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The amount of camphor in an analgesic ointment can be determined by GC using the

ID: 1058425 • Letter: T

Question

The amount of camphor in an analgesic ointment can be determined by GC using the method of internal standards. A standard sample was prepared by placing 45.2 mg of camphor and 2.00 mL of a 6.00 mg/mL internal standard solution of terpene hydrate in a 25.00 mL volumetric flask and diluting to volume with CCl_4. When an approximately 2 mu L sample of the standard was injected, the FID signals for the two components were measured (in arbitrary units) as 67.3 for camphor and 19.8 for terpene hydrate. A 53.6 mg sample of the analgesic ointment was prepared for analysis by placing it into a 50.0 mL volumetric flask along with 10 mL of CCl_4. After heating to 50 degree C in a water bath, the sample was cooled to below room temperature and filtered. The residue was washed with two 5 mL portions of CCl_4, and the combined filtrates were collected in a 25.00 mL volumetric flask. After adding 2.00 mL of the internal standard solution, the contents of the flask were diluted to volume with CCl_4. Analysis of an approximately 2 mu L sample gave FID signals of 13.5 for the terpene hydrate and 24.9 for the camphor. Report the %w/w camphor in the analgesic ointment.

Explanation / Answer

7. analysis of camphor

Standard sample with,

45.2 mg/25 = 1.808 mg/ml Camphor

6 x 2/25 = 0.48 mg/ml of terpene hydrate as internal standand

2 uL aliquot gave GC signal = 67.3 of camphor and 19.8 for terpene hydrate

Response factor = (67.3/1.808)/(19.8/0.48) = 3.4

Sample of analgesic ointment analysis

concentration of camphor in diluted sample = 24.9 x 0.48/3.4 x 13.5 = 0.2604 mg/ml

In 25 ml = 0.2604 x 25 = 6.51 mg camphor is present

%w/w camphor in analgesic ointment = 6.51 x 100/53.6 = 12.14%

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