Running Head: ANALYTICAL CHEMISTRY 1

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ANALYTICAL CHEMISTRY 2

Introduction:

Over 25 years, pharmaceutical companies have been manufacturing mixtures of

phenacetin, aspirin and caffeine. This mixture is also known as APC is used to relieve pain as

well as reducing fever. Nevertheless, improper application of this substances may bring about

side effects to such individuals. For example, overdosing phenacetin increases the risk of

contracting kidney problems. Overdosing aspirin may risk individuals to heartburns, ulcers,

stomach pains (Balcerwska-Czerniak, 2017). High dosages of caffeine may expose such

individuals to risks of developing central nervous system disorders. Therefore, determination

of the mixture of three compounds safeguards lives of individuals.

Parke et al (1951), attempted to outline the best method that could be by chemists to

simultaneously determine the mixture comprised of the three compounds through the

application of infrared spectrometry. Identification of Fourier Transform Infrared (FTIR-

coupled with multivariate linear regression) has been crucial in analysing the mixture of the

three compounds (Balcerwska-Czerniak, 2017). FTIR spectroscopy applies the principle of

Michelson interferometer whereby the beam splitter divides the two optical beams in various

directions thereafter recombining to interact with the sample. Thereafter, interferogram turns

into infrared spectrum that is then presented on a computer screen. Beer’s law for a particular

wavelength is applied to the spectrophotometric analysis of absorbance of the sample with the

following equation A=absorbance, B=absorption coefficients, C=sample concentration, I=

path length. Sample concentration is linearly proportional to absorption (Liu, X.Z. et al. 1999).

Using multivariate regressions, precise analyses are obtained because wavelengths are

more than the components number in the system. It's also crucial, especially where components

may affect each other or else their spectra overlap. This technique also minimizes an influence

of chemical matrix impacts.

ANALYTICAL CHEMISTRY 3

Experimental

The mixture was precisely weighed out into three volumetric flasks (25 Ml).

Approximate amounts of every compound were listed in a table. Chloroform was then added

to every flask in order to dissolve the solids. Immediately after dissolving the solids, every

flask was diluted to the mark with chloroform. Thereafter, FTIR system was used to measure

the sample spectra. A background scan was taken since FTIR is a single beam in order to

account for any instrument losses as well as components absorptions in the atmosphere. A

syringe was then used to load the sample into liquid sampling cell. The syringe was rinsed 3 to

5 times between the samples. After all the data for 14 solutions were gathered, it was delivered

into a spreadsheet. After the process of importing the whole data competed, necessary

calculations and matrix maths were completed automatically (Gindy, A.E. 2012).
ANALYTICAL CHEMISTRY 4

References

Balcerowska‐Czerniak, G., & Kupcewicz, B. (2017). Score‐based quantitative

principal component analysis with application to the study of active

pharmaceutical ingredients based on attenuated total reflection fourier‐

transform‐infrared spectra. Journal of Chemometrics, 31(2).

Gindy, A. E., & Hadad, G. M. (2012). Chemometrics in pharmaceutical analysis: an

introduction, review, and future perspectives. Journal of AOAC International,

95(3), 609-623.

Liu, X. Z., Liu, S. S., Wu, J. F., & Fang, Z. L. (1999). Simultaneous monitoring of

aspirin, phenacetin and caffeine in compound aspirin tablets using a sequential

injection drug-dissolution testing system with partial least squares calibration.

Analytica Chimica Acta, 392(2-3), 273-281.