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Correlation cel-pH

cel = k-2.303 Relation (5) is the calibration function of pH potentiometric measurements with glass electrode. Theoretical sensitivity of the electrode is defined as follows:

Electrode sensitivity Electrode sensitivity depends on temperature, with a value of - 0.059 V / pH unit at 25 C. Most electrodes present deviations from ideal behavior, so that the actual sensitivity defines an electrode. This correlates with theoretical sensitivity coefficient through s (s> 0.95), which expresses the electrode deviation from ideal operation:

S=Sts
In conclusion, the calibration function of the electrode glass membrane is expressed as follows:

cel = k + S pH 4. Measuring pH with a pH meter Measuring the pH of a solution using as indicator electrode glass membrane electrode, is performed using instruments called pH-meters. These tools are millivoltmeters precision (accuracy of at least 0.001 V), whose scale is calibrated in pH units, the following linear correlation between pH and emf of the cell:

a and b are adjustable parameters of pH meter.

Calibration function of membrane glass electrode is of type (8), cel=k=SpH , and is rewritten in the form:

where a '=-k / S and b' = 1 / S are electrode glass cell parameters. Calibration involves adjusting the pH meter size and b so that the conditions a = a 'and b = b'. To this end we use two standard solutions of pH. Correction parameter b is compared with a second standard solution pH (slope adjustment). After calibration can be performed quickly and accurately determine the pH of a large number of samples without requiring frequent recalibration of the pH meter. However, due to slow changes over time parameters such as potential asymmetry is advisable to check daily tool using standard solutions and repeat, if necessary, calibration. Special attention must be paid to temperature. Indicated that the sample temperature be equal to the standard solutions. In addition, it must be taken into account that the pH standard solution is slightly dependent on temperature. Deviations are tabulated in specialized papers. If there are large differences between the sample temperature and standard solutions recourse may be had to corrections made using special settings, which provided the pH meter. Table 1 shows a range of pH and concentrations of standard substance mole (m) of the solutions to be rigorously prepared so as to have their pH value indicated in the table.

Table 1 - Standards of pH Nr. PH standards, according to NIST (National Institute of Standards and Technology) 1 2 3 4 5 6 7
Potassium hydrogen tartrate (C4H5O6K) Potassium citrate biacid (C6H7O7K) Potassium hydrogen phthalate (C8H5O4K) KH2PO4/Na2HPO4 KH2PO4/Na2HPO4 Na2B4O7*10H2O NaHCO3/Na2CO3

Substance

Concentration,m (mol sol/Kg H2O) Saturated solution 0.05 0.05 0.025+0.025 0.008695+0.03043 0.01 0.025+0.025

pHs at 25 C 3.557 3.776 4.008 6.865 7.413 9.180 10.012

5. Glass electrode characteristics 1) Linear response range is generally located between pH 1 and 11. Outside this pH range measurements are affected by errors. For measurements outside this range may be used hydrogen electrode. 2) Sensitivity glass electrode is theoretically expressed by the relation (6). Real sensitivity calibration function defines the expression (equation 8). Sensitivity depends on temperature, which require temperature control both during calibration and measurement stage pH. 3) The accuracy of pH measurements is about 0.01 pH units. Commonly accepted precision measurements is 0.1 pH units. 4) Mechanical and electrical resistance of the membrane. The membrane is made of thin glass with thickness less than 1 mm, resulting in poor mechanical strength and require very careful handling of the electrode. The electrical resistance of the membrane is high (above 10 ^ 8 ), so that the instrument used to measure EMF must have an internal resistance of the order 10 ^ 14 to 10 ^ 16

B. EXPERIMENT DESCRIPTION
Reagents and tools
- Standards of pH (solutions 3 and 6 of Table 1) - 150 ml beaker (3) - Glass electrode - Reference electrode (saturated calomel electrode and silver / silver chloride) - PH meter

Way of working
1. Prepare two standard solutions of pH necessary to calibrate the pH meter. 2. Glass electrode and the reference electrode was washed with distilled water, avoiding reaching peak membrane glass wash bottle. Dry by blotting with filter paper and insert into the cup containing the first standard pH (standard solution 3 in Table 1).

WARNING! Is required Special attention to handling the electrodes! Electrodes not flip and not moving from worktable!

3. It is electrochemical cell as illustrated in Fig. 2. 4. Be observed in their use of the pH meter. 5. After stabilizing the pH meter indication adjust the pH value indicated in the corresponding standard value used (pH = 4.008 to 25 C) by performing switch handling the adjustment of asymmetry.

6. Electrochemical cell recovers repeating steps 2-4 using the pH standard solution 6 in Table 1. 7. After stabilizing the pH meter indication adjust the pH value indicated in the corresponding standard value used (pH = 9.18 to 25 C), the handling switch conducting slope adjustment. 8. Check the correctness of calibration (optional step) using a pH different standard. 9. To determine the pH of an unknown sample electrode was washed with distilled water, dried by blotting with filter paper and insert into the cup containing the sample. 10. After stabilization indication reads pH displayed on the screen of pH meter. 11. The results are presented in a table like the one below:

Presentation of experimental results Solution Standard 1 Standard 2 Standard 3 Sample pH