Name: Mas, Mylyn L.

Date Submitted: 10/28/16

Pharm Chem 135 Section: PH6

Date Performed: 11/05/16

Experiment No. 5
Complexometry
Assay of Alumina and Magnesia Oral Suspension for Aluminum Content
I. DATA AND RESULTS
A. Volume/Weighing Measurements
Sample 1: Alumina and Magnesia Oral Suspension
Volume of Sample (Stock Solution):
(Trial 1) : 250.0 mL (Trial 2) : 250.0 mL
Aliquot: (Trial 1) : 10.0 mL (Trial 2) : 10.0 mL (Blank): 10.0 mL (water)
B. Titration Data
Volume of Titrant Used:
Volume Reading

Trial 1

Trial 2

Blank (n/a based on

Initial Reading

0.00 mL

0.00 mL

USP)
25.05 mL

Final Reading

25.05 mL

25.05 mL

50.10 mL

Total Volume Used

25.05 mL

25.05 mL

24.05 mL

Volumetric Solution Used: Disodium Edetate

Nf= 0.9617
Prepared by: Viloria, Lovely Mae R.
Volume of Back Titrant Used:
Volume Reading

Trial 1

Trial 2

Blank (n/a based on

Initial Reading

0.00 mL

0.00 mL

USP)
13.45 mL

Final Reading

13.60 mL

13.45 mL

43.75 mL

Total Volume Used

13.60 mL

13.45 mL

30 .30 mL

Volumetric Solution Used: 0.05 M Zinc Sulfate

Nf= 0.58
Prepared by: Cleo Valiente
Calculated % of Active Ingredient:
Labelled Claim: 225 mg/5 mL
Trial 1: 104.93 % of Al(OH)3 in Sample

Trial 2: 105.87 % of of Al(OH)3 in Sample

% Deviation Between Trials: 0.8981 %

(Acceptance criteria: 90.0 %-110.0%)
Sample: PASSED THE OFFICIAL REQUIREMENT
II. DISCUSSION
A suspension of Alumina and Magnesia Oral Suspension (Labelled Claim: 225 mg/5mL)
was assayed. Sample is composed of white suspended particles that needs to be shaken well
before use. It was stored in a white plastic container that was tightly closed. The sample was not
freshly prepared and was opened during the week of the assay (October 24-28, 2016).
Two titration trials were performed for the assay of Aluminum Hydroxide content of
Alumina and Magnesia Oral Suspension with Disodium Edetate VS as the excess titrant and
0.05 M Zinc Sulfate VS as the back titrant. A 0.8981 % deviation between both trials was
acquired. The % deviation value falls within the + 3% deviation range, indicating that the results
obtained are of high precision. In addition, a 104.93 % and 105.87% active ingredient for Trial
1 and Trial 2, respectively were calculated . The % active ingredient of the sample met the
acceptance criteria set for Aluminum Hydroxide content of Alumina and Magnesia Oral
Suspension (90.0-110.0 %) which means that the sample is of good quality.
A modification of the original procedure done is the amount of dithizone to be added on
the sample. The procedure indicates addition of 2 mL of dithizone, however, since at this volume
no color is evident (sample is still colorless) a 6 mL volume of dithizone was used. At 6 mL, the
green-violet color became evident. This addition of volume has no significant effect on the assay
since the formation of the zinc dithizonate complex is only dependent if there are already free,
excess zinc on the reaction mixture and not on the amount of dithizone present. In addition, the

zinc dithizonate complex is less stable than the Zinc-EDTA complex which means that the Zinc
will prefer EDTA complexation more, if there is still EDTA in the solution and not on the small
excess volume of dithizone.
One significant difficulty encountered during the assay was the determination of the
endpoint. Color change to determine endpoint was from green-violet to first signs of rose-pink. It
was difficult to determine the transition since a.) the color change consists of 2 highly
contrasting colors and b.) the endpoint is accurately determined thru first signs of rose pink, with
no excess. The reaction mixture contains dithizone which means that light should be avoided,
however, to determine the first tinge of rose-pink, there is a need to align the mixture against
light. To remedy this, the sample was placed against a white background, and the first sign of
pink was determined only when the solution turned slightly pink. This means that there are
already excess zinc in the solution indicating that the endpoint is not accurately determined.
IV. CONCLUSION AND RECOMMENDATION

The aluminum hydroxide content of Alumina and Magnesia Oral Suspension sample
passed the acceptance criteria set by USP, which means that the sample is in a good quality.
The % deviation between trials indicates that the results obtained are of high precision.
However, the difficulty encountered in the accurate determination of the endpoint indicates a low
reliability of the results.
It is highly recommended that the titration must be performed away from light. In
addition, the dithizone to be used must be freshly prepared also away from light and should be
fully covered with aluminum foil to prevent decomposition.