Quality control in urinary stone analysis: results of 44 ring trials (1980–2001)

Author(s):  
Albrecht Hesse ◽  
Rolf Kruse ◽  
Wolf-Jochen Geilenkeuser ◽  
Matthias Schmidt

AbstractUrinary stone analysis is the most important diagnostic step after stone removal from the body. The methods employed for these analyses are based on diverse analytical principles. Chemical methods are used for detecting individual ions. Infrared spectroscopy is used for examining molecular structures, and X-ray diffraction for determination of the crystalline structure of a substance. Since 1980, a twice-yearly ring trials quality control survey has been on offer to examine the quality of urinary stone analyses. A summary of the results of 44 ring trials (1980–2001) has been compiled for individual pure substances and binary (two-component) mixtures. On average, 100 laboratories have participated in these ring trials. Initially, over 80% of the participants carried out their analyses using chemical methods. In 2001, this figure decreased to a mere 13%. In contrast, a progressive increase in the use of infrared spectroscopy was observed, up to 79% of all participants employed this method. X-Ray diffraction was only employed in a small number of specialised laboratories (5–9%). The chemical methods produced a very high proportion of errors (6.5–94%) with both the pure substances and binary mixtures, whereas high error rates for infrared spectroscopy and X-ray diffraction were confined to individual substances only. Due to the poor results in the ring trials, the majority of laboratories stopped using chemical analysis, which is now considered to be obsolete. Regarding mixtures, error rates of over 10% also occurred with infrared spectroscopy and X-ray diffraction. Ring trials are indispensable for the quality management of urinary stone analysis.

2005 ◽  
Vol 13 (2) ◽  
pp. 136-140 ◽  
Author(s):  
Marcio Baltazar Conz ◽  
José Mauro Granjeiro ◽  
Gloria de Almeida Soares

The aim of this work was to characterize six hydroxyapatites in granular form for applications in medicine and dentistry as bone graft and to compare with manufacturers' specification. These samples were produced by four different manufacturers, and all of them are easily available in the Brazilian market. Physicochemical characterization was carried out by using electron microscopy (SEM), X-ray diffraction (XRD), infrared spectroscopy (FTIR) and surface area (BET) measurements. The results show that just one hydroxyapatite sample exhibited characterisitics in perfect agreement with the manufacturers' specifications. The studied parameters, namely crystallinity, surface area and composition may be used to estimate hydroxyapatite's biodegradability and as a criterion for quality control.


Author(s):  
R. J. Narconis ◽  
G. L. Johnson

Analysis of the constituents of renal and biliary calculi may be of help in the management of patients with calculous disease. Several methods of analysis are available for identifying these constituents. Most common are chemical methods, optical crystallography, x-ray diffraction, and infrared spectroscopy. The application of a SEM with x-ray analysis capabilities should be considered as an additional alternative.A scanning electron microscope equipped with an x-ray “mapping” attachment offers an additional dimension in its ability to locate elemental constituents geographically, and thus, provide a clue in determination of possible metabolic etiology in calculus formation. The ability of this method to give an undisturbed view of adjacent layers of elements in their natural state is of advantage in determining the sequence of formation of subsequent layers of chemical constituents.


Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4723
Author(s):  
Sara Dalle Vacche ◽  
Vijayaletchumy Karunakaran ◽  
Alessia Patrucco ◽  
Marina Zoccola ◽  
Loreleï Douard ◽  
...  

Nanocellulose was extracted from short bast fibers, from hemp (Cannabis sativa L.) plants harvested at seed maturity, non-retted, and mechanically decorticated in a defibering apparatus, giving non-aligned fibers. A chemical pretreatment with NaOH and HCl allowed the removal of most of the non-cellulosic components of the fibers. No bleaching was performed. The chemically pretreated fibers were then refined in a beater and treated with a cellulase enzyme, followed by mechanical defibrillation in an ultrafine friction grinder. The fibers were characterized by microscopy, infrared spectroscopy, thermogravimetric analysis and X-ray diffraction after each step of the process to understand the evolution of their morphology and composition. The obtained nanocellulose suspension was composed of short nanofibrils with widths of 5–12 nm, stacks of nanofibrils with widths of 20–200 nm, and some larger fibers. The crystallinity index was found to increase from 74% for the raw fibers to 80% for the nanocellulose. The nanocellulose retained a yellowish color, indicating the presence of some residual lignin. The properties of the nanopaper prepared with the hemp nanocellulose were similar to those of nanopapers prepared with wood pulp-derived rod-like nanofibrils.


2013 ◽  
Vol 803 ◽  
pp. 80-84
Author(s):  
Yu Qi Liu ◽  
Yong Yang ◽  
Rui Yang ◽  
Xiao Jun Xu

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).


2021 ◽  
Author(s):  
Rahma Rahzelli Zrelli ◽  
Fathia Chehimi-Moumen ◽  
Dalila Ben Hassen-Chehimi ◽  
Malika Trabelsi-Ayadi

Abstract The synthesis of the diphosphate HYP2O7·3H2O was made via soft chemistry route from evaporation of aqueous solution at room temperature. The obtained compound, was characterized by means of X-ray diffraction (XRD) and infrared spectroscopy (IR). The results showed a high purity phase. IR spectrum of this diphosphate revealed usual signals related to P2O7 diphosphate group and water molecules. The thermal decomposition of the synthesized product by DTA / TG proceeded through four stages leading to the formation of the Y2P4O13 as a final product. On the other hand, its decomposition by CRTA took place in three stages leading to the formation of the anhydrous diphosphate HYP2O7 as a final product. X-ray powder diffraction and infrared spectroscopy were used to identify these materials. Furthermore the electrical properties of the HYP2O7 were investigated through impedance complex analysis. Modest conductivity has been observed in this material at relatively medium temperature range. Activation energy of 0.67 and 1.44 eV, was deduced from the corresponding Arrhenius plot.The optical band gap of the title compound is calculated and found to be 2.71 eV.


1973 ◽  
Vol 28 (9-10) ◽  
pp. 600-605 ◽  
Author(s):  
Karl-Friedrich Tebbe ◽  
Hans Georg Schnering ◽  
Barbara Rüter ◽  
Gisela Rabeneck

Besides ‘Li2Al’ which was recently shown to be the phase Li9Al4 there exists the phase Li3Al2 characterized by preparation and X-ray diffraction methods. It cristallizes with a rhomboedric unit cell, R3̄m, a = 4.508 Å, c = 14.26 Å and z = 3 formula units (hexagonal setting). The structure can be looked at as a variant of the body centred cubic packing with Αl-atom layers of puckered six membered rings. The structural relation of the phases LiAl, Li3Al2, Li9Al4, Li is discussed.


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