Experiment 2

Determination of Zinc Oxide in Dermal Ointment and Talc Powder by EDTA
Titration with Method Validation

Johnsan Loie A. Villaristo
Abstract
1. Introduction
2. Materials and Methods

2.1. Standardization of EDTA
0.3 g to 0.1 mg of calcium carbonate was weighed and 4 mL 9% hydrochloric acid was
added. It was dissolved and transferred to a 250 mL volumetric flask. 15 mL of aliquot was
pipetted in a 250 mL Erlenmeyer flask at three replicates. 80 mL water, 4 pearls of potassium
hydroxide, and 1% murexide were added. It was titrated with ∼ 0.01 M EDTA prepared by
dissolving and diluting 4 g ethylenediaminetetraacetic acid dissodium salt dihydrate in 1-liter
volumetric flask.
2.2. Powder Method

About 1.0 g to 0.1 mg of talc powder was weighed in a 250 mL beaker. 50 mL 9%
hydrochloric acid was added and was stirred for ten minutes. It was transferred in a 250 mL
volumetric and diluted to mark using water. The suspension solution was filtered using
qualitative filter paper to a 400 mL beaker.
2.3. Ointment Method

About 0.6 g to 0.1 mg of dermal ointment was weighed in a 250 mL beaker. 50 mL 9%
hydrochloric acid and 50 mL diethyl ether were added. It was stirred in a magnetic stirrer and stir
bar in the fume hood for one hour. It was transferred in a separatory funnel and denser aqueous
phase was collected in a 250 mL volumetric flask. It was washed with 20 mL saturated sodium
chloride solution three times. It was diluted to mark using water.
2.4. Zinc Standard Solution

About 0.2408 g analytical grade zinc oxide was weighed and treated accordingly to ointment
or powder method. 500 mL volumetric flask was used instead producing Zn(II) standard solution
of about 0.006 mol/L.
2.5. EDTA Titration

Aliquots of 20 mL of three replicates of sample containing Zinc (II) were pipetted in a 250
mL Erlenmeyer flask. 10 mL of ammonia buffer at pH 10 (prepared by diluting to 1-liter
volumetric flask the dissolution of 70 g NH 4Cl in 570 mL NH4OH), and two drops of 1%
Eriochrome Black-T indicator were added. It was titrated with standardized EDTA solution. For
the blank, 1.8% HCl was used instead.
3. Results
3.1. Standardized EDTA Solution
Three replicates of 15 mL calcium carbonate aliquots were titrated titrated with the EDTA
solution. The exact mass and molar mass of the primary standard calcium carbonate used in the
experiment were 0.3066 g and 100.0869 g/mol respectively.
AVERAGE RELATIVE
VOLUME MOLARITY MOLARITY STANDARD
MOLARITY STANDARD
TRIAL EDTA CACO3 EDTA DEVIATION
EDTA DEVIATION
(ML) (MOL/L) (MOL/L) (MOL/L)
(MOL/L) (%)
1 16.29 0.01128
2 16.01 0.01225 0.01148 0.01125 0.00024 2.15
3 16.71 0.01100
Figure 1. Exact concentration of EDTA solution.
3.2. Determination of Zinc Oxide in Talc Powder and Dermal Ointment Sample
Three replicates of 20 mL of sample aliquots were titrated with the standardized EDTA
solution. The volume EDTA were averaged (see Appendix A), and zinc oxide was calculated
using the molar mass 81.379 g/mol. A blank was also done with an average volume EDTA of
0.30 mL.
V
Equation: m ZnO = ( Vt – Vb )M ZnO
Vo
WEIGHT AVERAGE WEIGHT WEIGHT PERCENT
SAMPLE SAMPLE VOLUME EDTA ZINC OXIDE ZINC OXIDE
(G) (ML) (G) (%)
Talc Powder 1.0179 0.90 0.0068 0.67

Dermal Ointment 0.6349 12.27 0.1370 21.57
Figure 2. Weight percent zinc oxide in the sample.
3.3. Method Validation

a. Linearity
Linearity was established using 10.00, 15.00, 20.00, 25.00, and 30.00 mL aliquots of
Zinc (II) standard that were prepared by powder method and ointment method respectively.
The exact weight of analytical grade zinc oxide was 0.24.
0.0160
0.0140
f(x) = 1.06270637942974 x − 0.000167943610820865
0.0120
R² = 0.998433853537303
weight ZnO (g)

0.0100
0.0080
0.0060
0.0040
0.0020
0.0000
0.0000 0.0050 0.0100 0.0150
actual mass ZnO (g)
(a) (b)
Figure 3. Weight zinc oxide versus actual mass zinc oxide in five different aliquots (a)
Linearity of powder method (b) Linearity of ointment method.
b. Precision
Precision was determined using the average standard deviation of three different volume
aliquots at three replicates. The weight of the talc powder was 1 g and the weight of dermal
ointment was 0.6039 g.
σ
Equation: RSD (%) = x 100
x
WEIGHT AVERAGE RELATIVE
VOLUME VOLUME WEIGHT STANDARD
PERCENT WEIGHT STANDARD
ALIQUOT EDTA ZINC OXIDE DEVIATION
ZINC OXIDE PERCENT DEVIATION
(ML) (ML) (G) (%)
(%) (%) (%)
(a)
WEIGHT AVERAGE RELATIVE

VOLUME VOLUME WEIGHT STANDARD
PERCENT WEIGHT STANDARD
ALIQUOT EDTA ZINC OXIDE DEVIATION
ZINC OXIDE PERCENT DEVIATION
(ML) (ML) (G) (%)
(%) (%) (%)
5.61 0.1284 21.27 20.40 0.67 3.29

10 5.69 0.1303 21.57
5.20 0.1191 19.72
20 10.51 0.1203 19.92
10.75 0.1231 20.38
10.99 0.1258 20.83
13.25 0.1214 20.09
25 13.10 0.1200 19.87
13.15 0.1204 19.94
(b)
Figure 4. Relative standard deviation of (a) powder method (b) ointment method.
c. Accuracy
Percent deviation was determined in accordance to the labeled amount of zinc oxide
present in the sample. The talc powder used in the experiment contains talc but does not
indicate exact amount of zinc oxide. Hence, percent deviation in the talc powder was not
determined. The dermal ointment contains 555.7 mg in 3.5 g of sample (see Appendix).
¿
Equation: % deviation = ¿ x̄−x label ∨ x ¿ x 100
label
WEIGHT PERCENT ACTUAL WEIGHT PERCENT
SAMPLE ZINC OXIDE PERCENT DEVIATION
(%) (%) (%)
Talc Powder - -
Dermal Ointment 20.40 15.88 28.49
Figure 5. Percent deviation of weight percent zinc oxide in talc powder or dermal ointment
and labeled weight percent.
d. Confidence Interval
Confidence interval was based critical t value in student-t distribution in a two-sided
interval of 95%. The total number of replicates was 9.
tσ
Equation: µ = x̄ ±
√N
SAMPLE CONFIDENCE INTERVAL (%)
Talc Powder ±
Dermal Ointment 20.40 ± 0.52
Figure 6. Confidence interval of the weight percent talc powder and dermal ointment.
3.4. TBC
3.5.
4. Discussion
References
1. TBC
Appendix A
Appendix B
Appendix C

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Experiment 2

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Determination of Zinc Oxide in Dermal Ointment and Talc Powder by EDTA

Titration with Method Validation

2. Materials and Methods

2.2. Powder Method

2.3. Ointment Method

2.4. Zinc Standard Solution

2.5. EDTA Titration

Talc Powder 1.0179 0.90 0.0068 0.67

3.3. Method Validation

weight ZnO (g)

WEIGHT AVERAGE RELATIVE

5.61 0.1284 21.27 20.40 0.67 3.29

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