Fluorescence Analysis of Thermoresponsive Polymers

Author(s):  
Cheryl Morris ◽  
Alan G. Ryder
Author(s):  
D. A. Carpenter ◽  
M. A. Taylor

The development of intense sources of x rays has led to renewed interest in the use of microbeams of x rays in x-ray fluorescence analysis. Sparks pointed out that the use of x rays as a probe offered the advantages of high sensitivity, low detection limits, low beam damage, and large penetration depths with minimal specimen preparation or perturbation. In addition, the option of air operation provided special advantages for examination of hydrated systems or for nondestructive microanalysis of large specimens.The disadvantages of synchrotron sources prompted the development of laboratory-based instrumentation with various schemes to maximize the beam flux while maintaining small point-to-point resolution. Nichols and Ryon developed a microprobe using a rotating anode source and a modified microdiffractometer. Cross and Wherry showed that by close-coupling the x-ray source, specimen, and detector, good intensities could be obtained for beam sizes between 30 and 100μm. More importantly, both groups combined specimen scanning with modern imaging techniques for rapid element mapping.


Author(s):  
D. A. Carpenter ◽  
Ning Gao ◽  
G. J. Havrilla

A monolithic, polycapillary, x-ray optic was adapted to a laboratory-based x-ray microprobe to evaluate the potential of the optic for x-ray micro fluorescence analysis. The polycapillary was capable of collecting x-rays over a 6 degree angle from a point source and focusing them to a spot approximately 40 µm diameter. The high intensities expected from this capillary should be useful for determining and mapping minor to trace elements in materials. Fig. 1 shows a sketch of the capillary with important dimensions.The microprobe had previously been used with straight and with tapered monocapillaries. Alignment of the monocapillaries with the focal spot was accomplished by electromagnetically scanning the focal spot over the beveled anode. With the polycapillary it was also necessary to manually adjust the distance between the focal spot and the polycapillary.The focal distance and focal spot diameter of the polycapillary were determined from a series of edge scans.


2020 ◽  
Vol 86 (10) ◽  
pp. 5-9
Author(s):  
D. G. Filatova ◽  
A. A. Arkhipenko ◽  
M. A. Statkus ◽  
V. V. Es’kina ◽  
V. B. Baranovskaya ◽  
...  

An approach to sorptive separation of Se (IV) from solutions on a novel S,N-containing sorbent with subsequent determination of the analyte in the sorbent phase by micro-x-ray fluorescence method is presented. The sorbent copolymethylenesulfide-N-alkyl-methylenamine (CMA) was synthesized using «snake in the cage» procedure and proven to be stable in acid solutions. Conditions for quantitative extraction of Se (IV) were determined: sorption in 5 M HCl or 0.05 M HNO3 solutions when heated to 60°C, phase contact time being 1 h. The residual selenium content in the solution was determined by inductively coupled plasma mass spectrometry (ICP-MS) using 82Se isotope. The absence of selenium losses is proved and the mechanism of sorption interaction under specified conditions is proposed. The method of micro-x-ray fluorescence analysis (micro-RFA) with mapping revealed a uniform distribution of selenium on the sorbent surface. The possibility of determining selenium in the sorbent phase by micro-RFA is shown. When comparing the obtained results with the results of calculations by the method of fundamental parameters, it is shown the necessity of using standard samples of sorbates to obtain correct results of RFA determination of selenium in the sorbent phase.


2020 ◽  
Vol 74 (4) ◽  
pp. 439-451
Author(s):  
Philipp Holz ◽  
Christoph Pönisch ◽  
Albrecht Brandenburg

Imaging fluorescence spectroscopy proves to be a fast and sensitive method for measuring the thickness of thin coatings in the manufacturing industry. This encouraged us to systematically study, theoretically and experimentally, parameters that influence the fluorescence of thin layers. We analyzed the fluorescence signal as a function of the scattering and reflectance properties of the sample substrate. In addition, we investigated effects of the layer properties on fluorescence emission. A ray-tracing software is used to describe the influence of these parameters on the fluorescence emission of thin layers. Experiments using a custom-made system for imaging fluorescence analysis verify the simulations. This work shows a factor five variation of fluorescence intensity as a function of the reflectance of the sample substrate. Simulations show variations by a factor of up to eight for samples with different surface roughness. Results on tilted samples indicate a significant increase of the detected fluorescence signal, for fluorescent droplets on reflective substrates, if illuminated and coaxially observed at angles greater than 25°. These findings are of utmost relevance for all applications which utilize the fluorescence emission to quantify thin layers. These applications range from in-line lubricant monitoring in press plants to monitoring of functional coatings in medical technology and the detection of filmic contaminations.


1983 ◽  
Vol 19 (2) ◽  
pp. 201-211 ◽  
Author(s):  
A. B. Cormie ◽  
D. E. Nelson

AbstractThe use of energy-dispersive X-ray fluorescence analysis (XES) for the routine identification of three tephras (Mazama, Bridge River, Mount St. Helens Yn) commonly found in archeological sites in British Columbia has been investigated. Researchers have often assumed that chemical analysis of bulk samples of glass separates would be hampered by contamination and weathering effects. Our results indicate that XES of bulk glass separates provides a very reliable method for rapidly identifying the three tephras in question, even with a very simple sample preparation. This should enable persons not skilled in geology or in tephrochronology to collect and to identify samples of these tephras. Finally, as a part of the study, similar measurements were made on the separated glass portions of these three tephras and of three others (Glacier Peak B and G, White River) from northwest North America. The results suggest that this method may provide tephrochronologists with a useful additional tool for studying tephras in other regions.


2021 ◽  
Author(s):  
Maximilian Felix Toni Meier ◽  
Franck Thetiot ◽  
Narsimhulu Pittala ◽  
Ingo Lieberwirth ◽  
Cleiton Kunzler ◽  
...  

We have designed novel macromolecular coordination ligands (MCLs) by conjugation of thermoresponsive polymers based on poly(N-isopropylacrylamide) (M ̅_n around 3 to 25 kg∙mol-1) with 1,2,4-triazole coordination sites. These triazole units...


Polymers ◽  
2020 ◽  
Vol 13 (1) ◽  
pp. 90
Author(s):  
Łukasz Otulakowski ◽  
Maciej Kasprów ◽  
Aleksandra Strzelecka ◽  
Andrzej Dworak ◽  
Barbara Trzebicka

Thermoresponsive polymers are a promising material for drug nanocarrier preparation, which makes the study of their aggregation in physiological conditions very important. In this paper, the thermal behaviour of the thermoresponsive polymers poly(N-isopropylacrylamide), poly(2-isopropyl-2-oxazoline-co-2-n-propyl-2-oxazoline) and poly[(2-hydroxyethyl methacrylate)-co-oligo(ethylene glycol) methyl ether methacrylate] were studied in phosphate buffer (PBS) and solutions of its salts in concentration as in PBS. The thermal response of the polymers was measured using UV-Vis and dynamic light scattering (DLS). The salts shifted the cloud point temperature (TCP) of the (co)polymers to higher values compared to the TCP of aqueous polymer solutions. In PBS and NaCl solutions, all polymers exhibited an unexpected and previously unreported transmittance profile. During heating, an additional aggregation of polymers appeared above the TCP accompanied by the formation of a precipitate. In monosodium phosphate solutions and pure water, the studied polymers showed lower critical solution temperature (LCST-type) behaviour. DLS measurements showed that a salt influenced the size of the resulting polymer particles. The sizes and stability of particles depended on the heating rate. In PBS and NaCl solutions, the size of particles in the dispersion decreased above 60 °C, and the precipitate appeared on the bottom of the cuvette. The additional aggregation of polymer and its falling out of solution may hinder the removal of carriers from the body and has to be taken into account when preparing nanocarriers.


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