FEBRUARY, 1919. Yol . XLIV., No. 616

THE ANALYST.

PROCEEDINGS OF THE SOCIETY OF PUBLIC ANAILYSTS AND OTHER ANALYTICAL CHEMISTS.

EFFECT OF MORPHINE CONCENTRATION ON THE B.P. METHOD OF MORPHINE ESTIMATION.

BY H. E. ANNETT, B.Sc, (LoND.), F.I.C., AND HARDAYAL SXNGH, B.Sc.

IN the course of work we have been carrying out on Indidn opium we have met with samples which have shown a wide mnge in morphine oontent. Some have yieldeq. over 18 per cent. morphine, whereas some samples have contained no morphine. WQ understand that the B.P. method has been worked out for the analysis of opium con- taining about 10 per cent. morphine. I n our work we have been studying the effects of various factors on morphine content in opium ; and since we have mainly used the B.P. method we have been interested in studying the conditions required to make that method reliable. We have found nothing of this nature in the literature, and it' seems worth while to record our experimental results.

Analyszs of Pure Morphine by the Nethod of the B.P. 1914.-A weighed quantity of orystalline morphine was in each case triturated with 2 grme. of freshly slaked lime and 20 C.C. of distilled water. A further 60 C.C. of distilled water was subsequently added, the whole was stirred at intervals during half an hour, and the morphine precipitated in 50 * C.C. of the filtered liquid. The morphine was filtered off and weighed, after drying at 60' C., and subsequently for two hours at 115" C.

V

Crystalline J *-1--.

'kigh t of

muan. Morphine

Weight of Amorphous Morphine in 50 C.C. taken

for Precipitation (calculated) .

Grm. 0.25 0-50 0.75 1.00 1-25 1-50

Grm. 0.147 0.294 0 441 0.588 0.735 0*882

Weight of Amorphous Morphine found (corrected by addition of 0-050 grm.).

arm. 0*1268 0.2818 0.4244 0.5860 0.7344 0-8934

Per Cent. Morphine recovered.

83.54 95.85 96-23 99-66 99-92

101.30

* The B.P. 1914 method states that 5 1 C.C. should be taken. In these expariments with pure morphine we only took 50 0.0. of lime solution, and we added 0.060 instead of 0'051 grrn. as a correction for the morphine remaining in solution.

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42 MORPHINE CONCENTRaTION

Quantities Taken.

(a} 8 grrns. ... ( b ) 4 7 ? ... ( c ) 2 ? 9 . .. (d) 12-75 C.C. ...

The results indicate that with quantities of 1 grm. of crystalline morphine an2 upwards the B.P. tmthod gives accurate results. When only 0.25 grm. of crystalline morphine was taken, the method gave low results. Since 8 grms. of opium are taken in the B.P. 1914 method, 0 25 grm. rnorphins would correspond to an opium of less Ishan 3 per cent. amorphous morphine content.

Analyszs of Samples of an Opmm conik.xiizi.rzg Various Proportions of Sturch.-A sample of moist opium was well tiiixed and varying amounts, recorded b~low, were then weighed, arid the morphiue estimated by the B.P. process.

Sample Number

r.

S~mplc.

8 grms. opium . . . ... . . I

6 grrns. opiniri + 2 grrns. starch 4 grrnzl. opiiirn + 4 grms. starch 2 grrns. opium + 6 grms. starch 8 grms. Htarch ... ... ...

Weight of

3101 phine obtained.

A I U O ~ 1 1 h OUY

Grm. 0 2675 0.1592 0 0347 0.00 12 0.0046

Weight of Am01 phous Morphine (corrected + 0.051 grm.).

Grm. 0.3185 0 2102 0.0857 0.0522 -

Yer Cent. Morphine in Sample.

6.37 4-20 1-71 1.044 -

Per Cent. calculated.

6.37 4-78 3-18 1.59 0.00

It wonld seem from these figures that with opium low in morphine the B.P. mtstliod gives results for the morphine content which are considerably below the truth.

(a) 8 grms. ... ( b ) 4 1 9 ... (c ) 2 > f ... (d) 12-75 C.C. ...

rr.

Weight of Anhydrous Mor-

phine.

0.3149 0.1368 0 0727 0*0840

0.4780 0 2308 01268 0.1168

Weight of Anhy- drous Morphine

[corrected +- 0 051 grm j.

0.3659 0.1623 0.0854 0-0967

0.529 0.2563 0.1395 0.1296

Per Cent. Morphine in

Opium.

7.32 6.49 6.84 7-74

10.58 10-25 11 -16 10.37

Estimations by ll P. 1914 Xethod, using Reduced Quantities of Opium and Propor- iionately Redaced Quantities of Rrageizts.--In the course of our work we found it necedmry to get ari idea of the morphine content in samples of opium too small to be enalywd in the usual way. We therefore wished to see if we could use 4 grms. and even 2 grms. of opium instead of the 8 grms. laid down in the B.P. method. We festrd this point on two samples (I. and 11.). In each case wa weighed out (01) Sgrms., (b) 4 grm., (c) 2 grms., of the well-mixed powdered opium sample.

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METHOD8 OF CALCULATING ADDED WATER IN MILK 43

(a) was analysed in the ordinary way (B.P. 1914) ; (b) was analysed using half the quantities of the reagent8 recommended. The correction used was 0.0255 grm., and 25.5 C.C. of tht, lime solution were taken for precipitation. ( c ) was analysed using quarter quantities of the reagents. The correction used was 0.0127, and 12.75 C.C. of the lime solution were taken for precipitation.

After taking 51 C.C. of the lime filtrate from (a) for analysis, enough liquid was left to take a further 12-75 C.C. This was then precipitated ss described under (c) and is designated (d) in the table.

The error of the B P. 1914 method is stated to be 0.5 per cent. morphine either way. I n view of this it, must be concluded that the results here set out show that useful results can be obtained by snalysing opium samples when only 4 grms., or even 2 grins., of the sample are availrtble.

AG KI(:UJ;I*UBA L COLLEGE, CAWNPOIUC, INDIA.

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