| Literature DB >> 28903219 |
Suzana Cakić1, Ljiljana Raskovic2, Časlav Lačnjevac3, Milos Rajkovic4, Miroljub Barać5, Miodrag Stojanovic6.
Abstract
The FTIR spectroscopy has been employed in this research work to monitor theprocess of nitrodope photodegradation, by measuring surfaces of bands typical of a nitrogroup. Nitric esters are subject to degradation, which is reflected on a quantitative ratio ofthe surfaces of the IR bands that originate from the nitric ester. The obtained results showthat the length of the UV rays' activity on the samples over the time periods of 240, 480and 960 minutes directly affects the spectrum appearance of the same sample before andafter the irradiation. The longer the action time of the UV rays and the higher a masspercentage of nitrocellulose in the nitrodope is, the smaller the bands' surfaces become, i.e.the level of degradation is higher. In order to confirm the degradation of nitrodope, thedegree of crosslinking has also been examined by determining the König hardness and alsothe mean viscosity molar mass has been defined repeatedly applying the capillaryviscosimetry method.Entities:
Keywords: FTIR spectroscopy; König hardness; UV-radiation; nitrocellulose; nitrodope
Year: 2007 PMID: 28903219 PMCID: PMC3864514 DOI: 10.3390/S7102139
Source DB: PubMed Journal: Sensors (Basel) ISSN: 1424-8220 Impact factor: 3.576
Figure 1.Pathways of secondary decomposition.
The effect of UV light on cellulose nitrate stability.
| Condtionon | Relative Viscosity | Intrinsic Viscosity | |||
|---|---|---|---|---|---|
| Start | Finish | Start | Finish | ||
| Dark, air | 1,266 | 1,258 | 1,187 | 1,031 | |
| UV, N2 | 1,268 | 1,231 | 1,179 | 1,148 | |
| UV, air | 1,270 | 1,031 | 1,195 | 0,153 | |
The hardness values of the nitrodope dry films before and after the action of UV rays.
| Sample I | Sample II | Sample III | Sample IV | |
|---|---|---|---|---|
| 0 | 118 | 162 | 179 | 182 |
| 240 | 129 | 154 | 169 | 176 |
| 0 | 140 | 176 | 185 | 192 |
| 480 | 166 | 166 | 178 | 181 |
| 0 | 133 | 170 | 175 | 188 |
| 960 | 148 | 169 | 172 | 182 |
Viscosity values of nitrodope solution in acetone for sample I.
| 0,25 | 25,0 | 1,06383 | 0,06383 | 0,25532 |
| 0,50 | 26,5 | 1,12766 | 0,12766 | 0,25532 |
| 0,75 | 28,5 | 1,21277 | 0,21277 | 0,28369 |
| 0,25 | 24,5 | 1,04255 | 0,04255 | 0,17021 |
| 0,50 | 25,8 | 1,09787 | 0,09787 | 0,19574 |
| 0,75 | 27,0 | 1,14894 | 0,14894 | 0,19858 |
| 0,25 | 24,1 | 1,02553 | 0,02553 | 0,10213 |
| 0,50 | 25,0 | 1,06383 | 0,06383 | 0,12766 |
| 0,75 | 26,5 | 1,12766 | 0,12766 | 0,17021 |
Viscosity values of nitrodope solution in acetone for sample II.
| 0,25 | 26,5 | 1,12766 | 0,12766 | 0,51064 |
| 0,50 | 28,1 | 1,19574 | 0,19574 | 0,39149 |
| 0,75 | 29,6 | 1,25957 | 0,25957 | 0,34610 |
| 0,25 | 26,2 | 1,11489 | 0,11489 | 0,45957 |
| 0,50 | 27,2 | 1,15745 | 0,15745 | 0,31489 |
| 0,75 | 29,6 | 1,25957 | 0,25957 | 0,34610 |
| 0,25 | 25,0 | 1,06383 | 0,06383 | 0,25532 |
| 0,50 | 26,0 | 1,10638 | 0,10638 | 0,21277 |
| 0,75 | 26,9 | 1,14468 | 0,14468 | 0,19291 |
Viscosity values of nitrodope solution in acetone for sample III
| 0,25 | 27,8 | 1,18298 | 0,18298 | 0,73191 |
| 0,50 | 29,0 | 1,23404 | 0,23404 | 0,46809 |
| 0,75 | 31,2 | 1,32766 | 0,32766 | 0,43688 |
| 0,25 | 26,8 | 1,14043 | 0,14043 | 0,56170 |
| 0,50 | 28,1 | 1,19574 | 0,19574 | 0,39149 |
| 0,75 | 30,0 | 1,27660 | 0,27660 | 0,36879 |
| 0,25 | 25,9 | 1,10213 | 0,10213 | 0,40851 |
| 0,50 | 26,9 | 1,14468 | 0,14468 | 0,28936 |
| 0,75 | 28,0 | 1,19149 | 0,19149 | 0,25532 |
Viscosity values of nitrodope solution in acetone for sample IV
| 0,25 | 28,7 | 1,22128 | 0,22128 | 0,88511 |
| 0,50 | 30,0 | 1,27660 | 0,27660 | 0,55319 |
| 0,75 | 31,9 | 1,35745 | 0,35745 | 0,47660 |
| 0,25 | 27,5 | 1,17021 | 0,17021 | 0,68085 |
| 0,50 | 29,0 | 1,23404 | 0,23404 | 0,46809 |
| 0,75 | 30,1 | 1,28085 | 0,28085 | 0,37447 |
| 0,25 | 26,6 | 1,13191 | 0,13191 | 0,52766 |
| 0,50 | 27,6 | 1,17447 | 0,17447 | 0,34894 |
| 0,75 | 28,0 | 1,19149 | 0,19149 | 0,25532 |
Figure 2.Dependence of reduced viscosity on the concentration of nitrodope dissolved in acetone, for sample I : a) no action of UV-rays, b) after 40-minute action of UV-rays, c) after 960-minute action of UV-rays.
Figure 3.Collective graph of the dependence of the mean molar mass of nitrodope on the mass percentage of nitrocellulose before and after the UV radiation.
Figure 4.Comparative FTIR spectrum of the nitric group for: a) sample I, b) sample II, c) sample III, d) sample IV.
Surfaces of the characteristic IR bands of a nitro group for nitrodope samples with different contents of nitrocellulose.
| νas(1660 cm-1) | νs (1280 cm-1) | νas(1660 m-1) | νs (1280 cm-1) | νas(1660 cm-1) | νs (1280 cm-1) | νas(1660 cm-1) | νs (1280 cm-1) | |||
|---|---|---|---|---|---|---|---|---|---|---|
| 0 | 38.28 | 66.70 | 41.86 | 67.86 | 45.60 | 68.44 | 47.53 | 70.21 | ||
| 240 | 37.41 | 65.55 | 40.05 | 66.70 | 43.71 | 67.86 | 46.56 | 68.15 | ||
| 480 | 36.55 | 64.41 | 39.16 | 65.55 | 42.78 | 66.70 | 44.65 | 67.57 | ||
| 960 | 35.28 | 63.84 | 38.28 | 64.98 | 41.86 | 65.55 | 43.24 | 66.12 | ||
Prescription content of colourless nitrodope.
| Component | Sample I mass % | Sample II mass % | Sample III mass % | Sample IV mass % |
|---|---|---|---|---|
| Nitro diluent | 36.8 | 36.8 | 36.8 | 36.8 |
| n-butylalcohol | 7.0 | 7.0 | 7.0 | 7.0 |
| Butyl acetate | 17.0 | 17.0 | 17.0 | 17.0 |
| Dioctylphthalate | 4.0 | 4.0 | 4.0 | 4.0 |
| 15 | 18 | 20 | 25 | |
| 5.0 | 5.0 | 5.0 | 5.0 | |
| 10.0 | 10.0 | 10.0 | 10.0 | |
| POLICOL N (phenol-formaldehyde resin) | 3.0 | 3.0 | 3.0 | 3.0 |
Medium-viscosity nitrocellulose containing 11.8 – 12.3 % of nitrogen.
Alkyd resin modified by dehydrated castor oil.
Alkyd resin modified by soybean oil.