Quimica Analytica Volume 4, Issue 1

August 7, 2013

Potentiometric Measurements Dr. Kathlia Cruza, Chrissie A. Arceob ABSTRACT Potentiometry is an important analytical method for the quantitative determination of the concentration of an analyte in a solution. This involved the use of different kinds of electrodes such as pH meter, and ion selective electrode. Calibration and standard addition methods were used in this experiment. The purpose of the study was to determine pH of various shampoo samples, and determine the concentration of the fluoride ion in different samples of toothpaste, and mouth wash. In the experiment, preparation of samples using a total ionic strength adjustment buffer was done. It was explained in the results the relationship of pH to hair damage, and the concentration level of Fluoride ion required for it not to become detrimental to human health. Errors in the data were assumed to be due to human and equipment error.

Introduction Potentiometry is defined as the measurement of the concentration of a solute in a solution that involves the use of an electrode. It is also a selective method that detects specific ions present in an analyte solution. In this experiment, two electrodes were used in the determination of pH (pH meter) and determination of Fluoride ion (ion selective electrode). The advantages of ion selective electrodes include its selectivity, efficiency, easy sample preparation, and the lack of interference and reactivity with the sample that is being analyzed. Two analytical techniques were done in the determination of the concentration of Fluoride ion: the standard addition and calibration methods. Standard addition method is the direct addition of standard to the analyte and is used when a small number of samples are to be analysed. The concentration of analyte in the unknown solution can be deduced using this method from the increase in signal (Harris, 2010). While in calibration method, it is commonly used when a large number of similar samples are to be analysed. Determination of the concentration of fluoride ion in toothpaste samples is important because it prevents tooth decay when it is around 1ppm, but it has harmful effects at 2-13.7 ppm range that includes staining, and cracking of the teeth. It is related that at a high concentration, it can cause osteosarcoma, a rare malignant bone tumor (Kharb, 2012).

Experimental Setup The following materials were used in the experiment: buffer solutions (pH= 4, 7, and 9), shampoo samples, TISAB (total ionic strength adjustment buffer) solution, and 0.1M F stock standard solution. The following apparatus were used in the experiment: beakers, pipets, volumetric flask, pH meter, and Fluoride-ion selective electrode. In the pH determination of hair shampoos, a pH electrode was first calibrated using the pH 4, 7, and 9 buffer solutions. After it was calibrated, it was then used to measure the pH of commercially available shampoos, in both concentrated and diluted forms (1:10 dilution). This was performed using samples that have high to low pH levels. In the determination of fluoride in toothpaste and mouth wash, the samples were prepared by weighing 0.20g of toothpaste in a 300-mL beaker and 50-mL TISAB solution was added to it. The solution was allowed to boil for 2 minutes, cooled, and was transferred to a 100-mL volumetric flask. It was diluted to mark with distilled water, mixed well, and set aside for the potential measurement. For mouth wash, 25-mL of it was poured into a 100mL volumetric flask with 50-mL of the TISAB solution. It was also diluted to mark, and mixed well. In determining the fluoride from sample using calibration curve method, a 5ppm fluoride solution

Footnotes: a Professor, School of CHE-CHM, Mapua Institute of Technology b CHM115L/B10. School of CHE-CHM, Mapua Institute of Technology

was prepared and 5, 10, 25, and 50-mL aliquots of it were transferred into a 100-mL volumetric flask with 50-mL TISAB solution. The potentials of each were determined and a calibration curve was prepared. From the graph, the concentration of fluoride in the sample was determined. In the standard addition method, different solutions containing different compositions of TISAB, tap water, and standard solution. The potential of each solution was measured and a plot of E vs (CV)std was made. The concentration of fluoride in the sample was determined. Results and Discussions

The table shown below shows the values of the E in millivolts and the logarithm of the molarity of the solution: Table 2. Calibration Curve Method Solution [M] log 1 2 3 4 5

E (mV) 164.1 155.4 154.6 153.5 152.6 129

2.63158E-05 5.26316E-05 7.89474E-05 0.000105263 0.000131579 0.000263158

4.5798 4.2788 4.1027 3.9777 3.8808 3.5798

The pH of the concentrated and diluted solutions of different shampoos is shown in the table below Table 1. pH of various shampoos Concentrated (pH) Conditioner Dove 5.670.671 Creamsilk 4.850.176 Palmolive 3.980.059 Head and Shampoo 7.000.089 Shoulders Dove 6.250.363 Sunsilk 5.960.103 Shampoo Palmolive with 6.640.038 (pink) Conditioner Palmolive 6.570.727 (violet) Palmolive 7.150.278 (green)

Diluted (pH) 4.280.050 4.310.035 4.290.605 7.380.098 6.460.087 6.10.076 6.820.016 6.950.070 6.90.140

It was observed that the diluted shampoo solution have a slightly higher pH because the concentration of the H+ was reduced. Human hair is naturally acidic, and has a pH ranging from 3.0 to 5.0. The results are in accordance to what Dembrink (1983) said that if these products have a pH higher than 8.0 to 12, then it can result to hair damage.

The graph obtained using calibration curve method is 174 169 164 E 159 154 m 149 V 144 139 134 129 3.5000

Conclusion This experiment aimed to have an understanding of potentiometric measurements using various kinds of electrodes. The first objective was achieved because the students had a hands-on in using the pH meter and the Fluoride-ion selective electrode. This experiment also determined the pH of different shampoo products using the standard pH meter, and in the discussion, the relationship of the pH to hair damage was mentioned. Lastly, the amount of fluoride ion in different samples of toothpaste and mouth wash was determined using a Fluoride-ion selective electrode. The importance of having an [F] less than 1ppm and its effect to human health was also discussed. References

It can be seen that the graph is not following a perfect linear trend, this is may be due to some experimental error and an error in handling/measuring the standards. This may also be due to the equipment used as it shuts down suddenly when used in the wrong position.

Table 3. Values of E in millivolts and concentration of different samples E (mV) stock solution with buffer toothpaste mouth wash tap water abs(log[M] ) log [M] 4.648829596 4.526267323 4.212979803 4.275571766 [M] 2.24476E05 2.97668E05 6.12379E05 5.30186E05

This table shows the concentration of the fluoride ion in different samples such as toothpaste, mouth wash, and tap water. The values are less than 1ppm and it means that the levels of fluoride ion in those are safe for human consumption and will not cause oral health problems.

( )

y = 30.517x + 27.435 R = 0.7893

4.0000 4.5000 log[F]

5.0000

Figure No.1 Calibration Plot Using Calibration Method

Dombrink, K., and Tanis, D. pH & Hair Shampoo. ChemMatters April 1983, page 8. Harris, D. Quantitative Chemical Analysis. W.H Freeman, 2010. Kharb. S, Sandhu, R., Kundu, S. Fluoride levels and osteosarcoma. South Asian Journal of Cancer, October-December 2012, Vol.1 (2), pages 76-77.

169.3

4.648829596

165.56

4.526267323

156

4.212979803

157.91

4.275571766