Analysis and identification of irradiated Spirulina powder by a three-step infrared macro-fingerprint spectroscopy

A three-step infrared (IR) macro-fingerprint method combining conventional IR spectra, and the secondary derivative spectra with two-dimensional infrared correlation spectroscopy (2D-IR), was developed to analyze Spirulina powder before and after gamma irradiation. In the IR spectra, most of the absorption peaks of samples irradiated at 1, 2.7, 6, and 10.4 kGy had lower intensities than the non-irradiated ones, whereas peaks at 1152, 1078, and 1051 cm⁻¹ were slightly enhanced with irradiation at 2.7, 6, and 10.4 kGy. Their second derivative spectra amplified the differences and revealed that irradiation affected the C=O band of carboxylic acid and esters, and the N–H band of proteins. The peaks at 1746 and 1741 cm⁻¹, and those at 1730 and 1725  cm⁻¹ became two broad peaks. Meanwhile, the three sharp peaks at 1548 cm⁻¹, 1544 cm⁻¹ and 1536 cm⁻¹ changed to two broad peaks at around 1547 and 1534 cm⁻¹ after irradiation at doses higher than 1 kGy. The characteristic IR bands from 1700 cm⁻¹ to 1600 cm⁻¹, which represent the C=O band in proteins, also have different shapes and intensities after irradiation. The finding indicated that irradiation affected the secondary structures of protein which was confirmed by curve fitting results. During the process of increasing the temperature from 50 to 210 °C, the ratio of amide I to II in absorption intensities in the 2D-IR spectra of the irradiated samples varied with different response for different samples. Saccharides in Spirulina powder had a higher thermostability than proteins, but the autopeaks of irradiated samples did show differences from the non-irradiated sample. The intensity of autopeaks at 1012 cm⁻¹ increased dramatically in the irradiated samples while that of peaks at 1053, 1071, and 1083 cm⁻¹ decreased after irradiation. Based on the three-step IR macro-fingerprint method, irradiated Spirulina powder samples were successfully and fast identified and discriminated.     

Microstructural modifications in swift ion irradiated PET

Polyethylene terephthalte (PET) was irradiated with carbon (70 MeV) and copper (120 MeV) ions to analyze the induced modifications with respect to optical, structural and thermal properties. In the present investigation, the fluence for carbon irradiation was varied from 1×10¹¹ to 1×10¹⁴ ions cm⁻², while that for copper beam was kept in the range of 1×10¹¹ to 1×10¹³ ions cm⁻². UV–vis, FTIR, XRD and DSC techniques were utilized to study the induced changes. The analysis of UV–vis absorption studies reveals that there is decrease of optical energy gap up to 10% on carbon ion irradiation (at 1×10¹⁴ ions cm⁻²), whereas the copper beam (at 1×10¹³ ions cm⁻²) leads to a decrease of 49%. FTIR analysis indicated the formation of alkyne end groups along with the overall degradation of polymer with copper ion irradiation. X-ray diffraction analysis revealed that the semi-crystalline PET losses its crystallinity on swift ion irradiation. It was found that the carbon beam (1×10¹⁴ ions cm⁻²) decreased the crystallite size by 16% whereas this decrease is of 12% in case of the copper ion irradiated PET at 1×10¹³ ions cm⁻². The loss in crystallinity on irradiation has been supported by DSC thermograms.     

Electronic and vibrational spectra of tourmaline – The impact of electron beam irradiation and heat treatment

Irradiation and heat treatment were performed on tourmalines of various colors from Antandrokomby, Madagascar. The samples were irradiated with 10 MeV electrons to fluencies of 2 ×10¹⁷ cm⁻² for 1 h and were heated at 550 °C for 3 h in air. Their electronic and vibrational spectra were investigated by UV–vis, mid-infrared, and WD-XRF spectroscopy for comparison to pristine samples. Changes in the Mn³⁺ ions after irradiation resulted in darker pink tourmalines, which had absorption peaks at 390 and 520 nm. These samples became colorless after subsequent heat treatment. After irradiation, colorless, light blue and yellow tourmalines displayed a new absorption band at 365 nm. Alteration of the stretching absorption bands and wavenumber after irradiation could be explained by the following reactions:OH⁻ + e⁻ beam irradiation → O⁻ + H°,Mn²⁺ + e⁻ beam irradiation → Mn³⁺ + e⁻ andFe²⁺ + e⁻ beam irradiation → Fe³⁺ + e⁻.Stretching vibration of the BO₃ structure occurred at 1330 cm⁻¹, while the SiO vibration absorption bands were assigned to around 1100 cm⁻¹. Colorless, green, and yellow tourmalines showed high-intensity peaks around 3608 and 3505 cm⁻¹ after irradiation. Pink and dark green tourmalines showed low-intensity peaks at 3605 and 3585 cm⁻¹, respectively. The combination modes of stretching and bending in the range of 4600–4300 cm⁻¹ were split after irradiation and heat treatment, and different color changes occurred after irradiation.     

Investigation of O7+ swift heavy ion irradiation on molybdenum doped indium oxide thin films

Molybdenum (0.5 at%) doped indium oxide thin films deposited by spray pyrolysis technique were irradiated by 100 MeV O⁷⁺ ions with different fluences of 5×10¹¹, 1×10¹² and 1×10¹³ ions/cm². Intensity of (222) peak of the pristine film was decreased with increase in the ion fluence. Films irradiated with the maximum ion fluence of 1×10¹³ ions/cm² showed a fraction of amorphous nature. The surface microstructures on the surface of the film showed that increase in ion fluence decreases the grain size. Mobility of the pristine molybdenum doped indium oxide films was decreased from ～122 to 48 cm²/V s with increasing ion fluence. Among the irradiated films the film irradiated with the ion fluence of 5×10¹¹ ions/cm² showed relatively low resistivity of 6.7×10^?4 Ω cm with the mobility of 75 cm²/V s. The average transmittance of the as-deposited IMO film is decreased from 89% to 81% due to irradiation with the fluence of 5×10¹¹ ions/cm².     

Characterization of a power bipolar transistor as high-dose dosimeter for 1.9–2.2 MeV electron beams

Results of the characterization studies on a power bipolar transistor investigated as a possible radiation dosimeter under laboratory condition using electron beams of energies from 2.2 to 8.6 MeV and gamma rays from a ⁶⁰Co source and tested in industrial irradiation plants having high-activity ⁶⁰Co γ-source and high-energy, high-power electron beam have previously been reported. The present paper describes recent studies performed on this type of bipolar transistor irradiated with 1.9 and 2.2 MeV electron beams in the dose range 5–50 kGy. Dose response, post-irradiation heat treatment and stability, effects of temperature during irradiation in the range from –104 to +22 °C, dependence on temperature during reading in the range 20–50 °C, and the difference in response of the transistors irradiated from the plastic side and the copper side are reported. DLTS measurements performed on the irradiated devices to identify the recombination centres introduced by radiation and their dependence on dose and energy of the electron beam are also reported.     

Proton (3 MeV) and copper (120 MeV) ion irradiation effects in low-density polyethylene (LDPE)

Low-density polyethylene (LDPE) was irradiated with proton (3 MeV) and copper (120 MeV) ions to analyze the induced modifications with respect to optical and structural properties. In the present investigation, the fluence for proton irradiation was varied up to 2×10¹⁵ protons cm⁻², while that for copper beam was kept in the range of 1×10¹ to 1×10¹³ ions cm⁻² to study the swift heavy ion-induced modifications in LDPE. Ultraviolet–visible (UV–vis), FTIR and X-ray diffraction (XRD) techniques were utilized to study the induced changes. The analysis of UV–vis absorption studies reveals that there is decrease of optical energy gap up to 43% on proton irradiation (at 2×10¹⁵ ions cm⁻²), whereas the copper beam (at 1×10¹³ ions cm⁻²) leads to a decrease of 51%. FTIR analysis indicated the presence of unsaturations due to vinyl end groups in the irradiated sample. The formation of OH and CO groups has also been observed. XRD analysis revealed that the semi-crystalline LDPE losses its crystallinity on swift ion irradiation. It was found that the proton beam (2×10¹⁵ ions cm⁻²) decreased the crystallite size by 23% whereas this decrease is of 31% in case of the copper ion-irradiated LDPE at 1×10¹³ ions cm⁻².     

Radiation induced in-situ generation of conductivity in the blends of polyaniline-base with chlorinated-polyisoprene

Radiation induced acid doping of PANI to generate electrical conductivity was achieved by radiation induced HCl release from chlorinated-polyisoprene (ClPIP). Blends of PANI with ClPIP were prepared by mechanical mixing/grinding in the composition range of 9–43% ClPIP by weight and pelletized under 10 t press. The pellets were irradiated in ⁶⁰Co Gammacell in air at room temperature to doses up to 300 kGy. The maximum electrical conductivity increase was observed for the blend PANI43 which changed from 10^?10 to 10^?4 S cm^?1 when it was irradiated to 300 kGy dose. Radiation induced changes on the blends were also studied by UV–vis spectroscopy using reflection technique and FTIR spectroscopy. The broad absorption band in the visible range (630 nm) increased by increasing irradiation dose. The band (1110 cm^?1) in the IR spectra which is indicative of conductivity showed linear correlation with irradiation dose.     

Effect of swift heavy ion irradiation on ethylene–chlorotrifluoroethylene copolymer

The swift heavy irradiation induced changes taking place in ethylene–chlorotrifluoroethylene (E–CTFE) copolymer films were investigated in correlation with the applied doses. Samples were irradiated in vacuum at room temperature by lithium (50 MeV), carbon (85 MeV), nickel (120 MeV) and silver (120 MeV) ions with the fluence in the range of 1×10¹¹–3×10¹² ions cm^?2. Structural and thermal properties of the irradiated as well as pristine E–CTFE films were studied using FTIR, UV–visible, TGA, DSC and XRD techniques. Swift heavy ion irradiation was found to induce changes in E–CTFE depending upon the applied doses.     

Evolution of microstructure and crack pattern in NiO thin films under 200 MeV Au ion irradiation

NiO thin films grown on Si (100) substrate by electron beam evaporation method and sintered at 700 °C were irradiated with 200 MeV Au¹⁵⁺ ions. The fcc structure of the sintered films was retained up to the highest fluence (1×10¹³ ions cm^?2) of irradiation. However the microstructure of the pristine film underwent a considerable modification with increasing ion fluence. 200 MeV Au ion irradiation led to compressive stress generation in NiO medium. The diameter of the stressed region created by 200 MeV Au ions along the ion path was estimated from the variation of stress with ion fluence and found to be ～11.6 nm. The film surface started cracking when irradiated at and above the fluence of 3×10¹² ions cm^?2. Ratio of the fractal dimension of the cracked surface obtained at 200 MeV and 120 MeV (Mallick et al., 2010a) Au ions was compared with the ratio of the radii of ion tracks calculated based on Coulomb explosion and thermal spike models. This comparison indicated applicability of thermal spike model for crack formation.     

Study on continuous (254 nm) and pulsed UV (266 and 355 nm) lights on BVD virus inactivation and its effects on biological properties of fetal bovine serum

Both continuous UV lights and pulsed UV lasers have potentials to inactivate known and emerging viruses. Bovine viral diarrhea virus (BVDV), from the Pestivirus genus, is known to be a common viral contamination in (fetal) bovine serum (FBS). Also, BVDV has been used in the blood product industry as a surrogate for Hepatitis C virus (HCV), due to its similarity in structure and genome. Germicidal UV lamp with the wavelength of 254 nm and Nd:YAG laser (pulsed UV laser) in its third and fourth harmonic with the wavelengths of 355 and 266 nm, respectively, were used. BVDV suspended in PBS or FBS were exposed to different intensities and doses and then reduction in BVDV titer were calculated. To complete inactivation of BVDV suspended in PBS and PBS containing 5% FBS, 1.6 (t = 30 min) and 3.2 (t = 60 min) J/cm² were used. The minimum doses for inactivation of BVDV suspended in PBS with the 355 and 266 nm of pulsed UV laser were 352 and 92.25 J/cm². Also, the minimum doses for inactivation of BVDV suspended in FBS with 355 and 266 nm wavelengths of pulsed UV laser were 704 and 127 J/cm². To evaluate the irradiated FBS quality to support cell culture growth, FBS was treated with the dose of 190.5 J/cm² and 266 nm pulsed UV laser and was used to grow Vero cells, in comparison with a control group. The viability of cells in two groups was identical and the statistical evaluation showed no significant difference in 12 passages.     

Influence of 670 nm low-level laser therapy on mast cells and vascular response of cutaneous injuries

Laser biomodulation has been getting considerable attention when it comes to its effects on the inflammatory process. Its action upon mast cells have been already studied, but none of the previous papers related the resulting effect to the inflammatory and vascular status of the wounds. Therefore, the acute inflammatory process as well as the mast cells behavior and the vascular response were analyzed under the influence of laser treatment on cutaneous wounds. Surgical procedures were performed on 60 rats divided into sham and laser groups. Low-level laser therapy was performed following surgical procedures (670 nm, 9 mW, 4 J/cm², 124 s). Histological specimens were analyzed for cell morphology and immunohistochemistry using anti-von Willebrand Factor and anti-Vascular Endothelial Growth Factor antibody. Laser treatment resulted in an increased acute inflammatory response in irradiated tissues; surgical wounds treated with laser therapy had increased polymorphonuclear cells, mast cells and vasodilation and lower numbers of vessels than those in control rats. Laser treatment resulted in higher expression of VEGF in irradiated tissues 6–24 h post-treatment (p = 0.002). It is possible to observe an amplification of acute inflammatory process during the first hours after surgical procedure in rats submitted to laser therapy.     

Effect of post-irradiation thermal treatments on the stability of gamma-irradiated glass dosimeter

A commercial window glass has been investigated as a routine high dose dosimeter for gamma irradiation. The irradiated samples showed rapid fading at room temperature immediately after irradiation. This short-term rapid fading was followed by a slow fading at long-term. This strong initial fading is a problem for dosimetry purposes. However, when the dosimeter is measured at the same time interval after irradiation, it maintains proportionality to dose. Calibration curves have to be used for different time intervals after irradiation. In order to improve post-irradiation stability dosimeters were submitted to different post-irradiation thermal treatments from (−20) up to 150 °C. After that, optical absorbance measurements were carried out up to 2 months at room temperature. The heating at 150 °C for 20 min was found to be the most suitable procedure for the removal of unstable entities responsible for the initial rapid fading. Due to these heat treatments, variation of response was found almost negligible 24 h after irradiation for several months. Calibration curves demonstrated the applicability of this glass as routine dosimeter in the dose range of 0.5–90 kGy.     

In vitro evaluation of Radachlorin® sensitizer for photodynamic therapy

This paper reports the evaluation of a new photosensitizer, Radachlorin® in comparison with one of its well known components but used solely, Chlorin e₆. The photodynamic properties and cell uptake and localisation of the two drugs were compared. In vitro studies were conducted on human adenocarcinoma cells (HT29) and lung carcinoma cell line (A549). Both dyes showed an absorption maximum between 640 and 650 nm, but those absorption peaks are enhanced by interactions with serum, with a shifted maximum at 661 and 664 nm, and much higher absorbance. As Radachlorin® is constituted of different products and as photoreactivity is dependent on absorbed light energy, we chose to adapt concentrations so that both drugs had the same absorption at the irradiation wavelength (664 nm) for photoreactivity tests, and express concentrations in optical density at 664 nm. The capacity of the two drugs to generate Reactive Oxygen Species was identical, but on HT29 cells, Radachlorin® reaches its optimal LD50 sooner than Chlorin e₆. Radachlorin® LD50 on HT29 cells was 0.0251 OD_664nm after 2 h and 0.0672 OD_664nm for Chlorin e₆ for a 20 J cm^?2 irradiation. Radachlorin® gave very similar results on A549 cells, LD50 being 0.05 for 5 J irradiation, and 0.026 for 10 and 20 J cm^?2. Pharmacokinetics using fluorescence showed that, even if Radachlorin® quickly crossed HT29 (a human colonic cancer line) cell membrane, cellular distribution evolved from a diffuse cytoplasmic repartition 1 hour after Radachlorin® addition to a delimited localisation into organelles all around the nucleus. Radachlorin® intracellular fluorescence decreased after 4 h, whereas we did not observe a decrease of Chlorin e₆ intracellular fluorescence for times up to 24 h. In both case, a quick decline was observed as soon as the culture medium was replaced with a drug-free one. Radachlorin® appears to be an excellent photosensitizer, with similar phototoxicity to Chlorin e₆ on cell cultures, but with quicker kinetics, which could be an improvement if confirmed on further in vivo studies.     

Photodynamic therapy with aluminum-chloro-phtalocyanine induces necrosis and vascular damage in mice tongue tumors

In this paper we describe the efficacy of the liposomal-AlClPc (aluminum-chloro-phthalocyanine) formulation in PDT study against Ehrlich tumor cells proliferation in immunocompetent swiss mice tongue. Experiments were conduced in sixteen tumor induced mice that were divided in three control groups: (1) tumor without treatment; (2) tumor with 100 J/cm² laser (670 nm) irradiation; and (3) tumor with AlClPc peritumoral injection; and a PDT experimental group when tumors received AlClPc injection followed by tumor irradiation. Control groups present similar macroscopically and histological patterns after treatments, while PDT treatment induced 90% of Ehrlich tumor necrosis after 24 h of one single application, showing the efficacy of liposome-AlClPc (aluminum-chloro-phthalocyanine) mediated PDT on the treatment of oral cancer.     

Opto-structural characterization of proton (3 MeV) irradiated polycarbonate and polystyrene

Polycarbonate (Makrofol-N) and polystyrene thin films were irradiated with protons (3 MeV) under vacuum at room temperature with the fluence ranging from 1×10¹⁴ to 1×10¹⁵ protons cm⁻². The change in optical properties, degradation of the functional groups and crystallinity of the proton-irradiated polymers were investigated with UV–vis, Fourier-transform infrared (FTIR) and X-ray diffraction (XRD) techniques, respectively. The UV–vis analysis revealed that the optical band gap of irradiated Makrofol-N is reduced by 30% as compared to 27.5% in polystyrene at highest fluence of 1×10¹⁵ protons cm⁻², owing to higher electronic energy loss of protons in Makrofol-N. The calculations of the number of carbon atoms per conjugation length, N and number of carbon atoms per clusters, M embedded in the network of polymers further revealed that Makrofol-N is more modified as compared to polystyrene on proton irradiation. FTIR results reveal the reduction in absorption intensity of the main characteristic bands of both the polymers after irradiation. The proton-irradiated Makrofol-N shows a strong decrease of almost all of its characteristic absorption bands at about 1×10¹⁴ protons cm⁻². Beyond a critical dose an increase of almost all its characteristic bands are noticed, however, no such effect had been observed in polystyrene at this particular fluence. Appearance of new –OH groups was observed at the higher fluences in the FTIR spectra of both proton-irradiated polymers. XRD measurements show the decrease of the main peak intensity and the crystallite size, confirming the increase of amorphization in polymers under irradiation.     

Dielectric study of post-irradiation effects in gamma-irradiated polyethylenes

The post-irradiation dielectric behaviour of different polyethylenes (PEs) has been studied by means of dielectric loss (tan δ) analysis over the wide temperature (25–325 K) and frequency (1 kHz–1 MHz) ranges. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were previously gamma irradiated in air to absorbed dose of 300 kGy. The irradiated samples were divided into two groups, and for the first one annealing treatment which can substantially reduce the concentration of free radicals were employed. For the second group, e.g. samples stored in air at room temperature after irradiation, post-irradiation evolution in free radical concentration, dielectric relaxation spectra and carbonyl content was investigated as a function of storage time, up to 90 days. Dielectric relaxation behaviour is related to differences in the initial structures of PEs (such as branching, crystallinity, etc.) and to the radiation-induced effects; carbonyl groups that were introduced by irradiation and/or delayed (post-irradiation) oxidation were regarded as tracer groups. Electron spin resonance (ESR), differential scanning calorimetry (DSC), infrared (IR) spectroscopy and gel measurements were used to determine the changes in free radical concentration, crystal fraction, oxidation and degree of network formation, respectively.     

Positron annihilation study of proton-irradiated reactor pressure vessel steels

The microstructures, irradiation-induced defects and changes of mechanical property of Chinese domestic A508-3 steels after proton irradiation were investigated by TEM, positron lifetime, slow positron beam Doppler broadening spectroscopy and hardness measurements. The defects were induced by 240 keV proton irradiation with fluences of 1.25×10¹⁷ ions cm^?2 (0.26 dpa), 2.5×10¹⁷ ions cm^?2 (0.5 dpa), and 5.0×10¹⁷ ions cm^?2 (1.0 dpa). The TEM observation revealed that the as-received steel had typical bainitic–ferritic microstructures. It was also observed that Doppler broadening S-parameter and average lifetime increased with dose level owing to the formation of defects and voids induced by proton irradiation. The correlation between positron parameters and hardness was found.     

Effects of electron beam irradiation on the photoelectrochemical properties of TiO2 film for DSSCs

TiO₂ has been widely utilized for various industrial applications such as photochemical cells, photocatalysts, and electrochromic devices. The crystallinity and morphology of TiO₂ films play a significant role in determining the overall efficiency of dye-sensitized solar cells (DSSCs). In this study, the preparation of nanostructured TiO₂ films by electron beam irradiation and their characterization were investigated for the application of DSSCs. TiO₂ films were exposed to 20–100 kGy of electron beam irradiation using 1.14 MeV energy acceleration with a 7.46 mA beam current and 10 kGy/pass dose rates. These samples were characterized using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and X-ray photoelectron spectroscopy (XPS) analysis. After irradiation, each TiO₂ film was tested as a DSSC. At low doses of electron beam irradiation (20 kGy), the energy conversion efficiency of the film was approximately 4.0% under illumination of simulated sunlight with AM 1.5 G (100 mW/cm²). We found that electron beam irradiation resulted in surface modification of the TiO₂ films, which could explain the observed increase in the conversion efficiency in irradiated versus non-irradiated films.     

Detection of irradiated quail meat by using DNA comet assay and evaluation of comets by image analysis

A simple technique of microgel electrophoresis of single cells (DNA comet assay) was used to detect DNA comets in irradiated quail meat samples. Obtained DNA comets were evaluated by both photomicrographic and image analysis. Quail meat samples were exposed to radiation doses of 0.52, 1.05, 1.45, 2.00, 2.92 and 4.00 kGy in gamma cell (gammacell ⁶⁰Co, dose rate 1.31 kGy/h) covering the permissible limits for enzymatic decay and stored at 2 °C. The cells isolated from muscle (chest, thorax) in cold PBS were analyzed using the DNA comet assay on 1, 2, 3, 4, 7, 8 and 11 day post irradiation. The cells were lysed between 2, 5 and 9 min in 2.5% SDS and electrophorosis was carried out at a voltage of 2 V/cm for 2 min. After propidium iodide staining, the slides were evaluated through a fluorescent microscope. In all irradiated samples, fragmented DNA stretched towards the anode and damaged cells appeared as a comet. All measurement data were analyzed using BS 200 ProP with software image analysis (BS 200 ProP, BAB Imaging System, Ankara, Turkey). The density of DNA in the tails increased with increasing radiation dose. However, in non-irradiated samples, the large molecules of DNA remained relatively intact and there was only minor or no migration of DNA; the cells were round or had very short tails only. The values of tail DNA%, tail length and tail moment were significantly different and identical between 0.9 and 4.0 kGy dose exposure, and also among storage times on day 1, 4 and 8. In conclusion, the DNA Comet Assay EN 13784 standard method may be used not only for screening method for detection of irradiated quail meat depending on storage time and condition but also for the quantification of applied dose if it is combined with image analysis. Image analysis may provide a powerful tool for the evaluation of head and tail of comet intensity related with applied doses.