE.
Sr(OH) 2 + 8H 2 0.
INORGANIC PREPARATIONS. 93
94 LABORATORY MANUAL OF
CADMIUM CARBONATE.
CdC0 3 .
INORGANIC PREPARATIONS. 95
3CO 2 .
96 LABORATORY MANUAL OF
BARIUM CHLORIDE.
BaCl 2 + 2H 2 O.
a. From heavy spar. Mix together 8 parts of pul-
verized barium sulphate, 2 parts of charcoal powder, and I
part of common rosin. Put the mixture in a crucible and
expose it in a blast furnace to a long-continued red heat.
Triturate the crude barium sulphide obtained, boil about A
of the powder with 4 times its quantity of water, and add
hydrochloric acid until all effervescence of hydrogen sul-
phide has ceased, and the fluid manifests a slight acid reac-
tion. Add now the remaining A part of the barium sul-
phide, boil some time longer, then filter, and let the alkaline
INORGANIC PREPARATIONS. 97
BARIUM NITRATE.
Ba(NO 3 ) 2 .
98 LABORATORY MANUAL OF
BARIUM PEROXIDE.
Ba0 2 .
BARIUM PERHYDRATE.
Ba(OH) 4 + 6H 2 O.
BARIUM CARBONATE.
BaCO 3 .
Dissolve crystallized barium chloride in water, heat to
boiling, and add a solution of ammonium carbonate mixed
INORGANIC PREPARATIONS. 99
BARIUM DITHIONATE.
DITHIONIC ACID.
H 3 S 3 6 +xH 2 0.
cr~\ rr
DISTILLED MERCURY.
Hg.
101
FIG, 8.
PURIFICATION OF MERCURY.
MERCURIC CHLORIDE,
HgClg. (FROM RESIDUES.)
MERCURIC CYANIDE.
Hg(CN) 2 .
A diluted prussic acid solution is mixed in a flask with
yellow mercuric oxide until the solution reacts strongly
alkaline to litmus paper. Filter and add to the filtrate
enough prussic acid to make the odor of it noticeable and
so that the filtrate will react distinctly acid, then evaporate
to crystallization. Before the mother liquor is again evap-
orated to crystallization, add a little more prussic acid.
CINNABAR.
HgS.
MERCUROUS NITRATE
Hg 3 ( N O 3 ) 3 crystallized + 2 H 3 O .
MERCUROUS IODIDE.
Hg 2 I 3
INORGANIC PREPARATIONS. 1 07
MERCUROUS BROMIDE.
Hg 2 Br 3 .
BORON.
B.
BORAX.
Na 2 B 4 O 7 .
SILICON.
Si
SILICON CHLORIDE.
SiCl 4 .
ITY ''
ALUMINIUM HYDRATE.
Al3(OH)e,//w Cryolite.
A1 2 O 3 .
INORGANIC PREPARATIONS.
AloCl 6 .
HYDROGEN BROMIDE.
HBr.
C 6 H 6 +4Br = C 6 H 4 Br 2 + 2HBr.
The small quantity of ferrous bromide (FeBr 3 ) acts as
HYDROGEN IODIDE.
HI.
IODINE PENTOXIDE.
I25.
IODINE TRICHLORIDE.
IC1 3 .
HYDROCYANIC ACID.
HCN.
stand on ice ; the vapors escaping from the last bottle are
led into cold water. The insoluble residue* forming in the
retort causes a slight jolting of the contents, but by heat-
ing uniformly and carefully no danger need be feared.
The distillate is almost pure. If absolutely anhydrous
hydrogen cyanide is required, fill the first of the Woulfif
bottles before distillation half-way with porous calcium
chloride, and at the conclusion set it in warm water, in order
to distill its contents into the second bottle. The product
should not be preserved in an anhydrous, but in a diluted
condition ; the aqueous hydrocyanic acid keeps still better
if one drop of diluted mineral acid is added to every 100
c. c.
HF.
STANNOUS CHLORIDE.
SnCte, Crystallized + 2H 2 O.
SnCl 2 .
SnCl 4 .
PHOSPHORUS
FROM
H 3 P0 4 .
PHOSPHORUS TRISULPHIDE.
CALCIUM PHOSPHIDE.
CaP.
* For this purpose wind a little thin asbestos cord around the glass tube,
then twist it into the iron tube, after having moistened the asbestos with
water glass. The joints are covered with a pasty mixture of powdered
oxide manganese and water glass, then dried at moderate heat. The glass
tube must be sufficiently wide to conveniently allow the passage of the
phosphorus sticks.
HYDROGEN PHOSPHIDE.
PH 3 .
ARSENIC ACID.
H 3 AsO 4 .
2AsCl 5 4- 5H 3 S = As 3 S 5 + 10HC1;
2AsCl 3 + 3H 9 S = As 3 So + 6HC1.
HYDROGEN ARSENIDE.
H As.
The action of zinc on an acid solution of arsenious acid
produces a gas containing 70 per cent, by volume of hy-
drogen arsenide. Sodium amalgam containing not more
than 4 grams of sodium in 50 c. c. of mercury, by its action
on a concentrated solution of arsenious acid, produces a
gas containing 86 per cent, by volume of hydrogen arsenide.
A gas containing a large quantity of arsenic may be pre-
pared by the action of aluminium on a somewhat dilute
alkaline solution of potassium arsenite, while a solution of
arsenic disulphide in potash, when subjected to the action
of aluminium, evolves a gas quite free from arsenic.*
ARSENIC PENTASULPHIDE.
As 2 S 5 .
SbCl 3 .
ANTIMONY OXYCHLORIDE.
Sb 4 O 5 Cl 2 .
then dried.
ANTIMONIOUS SULPHATE.
Sb 2 (S0 4 ) 3 .
BISMUTH NITRATE.
Bi(N0 3 ) 3 + 5H 3 0.
BISMUTH HYDROXIDE.
B O OH.
BISMUTH IODIDE.
BiI 3 .
.S^$&& UBRxi/?p\
tTHIVEHSITY;
c*
BISMUTHIC ACID.
HBiO 3 .
Co(NO 3 ) 2 , Crystallized + 5H 2 O.
H3O3.
SULPHUR MONOCHLORIDE,
AND
SULPHUR DICHLORIDE,
SClg.
300 grams sulphur are heated to its melting point in a
tubulated retort over a low flame, and as in the case of tinte-
CHROMYL CHLORIDE.
CrO 2 Cl 3 .
CrO 3 + 2HC1 H 2 O =
152
LABORATORY MANUAL OF
ble. The tubes are wound with a little asbestos cord and
fit tight in the openings ; in order to make both crucibles
tight, a narrow, thin strip of soft asbestos board is wrapped
FIG. 10.
CHROMIUM OXIDE.
Cr 3 O 3 .
CHROMIUM ACETATE.
(CH 3 COO) 2 Cr.
500 grams fuming HC1 are poured over 100 grams po-
tassium dichromate in a flask, and the chlorine gas, which
develops, upon warming, after being washed with water, is
used in the preparation of chlorine water or of hypo-
chlorite of sodium. The remaining solution is evaporated
to a very small volume, poured off from the separated po-
tassium chloride into a flask with 300 grams of granulated
zinc and rinsed with 400 c. c. fuming HC1. The flask, in
which a violent evolution of hydrogen should take place,
is closed with a double-bored rubber stopper similar to
that of a wash bottle. As soon as the solution has as-
sumed a light blue color similar to copper sulphate solution,
the glass tube permitting the free passage of the gas is
closed, so that the hydrogen which continues to develop
vigorously presses the solution out of the flask through
the second tube which reaches to the bottom. It is filtered
through a small bulb-tube with asbestos and then enters
POTASSIUM CHLOROCHROMATE.
KO-C.O,
,
KG Cr0 2 - KO CrO,,Cl
Of TW
SELENIUM.
Se.
HYDROFLUOSILICIC ACID.
H 3 SiF 6 .
IOO grams calcium fluoride powder are mixed with
100 grams dry quartz-sand (sea-sand), and carefully heated
with 350 c. c. cone, sulphuric acid. The escaping gas is
led through an empty bottle containing a safety-tube
closed with a little cone, sulphuric acid, and then into a
porcelain dish, at the bottom of which a small vessel with
mercury has been placed. The gas tube is fastened so
that it dips into the mercury, and then 400 c. c. distilled
water are poured over it. After the gas evolution has
ceased, the silicic acid, which has separated in the water,
is filtered, washed with a little water, until the combined
filtrates amount to 400 c. c., and the still cloudy acid is
filtered through a folded filter.
PERCHLORIC ACID.
HC10 4 .
MANGANESE.
Mn.
MANGANESE CHLORIDE.
MnCl 2 + 4H 3 O.
Residues of chlorine produced from black oxide of man-
ganese and HC1 are evaporated to dryness in a porcelain
dish, and the residue heated for a time on the gas stove
with low flame. It is then boiled up with water and iVth
MANGANOUS SULPHIDE.
MnS.
MANGANESE SULPHATE.
MnSO 4 ,5H 2 O.
POTASSIUM MANGANATE.
K 2 MnO 4 .
BARIUM MANGANATE.
BaMnO 4 .
BaMn 3 O 8 .
FERRIC CHLORIDE.
Fe 3 Cl 6 .
FeCl 2 .
Fe 3 Cl 6 + 2H = 2FeCl 2 + 2HC1.
Fe 2 Cl 6 .
1 66 LABORATORY MANUAL OF
FERROUS SULPHATE.
FeSO 4 ,7H 2 O.
The last traces of nitric acid are removed from the fer-
ric sulphate solution by evaporation.
BERLIN BLUE.
1 68 LABORATORY MANUAL OF
PURE PLATINUM.
Pt.
The following method of Finkener's for obtaining plati-
num free from impurities, especially iridium, is here describ-
ed; it depends on recrystallization of sodium platinochloride.
Commercially purified platinum is dissolved in aqua regia, to
the solution of the chloride, freed from oxides of nitrogen,
the calculated amount of pure sodium chloride is added, the
solution is concentrated to a small bulk, and allowed to cool
whilst being continuously stirred. The crystals which sep-
arate are freed from mother liquor by suction, washed with
a concentrated solution of sodium chloride, and dissolved
in a one per cent, solution of sodium carbonate. The solution
is allowed to cool, when the salt again separates. It is
then dried at 120 C., reduced in a current of hydrogen at a
low temperature, and the platinum sponge thus obtained is
washed for a long time with water, and finally dried and
ignited. The metal thus obtained is extremely pure ; no
PLATINIC CHLORIDE.
PLATINIC CHLORIDE.
From Residues,
PLATINOSOCHLORIDES.
LABORATORY MANUAL OF
PENTATHIONIC ACID.
OF THC.
UNIVERSITY;
r. OF '
LAMINE.
HYDROXYLAMINE HYDROCHLORIDE.
HYDRAZINE.
CHYDRAZAINE OR PROTOXIDE OF
AMMONIA.
CARBON OXYSULPHIDE.
COS.
LABORATORY MANUAL OF
INORGANIC PREPARATIONS. I 77
H 2 SO 4 + 2KOH = K 2 SO 4 + H 2 O
98 112 2 174-2 36
or 49 56.1
so also with Na 2 CO 3 .
i8o
LABORATORY MANUAL OF