scholarly journals Purification of Crude Sodium Di-Uranate from Tummalapalle Source, India to Nuclear Grade Ammonium Di-Uranate Using Sulphamic Acid Dissolution Route

2021 ◽  
pp. 40-58
Author(s):  
Sujoy Biswas ◽  
Aswin Pradeep ◽  
Vijay Hiraman Rupawate ◽  
Manharn Lal Sahu ◽  
Madangopal Krishnan

Crude Sodium Di-Uranate (SDU) of Tummalapalle mine India, contains 2-3% (w/w) of silica besides 5-7% (w/w) of organic matter including polyacrylamides and humic masses with 2-5% Zirconium (Zr) (w/w) as major impurities, hence the direct conversion of SDU, to Nuclear Grade (NG) Ammonium Di-Uranate Cake (ADUC) for fuel fabrication via HNO3-Tributyl Phosphate (TBP) extraction route is onerous due to silica gel creation, third phase inception enounces presence of excess Zr and micro-emulsion formation confirms organic matter introduces difficulties in filtration, recovery and purification stages. Various analytical techniques such as X-Ray Diffraction Analysis (XRD), Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray Spectroscopy (EDS), Fourier Transform Infrared Spectroscopy (FTIR) as well as Inductively Coupled Optical Emission Spectrometer (ICP-OES) has been utilized to characterize raw material (SDU), intermediate products (gel and residues) as well as final product (NG-ADUC). In this research; an innovative, novel route for dissolution of SDU employing sulphamic acid (25% w/v) to remove silica, organic matter, and Zr followed by the conventional route to NG-ADU; eliminates the three major process difficulties viz., (i) gelation, (ii) third phase formation and (iii) microemulsion formation. In addition, sulphamic acid extracted Uranium (U)-bearing stream ultimately articulates 99.5% overall U recovery and enunciates nuclear grade U with desirable morphological characteristics.

Author(s):  
Ashok B. Patel ◽  
Avadhi R. Bundheliya ◽  
Amitkumar J. Vyas ◽  
Nilesh K. Patel ◽  
Ajay I. Patel ◽  
...  

Sources of metal impurities can from anywhere in drug product as raw material which may produce using metal catalyst, excipients, process materials, Water or any solvent used, manufacturing equipment, environment, packaging materials. So, it leads to metal impurity in high amount present in final drug product that is why it is important to check the impurity level in final drug product or as well as in process also that it should be present in low or acceptable amount. Any Drug product is not completely pure, some amount of metal impurities are always present in pharmaceutical product may cause various toxicity when it will be administered. Thus it is necessary to check impurity level is present at acceptable amount. The present review gives an account of updated information about metal impurities and reviews the regulatory aspects for such metal impurities in drug substance/drug product. In addition the aim of this article is to discuss the currently used different analytical techniques for detection of metals from drug product like spectrophotometry, X – Ray florescence spectrometry, AAS, INAA, ICP – AES, ICP – MS, MP – AES, Laser Ablation – ICP – MS etc which is used for quality control of metal impurities in pharmaceuticals.


Author(s):  
John H.L. Watson ◽  
John L. Swedo ◽  
E. Osborne Coates

Prolonged inhalation of tungsten carbide has long been suspected of causing progressive lung disease in humans. In the work reported, tungsten carbide (WC) has been identified by X-ray diffraction in lung tissue from a tungsten carbide worker. While the major part of the raw material handled by the patient is known to have been tungsten carbide, it also contained 6% cobalt, with trace amounts of other metals. Neutron activation analysis with the same tissue has confirmed the presence of large amounts of tungsten, and the faint lines of tungsten were also revealed by optical emission spectroscopy. Light microscopy has showed extensive, patchy, interstitial pneumonitls with considerable cellular component, interstitial fibrous tissue and metaplasia of the alveolar epithelium. For electron microscopy the tissue was fixed in caccodylate buffered glutaraldehyde, post-fixed in phosphate buffered osmium tetroxide, embedded in Araldite and thin sectioned with a diamond knife. The sections were further contrasted with lead citrate and uranyl acetate.


2008 ◽  
Vol 569 ◽  
pp. 341-344
Author(s):  
F. Vázquez Acosta ◽  
Leticia M. Torres-Martínez ◽  
Lorena L. Garza-Tovar ◽  
A. Martínez-de la Cruz ◽  
Wallter López González

A kaolin obtained from a region near to San Luis Potosí (México) was characterized by X-ray powder diffraction (DRX), optical microscopy (OM), scanning electron microscopy (SEM), X-ray fluorescence (XRF), thermal analysis (DTA/TGA), and chemical analysis. Mineralogical and morphological characteristics of the mineral are presented. The kaolin sample was formed mainly by kaolinite, but other minor phases were also detected such as quartz, cristobalite, trydimite, and dolomite. For iron lixiviation process, concentrate HCl was employed. The high content of volcanic glass detected, evidenced by optical microscopy, revealed an incomplete kaolinization process of the raw material. In agreement with these results, X-ray fluorescence analysis showed high- SiO2 and low-Al2O3 content in the sample as is expected on weakly kaolinized materials.


2019 ◽  
Vol 14 ◽  
pp. 155892501989034 ◽  
Author(s):  
Xu Peng

The silica leached from coal fly ash using alkali, via the hydrothermal method, can be used as the raw material for the synthesis of xonotlite fibers through the hydrothermal synthesis method. This investigation was made to examine how the fly ash desilicated liquid influences the crystal growth and microstructure of xonotlite fibers. The obtained samples were characterized by X-ray diffraction and scanning electron microscope techniques to investigate their mineralogical composition and morphological characteristics. The results indicated that the pure desilication liquid leached from coal fly ash could be used to prepare xonotlite fibers. Xonotlite fibers with single crystal characteristics and large aspect ratio of 100–400 were successfully fabricated from fly ash desilication liquid, which is used as the silica material, at 240°C for 6 h.


2016 ◽  
Vol 22 (1) ◽  
pp. 32-37
Author(s):  
ANA-MARIA GEORGESCU ◽  
FRANÇOISE NARDOU ◽  
DENISA NISTOR ILEANA

A calcium bentonite from Orasu Nou deposit (Romania) was used as raw material. The natural bentonite provided by S.C. Bentonita S.A., Satu Mare has the following mineralogical composition: 57 % montmorillonite, 40 % cristobalite, and 3 % quartz. Due to the relatively high percentage of impurities in natural calcium bentonite, we decided to purify the raw material, in order to improve the quality of montmorillonite. Through purification procedure, well defined granulometric fractions with particles of less than 2 μm, are obtained. The crude and purified calcium bentonites were characterized by textural analysis, scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDX). The physical, structural and morphological characteristics are affected by the purification process. The purified bentonite can be used to obtain advanced materials, which can be tested as adsorbents for environmental remediation.


Soil Research ◽  
2019 ◽  
Vol 57 (6) ◽  
pp. 535
Author(s):  
Ilaria Piccoli ◽  
Nicola Dal Ferro ◽  
Patrice J. Delmas ◽  
Andrea Squartini ◽  
Francesco Morari

Soil organic matter (SOM) plays a key role in soil structure formation, although the bidirectional relationship between SOM and the soil pore network is complex and needs further investigation. Despite great advances provided by X-ray computed microtomography (µCT), it has only been used in a few studies to investigate the organic matter 3D-arrangement within the soil matrix. Results are based on the X-ray linear attenuation coefficient (α), and mixtures of organic and mineral soil fractions could imply overlapping of information that makes any segmentation procedure difficult. The aim of this study was to visualise, segment, and quantify the particulate organic matter fraction (POM) within the soil matrix through X-ray µCT in combination with contrast agents (phosphomolybdic acid and silver nitrate). Two series of repacked soil cores, ‘dry’ and ‘wet’, were scanned through X-ray µCT at a 7-µm resolution. Different segmentation approaches were tested to separate POM from other soil phases: manual, global, and local thresholding methods. Reported algorithms were also compared with a supervised grey value-based (GV) approach followed by morphological operations. Results showed contrast agents increased α of POM, simplifying its identification and the following segmentation on dry cores. The POM was discriminated from the mineral fraction and its content correctly estimated. This was particularly accurate when applying manual thresholding or GV approach with respect to indicator kriging, suggesting that operator-based ability to set threshold level is still the best solution for accurate POM segmentation. Beyond single-phase accounting, different thresholding algorithms and morphological operations also affected POM morphological characteristics. In particular, the simpler was an object shape, the easier was its segmentation. Improvements are thus required to increase the efficiency of automated thresholding algorithms. Moreover, wet cores were exposed to washing-out phenomena that compromised any digital image processing and further POM quantification, implying that more effort should be made to find other suitable staining agents.


2020 ◽  
Vol 126 (4) ◽  
Author(s):  
C. Florian ◽  
R. Wonneberger ◽  
A. Undisz ◽  
S. V. Kirner ◽  
K. Wasmuth ◽  
...  

Abstract In this contribution, chemical, structural, and mechanical alterations in various types of femtosecond laser-generated surface structures, i.e., laser-induced periodic surface structures (LIPSS, ripples), Grooves, and Spikes on titanium alloy, are characterized by various surface analytical techniques, including X-ray diffraction and glow-discharge optical emission spectroscopy. The formation of oxide layers of the different laser-based structures inherently influences the friction and wear performance as demonstrated in oil-lubricated reciprocating sliding tribological tests (RSTTs) along with subsequent elemental mapping by energy-dispersive X-ray analysis. It is revealed that the fs-laser scan processing (790 nm, 30 fs, 1 kHz) of near-wavelength-sized LIPSS leads to the formation of a graded oxide layer extending a few hundreds of nanometers into depth, consisting mainly of amorphous oxides. Other superficial fs-laser-generated structures such as periodic Grooves and irregular Spikes produced at higher fluences and effective number of pulses per unit area present even thicker graded oxide layers that are also suitable for friction reduction and wear resistance. Ultimately, these femtosecond laser-induced nanostructured surface layers efficiently prevent a direct metal-to-metal contact in the RSTT and may act as an anchor layer for specific wear-reducing additives contained in the used engine oil.


2021 ◽  
Vol 11 (3) ◽  
pp. 1153
Author(s):  
Avishek Kumar Gupta ◽  
Matti Aula ◽  
Jouni Pihlasalo ◽  
Pasi Mäkelä ◽  
Marko Huttula ◽  
...  

A high titania slag that is used as a feedstock for TiO2 manufacturing is obtained by ilmenite smelting (FeO.TiO2). The composition of the slag obtained by smelting is dependent on the composition of the mineral used for slag preparation, i.e., ilmenite in our study. At the laboratory scale, ilmenite slags are mostly obtained by using ilmenite as the raw material. An easy and simple way would be to prepare the synthetic slag using the individual components and heating them to high temperature in a furnace. The titania slag has a high oxidizing nature and requires an inert atmosphere to prevent oxidation of the slag as well as the molybdenum crucible. This paper describes the preparation of synthetic ilmenite slag using an induction furnace and the study of the composition and the phases formed in the slag. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and inductively coupled plasma-optical emission spectroscopy (ICP-OES) were used as analytical techniques for studying the slag. A comparison between obtained synthetic slag and industrial ilmenite slag was performed to test the possibility of preparing slags in the laboratory as per the required composition. The slags show similar phase formation as obtained in industrial ilmenite slags, which means that the synthetic slags are identical to the industrial slags.


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


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