Oxidation of ultralene and paraffin due to radiation damage after exposure to soft X-rays probed by FTIR microspectroscopy and X-ray fluorescence

2021 ◽  
Vol 28 (1) ◽  
pp. 231-239
Author(s):  
Diana E. Bedolla ◽  
Giovanni Birarda ◽  
Sabina Giannotta ◽  
Valentina Faoro ◽  
Alberto Cescato ◽  
...  

Radiation damage upon soft X-ray exposure is an important issue to be considered in soft X-ray microscopy. The work presented here is part of a more extended study on the topic and focuses on the effects of soft X-rays on paraffin, a common embedding medium for soft-tissues, and on ultralene and Si3N4 windows as sample supports. Our studies suggest that the sample environment indeed plays an important role in the radiation damage process and therefore should be carefully taken into account for the analysis and interpretation of new data. The radiation damage effects were followed over time using a combination of Fourier transform infrared (FTIR) microspectroscopy and X-ray fluorescence (XRF), and it was demonstrated that, for higher doses, an oxidation of both embedding medium and ultralene substrate takes place after the irradiated sample is exposed to air. This oxidation is reflected in a clear increase of C=O and O—H infrared bands and on the XRF oxygen maps, correlated with a decrease of the aliphatic infrared signal. The results also show that the oxidation process may affect quantitative evaluation of light element concentrations.

Author(s):  
Shawn Williams ◽  
Xiaodong Zhang ◽  
Susan Lamm ◽  
Jack Van’t Hof

The Scanning Transmission X-ray Microscope (STXM) is well suited for investigating metaphase chromosome structure. The absorption cross-section of soft x-rays having energies between the carbon and oxygen K edges (284 - 531 eV) is 6 - 9.5 times greater for organic specimens than for water, which permits one to examine unstained, wet biological specimens with resolution superior to that attainable using visible light. The attenuation length of the x-rays is suitable for imaging micron thick specimens without sectioning. This large difference in cross-section yields good specimen contrast, so that fewer soft x-rays than electrons are required to image wet biological specimens at a given resolution. But most imaging techniques delivering better resolution than visible light produce radiation damage. Soft x-rays are known to be very effective in damaging biological specimens. The STXM is constructed to minimize specimen dose, but it is important to measure the actual damage induced as a function of dose in order to determine the dose range within which radiation damage does not compromise image quality.


Author(s):  
Martin E. Atkinson

The radiographs most frequently taken in general dental practice are of the teeth and their immidiate supporting tissues for detection of dental caries or assessment of bone loss in periodontal disease. Intraoral radiographs are taken by placing the X-ray-sensitive film or receptor in the mouth close to the teeth being investigated. Extraoral radiographs use larger films or receptors positioned externally and produce a view of the entire dentition and its supporting structures on a single film; they are used to ascertain the state of development of the dentitions prior to orthodontic treatment, for example. Dental panoramic tomographs (DPTs) are the most frequent extraoral radiographs. A radiograph is a negative photographic record. Dense structures such as bone are designated as radio-opaque; they absorb some X-rays and appear white on radiographs. More X-rays pass through less dense radiolucent structures such as air-filled cavities which show up as black areas. The contrast between different tissues of the structures which the X-ray beam passes through is determined by their radiodensity which, in turn, is largely due to their content of metallic elements. Calcium and iron are the prevalent heavy metals in the body. Calcium is combined with phosphate to form hydroxyapatite crystals in bones and mineralized tissues in teeth. Iron is present in haemoglobin in blood, but only large concentrations of blood, such as those found within the heart chambers, show up on X-rays. In sequence from densest to most lucent, the radiodensity of the dental and periodontal tissues are: enamel, dentine, cementum, compact bone, cancellous bone, demineralized carious enamel and dentine, dental soft tissues such as pulp and periodontal ligament, and air; gold and silver–mercury amalgam metallic restorative materials are even denser than enamel. A radiograph is a two-dimensional representation of a three-dimensional situation. The orientation of anatomical structures relative to the X-ray beam is a major factor determining their appearance on the film. For example, a beam travelling through the long axis of a radiodense structure will produce a whiter image on the film than one passing through its shorter axis because more X-rays are absorbed; the structure will also have a different shape.


1969 ◽  
Vol 13 ◽  
pp. 26-48
Author(s):  
A. K. Baird

Qualitative and quantitative analyses of elements below atomic number 20, and extending to atomic number 4, have been made practical and reasonably routine only in the past five to ten years by advances in: 1) excitation sources; 2) dispersive spectrometers; 3) detection devices; and 4) reductions of optic path absorption. At present agreement is lacking on the best combination of parameters for light element analysis. The principal contrasts in opinion concern excitation.Direct electron excitation, particularly as employed in microprobe analysis (but not limited to such instruments), provides relatively high emission intensities of all soft X-rays, but also generates a high continuum, requires the sample to be at essentially electron gun vacuum, and introduces practical calibration problems (“matrix effects“). X-ray excitation of soft X-rays overcomes some of the latter three disadvantages, and has its own limitations. Sealed X-ray sources of conventional or semi-conventional design can provide useful (if not optimum) light element emission intensities down to atomic number 9, hut with serious loss of efficiency in many applications below atomic number 15 largely because of window-thinness limitations under electron bombardment.


2019 ◽  
Vol 21 (23) ◽  
pp. 12389-12395 ◽  
Author(s):  
Remo N. Widmer ◽  
Giulio I. Lampronti ◽  
Nicola Casati ◽  
Stefan Farsang ◽  
Thomas D. Bennett ◽  
...  

Accumulation of radiation damage from synchrotron X-rays leads to complete amorphization of the initially crystalline metal–organic frameworks ZIF-4, ZIF-62, and ZIF-zni. The mechanism of this transformation is studied as a function of time and temperature and is shown to be non-isokinetic.


2014 ◽  
Vol 83 (9) ◽  
pp. 094301
Author(s):  
Takeshi Kai ◽  
Atsushi Tokuhisa ◽  
Kengo Moribayashi ◽  
Yuji Fukuda ◽  
Hidetoshi Kono ◽  
...  
Keyword(s):  
X Rays ◽  

2019 ◽  
Vol 26 (4) ◽  
pp. 912-921 ◽  
Author(s):  
Go Ueno ◽  
Atsuhiro Shimada ◽  
Eiki Yamashita ◽  
Kazuya Hasegawa ◽  
Takashi Kumasaka ◽  
...  

To investigate the effect of high-energy X-rays on site-specific radiation-damage, low-dose diffraction data were collected from radiation-sensitive crystals of the metal enzyme cytochrome c oxidase. Data were collected at the Structural Biology I beamline (BL41XU) at SPring-8, using 30 keV X-rays and a highly sensitive pixel array detector equipped with a cadmium telluride sensor. The experimental setup of continuous sample translation using multiple crystals allowed the average diffraction weighted dose per data set to be reduced to 58 kGy, and the resulting data revealed a ligand structure featuring an identical bond length to that in the damage-free structure determined using an X-ray free-electron laser. However, precise analysis of the residual density around the ligand structure refined with the synchrotron data showed the possibility of a small level of specific damage, which might have resulted from the accumulated dose of 58 kGy per data set. Further investigation of the photon-energy dependence of specific damage, as assessed by variations in UV-vis absorption spectra, was conducted using an on-line spectrometer at various energies ranging from 10 to 30 keV. No evidence was found for specific radiation damage being energy dependent.


1994 ◽  
Vol 38 ◽  
pp. 299-305
Author(s):  
Daniel J. Whalen ◽  
D. Clark Turner

Abstract Widespread interest in light element analysis using XRF has stimulated the development of thin x-ray tube windows. Thinner windows enhance the soft x-ray output of the tube, which more efficiently excite the light elements in the sample. A computer program that calculates the effect of window thickness on light element sample fluorescence has been developed. The code uses an NIST algorithm to calculate the x-ray tube spectrum given various tube parameters such as beryllium window thickness, operating voyage, anode composition, and take-off angle. The interaction of the tube radiation with the sample matrix is modelled to provide the primary and secondary fluorescence from the sample. For x-rays in the energy region 30 - 1000 eV the mass attenuation coefficients were interpolated from the photo absorption data compilation of Henke, et al. The code also calculates the x-ray background due to coherent and incoherent scatter from the sample, as well as the contribution of such scatter to the sample fluorescence. Given the sample fluorescence and background the effect of tube window thickness on detection limits for light elements can be predicted.


2018 ◽  
Vol 25 (3) ◽  
pp. 848-856 ◽  
Author(s):  
Diana E. Bedolla ◽  
Andrea Mantuano ◽  
Arissa Pickler ◽  
Carla Lemos Mota ◽  
Delson Braz ◽  
...  

Radiation damage is an important aspect to be considered when analysing biological samples with X-ray techniques as it can induce chemical and structural changes in the specimens. This work aims to provide new insights into the soft X-ray induced radiation damage of the complete sample, including not only the biological tissue itself but also the substrate and embedding medium, and the tissue fixation procedure. Sample preparation and handling involves an unavoidable interaction with the sample matrix and could play an important role in the radiation-damage mechanism. To understand the influence of sample preparation and handling on radiation damage, the effects of soft X-ray exposure at different doses on ultralene, paraffin and on paraffin-embedded rat tissues were studied using Fourier-transform infrared (FTIR) microspectroscopy and X-ray microscopy. Tissues were preserved with three different commonly used fixatives: formalin, glutaraldehyde and Karnovsky. FTIR results showed that ultralene and paraffin undergo a dose-dependent degradation of their vibrational profiles, consistent with radiation-induced oxidative damage. In addition, formalin fixative has been shown to improve the preservation of the secondary structure of proteins in tissues compared with both glutaraldehyde and Karnovsky fixation. However, conclusive considerations cannot be drawn on the optimal fixation protocol because of the interference introduced by both substrate and embedding medium in the spectral regions specific to tissue lipids, nucleic acids and carbohydrates. Notably, despite the detected alterations affecting the chemical architecture of the sample as a whole, composed of tissue, substrate and embedding medium, the structural morphology of the tissues at the micrometre scale is essentially preserved even at the highest exposure dose.


That a change of wave-length occurs in X-ray scattering was first indicated by absorption measurements with the ionisation chamber, which showed that the absorption coefficient of a light element like aluminium was slightly greater for the scattered than for the primary X-rays. Later more conclusive and direct evidence was obtained when spectrometric analysis of the scattered X-rays was made first by the ionisation and afterwards by the photographic method. This analysis disclosed the existence of an unshifted as well as the shifted line, and showed also that the latter becomes relatively more prominent with diminishing wave-length and lower atomic number of the scattering element. After the main features of the Compton effect were established by means of spectrometric measurements, however, absorption measurements with the ionisation method have again been employed for a detailed study of the phenomenon, for such measurements are much quicker than the spectrum experiments, where the final energy available is much smaller on account of the double scattering involved. As mentioned above, the absorption measurements were based on the slight increase in the absorption coefficient of a light element when the wave-length changes from the unmodified to the modified value. The much larger and sudden diminution in absorption of X-rays when the frequency is altered from the short to the long wave-length side of the critical K-absorption limit of the element used as a filter, furnishes us with an easy and convenient method of exhibiting the wave-length change in X-ray scattering. In the present paper will be described a photographic wedge photometer based on this principle, which enables the characteristics of the Compton effect to be readily observed. It may be pointed out that the same idea could no doubt be utilised also in connection with the ionisation measurements of the Compton effect.


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