**3.4.2 Spectroscopic analysis**

### **3.4.2.1 Ultraviolet spectroscopic studies**

The UV vis. spectra of OCP and its homopolymer POCP and OHP and its homopolymer POHP are shown in Fig 10 (a-d)

Fig. 10. Uv-vis. Spectra of OCP, OHP, POCP and POHP.


The absorption bands shown in the spectra are summarized in Table 3.

Table 3. The Uv-vis. assignments.

36 Electropolymerization

The UV vis. spectra of OCP and its homopolymer POCP and OHP and its homopolymer

C% H% Cl% S%

2.48 2.10

3.83 4.15

Cal/found Cal/found Cal/found Cal/found

23.22 23.01


4.00 3.48

Elemental analysis

47.5

54.25

Table 2. Elemental analytical data of the prepared homopolymers

Fig. 10. Uv-vis. Spectra of OCP, OHP, POCP and POHP.

No Structure of polymer

**3.4.2 Spectroscopic analysis** 

POHP are shown in Fig 10 (a-d)

1 POCP 47.1

2 POHP 55.24

**3.4.2.1 Ultraviolet spectroscopic studies** 

### **3.4.2.2 Infrared spectroscopic studies**

The infrared spectra of OCP monomer and its prepared homopolymer POCP are represented in Fig. 11(a) where the infrared spectra of OHP monomer and its prepared homopolymer POHP are represented in Fig. 11(b). The IR absorption bands and their assignments are given in Tables 4 and 5.

Fig. 11. IR spectra of OCP, POCP, OHP and POHP.

Electropolymerization of Some Ortho-Substituted Phenol Derivatives on Pt-Electrode from

Fig. 12. 1HNMR spectra of POCP and POHP in DMSO and DMSO+D2O.

there are three stages during thermolysis of the POCP sample

24.04% which is in good agreement with the calculated value (24.8%)

decomposition,is equal to 70.70. The found data equal to 69.5.

there are four stages during thermolysis of the polymer sample

Thermogravimetric analysis (TGA) for the electrochemically prepared POCP and POHP samples have been investigated and the TGA-curve is represented in Figure 13 (a and b). The TGA steps of the prepared POCP are shown in Fig 13(a) from which it is shown that

The first stage : including the loss of 2H2O molecules in the temperature range between 25oC and 120oC , The weight loss was found to be (5.30%) which is in good agreement with the calculated value (5.70%)this is in good agreement with what was found in the literature for

second stage: includes the loss of the dopant species , SO3 and one benzenoide ring in the temperature range between 120 oC and 400oC , the weight loss for this step was found to be

The third stage: in the range of temperature >490 oC, the remaining part of the polymer

The TGA steps of the prepared POHP are shown in Fig. 13 (b) from which it is shown that

The first stage: including the loss of 2H2O molecules in the temperature range between 25 oC and 100oC , The weight loss was found to be(4.35%) which is in good agreement with

**3.4.2.4 Thermogravimetric analysis(TGA)** 

water release [Sayyah et al 2010].

the calculated value(4.6%) .

**3.4.2.3 1HNMR spectroscopic studies** 

investigated sample.

Aqueous Acidic Solution; Kinetics, Mechanism, Electrochemical Studies and Characterization of… 39

The 1HNMR spectrum of the prepared POCP and POHP are represented in Fig.12 (a and b). The figure shows two solvent signals at δ=2.55 ppm and δ=3.55 ppm in case of POCP where in case of POHP the solvent signals appear at δ=2.15 ppm and δ=2.55 ppm. The protons of benzene rings in the polymeric structures appear in the region from δ=6.04 to δ=8 ppm in both cases. The singlet signal appears at δ=4.3 ppm in case of POCP and at 5.5 ppm in case of POHP is attributed to OH protons for water of solvation. The singlet signal appears at δ=10.1ppm in case of POCP and at δ=9.5 is attributed to OH proton attached to for benzene ring. The signals of different (OH) are disappeared when deuterated water was added to the


Table 4. IR adsorption bands and their assignments for OCP and POCP.(*where; s: strong, w: weak, b: broad, m:medium*}


Table 5. IR adsorption bands and their assignments for OHP and POHP.(*where; s: strong, w: weak, b: broad, m:medium*)
