cupwiest News, Determination of the Amount of Morphia in Opium. 47
hat the excess of indigo commences with the brown: ON THE
stage. If the brown Shien is gonad jute Sevgral times DETERMINATION OF THE AMOUNT OF
ts volume of water, the colour immediately changes to UM.
green. This treatment with water is a very convenient MORPHIA PRESENT IN OFI
method of ascertaining the final reaction. . By E. F. TESCHEMACHER, F.C.S., &c,
When 2 volumes of oil of vitriol are employed, the tint
jue to excess of nitrate is less deep and red than with
{ volume of acid, and approaches a dark sherry colour;
with more indigo this passes through the brown and green
stage. The brown, green, and superior tints, when poured
into water, yield green for an instant only, the colour
quickly passing into cinnamon. The cinnamon solution thus
Jbtained is capable of decolourising a rather considerable
quantity of indigo. It will be recollected that with
2 volumes of oil of vitriol far less indigo is oxidised than
when a smaller proportion of sulphuric acid is used: it
would appear that with 2 volumes of acid some lower
oxide of nitrogen remains in solution, and on the addition
of water becomes capable of destroying indigo.
With an intermediate proportion of oil of vitriol
{1} volumes) the tints are similar to those with 2 volumes,
ut more feeble in intensity ; the brown tint and the tints
superior to it change to green on dilution.
With_very weak solutions of nitre the tints obtained
with 1 volume of oil of vitriol are similar to those yielded
by stronger solutions ; the brown is changed into a dis-
Hin green on filling up the flask with water. With 14 vol-
ame of acid the final tints are feeble and unsatisfattory.
With 2 volumes of acid the tints produced are much
jeeper than with 14 volume; the indigo and blue are
specially intensified.
The best plan seems to be to adopt the brown tint
whenever possible as the point of final rea&tion, or, more
sxadly, that particular brown tint which yields a distinét
yellowish green on dilution. In all exact work a check
experiment should be made with rather less indigo than
‘hat yielding this green tint, to make sure that no smaller
amount of indigo will produce a similar reaction. Work-
ing with z volumes of oil of vitriol, the green tint produced
by dilution must generally be dispensed with ; but if the
sye has been educated to the particular shade of brown
which yielded green in the former cases, it will be able to
liscriminate this tint with fair accuracy without dilution.
In the case of weak solutions the eye can be helped by
ransferring the contents of the flask to a cylinder,
In the case of experiments with 1 volume of oil of
vitriol, the tint, whether in strong or weak solutions, soon
-eaches a definite point, beyond which no further change
occurs. But with 13 or 2 volumes of acid the tint conti-
ues to change slowly (especially in dilute solutions) after
-he first main rea&ion is over; if, therefore, definite re-
sults are wanted, it is quite necessary to time the experi-
ment, and to take that as the final tint which is observed
at a fixed interval after pouring in the oil of vitriol. I
aave taken two minutes as the period to elapse before the
;int is recorded, but, except in the case of weak solutions,
one minute would suffice.
The determination of the final rea®ion is undoubtedly
sne of the weak points of the method, but with care and
sractice the difference between similar experiments need
scarcely exceed 1 per cent in the case of moderately
strong solutions (1'0 to o'5 grm. of nitre per litre), and
with weak solutions (0°25 to o'10 grm. per litre) should not
be greater than 2 or 3 per cent, supposing that in each
case an indigo of appropriate strength is employed.
A few experiments have been made with an indigo so-
lution prepared by dissolving sublimed indigotine in
sulphuric acid. With this solution the colour produced
oy an excess of nitrate is much less deep than with a
solution of ¢ indigo-carmine ;” the tint is golden and not
red, and passes into bright green without an intermediate
orown stage. The colour reaction with this indigo solution
is very sharp.
[N placing in the hands of Chemists one more process for
letermining the amount of Morphia present in Opium, it
must not be assumed that the labours of my predecessors
n this field have been ignored or disregarded by me.
Most gladly would I have adopted any one of these numer-
Jus processes had it, on trial, afforded similar, definite
and reliable results in the amount and purity of the mor-
shia obtained. That these processes fail to yield satis-
factory results when they are based on sound methods of
srocedure, is, to my mind, due, partly to the authors
raving failed to describe and insist on the necessity of
‘ollowing each and every step, however minute, of their
srocess; and, partly, to their having, too readily, jumped
to the conclusion of the excellence and certainty of their
methods, without painstaking and long-continued investi-
jation of the subje, and repeated reviewal and testing of
avery discernible or probable source of error.
On the first of these grounds, I claim the indulgence of
Il who may take an interest in the subject, for the many
ninute directions and explanations I shall feel it to be re-
juisite to place before them ; and as to the second I would
\ssure them that the process described is but the outcome
and result of very numerous experiments, the details and
sonditions of which have been changed and modified, as
requent practice for some years past proved to be advisable
or necessary ; so that the method as now worked out and
described, but slightly resembles the process in its in-
teption.
Amongst the conditions requisite to success in deter-
nining the amount of Morphia present in Opium, are :—
1. The avoidance of the use of Alcohol to extract the
Morphia from the Opium. This rule leads at once to the
rejection of very many facile and seemingly excellent
methods ; and the reason for its adoption is, that Alcohol
jissolves the whole of the Narcotin as well as the Morphia
sresent in Opium, and that, in practice, it is very difficult
f not impossible to separate the whole of the Narcotin
ander such conditions from the morphia; soit is essential
that the greater part of the Narcotin should remain undis-
solved in the refuse of the opium and never pass into solu-
sion.
II. The separation of the Meconic acid. This should
se effe@ed at an early stage of the process, so as to pre-
vent the formation of a basic meconate on precipitation
»f the Morphia, which is very apt to occur unless all the
Meconic acid is separated in the first instance.
The other conditions are rather details of the process
‘han definite maxims, and are better included in the de-
scription of the method than apart from it.
Two special reagents are required in this process. The
one prepared by mixing 1 part of solution of ammonia
sp. gr. 0'880 with zo parts of methylated alcohol, or of
unmixed alcohol, and digesting in this mixture a large ex-
cess of Morphia for several days, with frequent agitation,
so as to saturate it with Morphia. This may then be
filtered for use when it will contain 0°33 per cent of Mor-
shia, and for convenience sake may be termed * Morphiated
Spirit.” The other is, Water saturated by frequent and
ong continued agitation with excess of Morphia and then
fitered, which may in its turn be called “ Morphiated
Water,” containing 0-04 per cent of this alkaloid. It must
se assumed that the sample of Opium to be examined has
seen properly drawn, and prepared by kneading and rolling
:ogether in a cool place ; but this is best left to a skilled
sampler, who is known to be competent to and careful in
1is work. ‘
PROCESS.
1000 grains of Opium are macerated for twelve to twenty
hours in about 4000 grains of cold distilled water, together
To be continued.)