Quantitative XRD Analysis of Advanced Coal Combustion Solid Residuals by the RIR Method

AbstractReference intensity ratios (RIRs) with zincite (ZnO) as the internal standard have been measured and calculated for key phases in coal combustion solid residuals. Detailed comparisons of measured and calculated corundum RIRs (converted from zincite RIRs), and literature I/Ic values led to the conclusion that for best results, laboratory measured values must be used. Using measured zincite RIRs and standard mixtures of important crystalline phases, a protocol for routine semi-quantitative analysis has been developed. The need to grind under ethanol to minimize decomposition of hydrated phases was demonstrated. An unusual procedure employing mixed peak and integrated intensities in the RIR of one key phase, ettringite (Ca6Al2(SO4)3(OH)12-26H2O), has been adopted for this protocol.

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Semi-Quantitative XRD Analysis of Fly Ash Using Rutile as an Internal Standard

Advances in X-ray Analysis ◽

10.1154/s0376030800020929 ◽

1988 ◽

Vol 32 ◽

pp. 569-576 ◽

Cited By ~ 1

Author(s):

A. Thedchanamoorthy ◽

G.J. McCarthy

Keyword(s):

Fly Ash ◽

Error Analysis ◽

North American ◽

Intensity Ratio ◽

Limit Of Detection ◽

Internal Standard ◽

Xrd Analysis ◽

X Rays ◽

Fly Ashes ◽

Crystalline Phases

AbstractXRD analysis of fly ash was quantitated using the Reference Intensity Ratio (RIR) method and rutile (TiO2) as an internal standard. Rutile RIR's for 15 of the crystalline phases commonly observed in North American fly ash were determined. Error analysis on the various steps in quantitation indicated that precision ranged from ±10% of the amount present for phases that diffract x-rays strongly to ±21% for weakly diffracting phases. Limit of detection in the mostly glassy fly ashes ranged from 0.2% for lime, the most strongly diffracting phase, to 3.5% for weakly diffracting mullite. Accuracy evaluated with a simulated fly ash was within the limits established by precision, but in actual fly ash samples, accuracy will be a function of the match between the crystallinity and composition of the analyte and the analyte standard. Overlaps among peaks of some of the important phases require intensity proportioning; for this reason, the method is best described as semi-quantitative.

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Quantitative XRD Analysis of Advanced Coal Combustion Solid Residuals by the RIR Method

Advances in X-Ray Analysis ◽

10.1007/978-1-4615-2972-9_40 ◽

1993 ◽

pp. 343-353 ◽

Cited By ~ 1

Author(s):

J. A. Bender ◽

J. K. Solem ◽

G. J. McCarthy ◽

M. C. Oseto ◽

J. E. Knell

Keyword(s):

Coal Combustion ◽

Xrd Analysis ◽

Solid Residuals

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Quantitative X-ray diffraction analysis of urinary calculi by use of the internal-standard method and reference intensity ratios.

Clinical Chemistry ◽

10.1093/clinchem/34.2.281 ◽

1988 ◽

Vol 34 (2) ◽

pp. 289-293 ◽

Cited By ~ 6

Author(s):

M A Wandt ◽

A L Rodgers

Keyword(s):

Standard Method ◽

Urinary Calculi ◽

Internal Standard ◽

Xrd Analysis ◽

Internal Standard Method ◽

X Ray Diffraction ◽

Stone Composition ◽

X Ray ◽

Intensity Ratios

Abstract The internal-standard method and the powder diffractometer have been applied here to the quantitative determination of urinary stone constituents by x-ray diffraction (XRD). Reference intensity ratios determined for six stone substances were used in the reduction of intensity data. Constituent concentrations calculated for 21 stones were compared with values obtained from an element-sensitive technique. We conclude that XRD analysis alone cannot be regarded as a routine technique for the quantitative characterization of uroliths, but that semiquantitative XRD analysis supplemented by accurate quantitative elemental data is more suitable for the precise determination of true stone composition.

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Exploitation of HPLC Analytical Method for Simultaneous Determination of Six Principal Unsaturated Fatty Acids in Oviductus Ranae Based on Quantitative Analysis of Multi-Components by Single-Marker (QAMS)

Molecules ◽

10.3390/molecules26020479 ◽

2021 ◽

Vol 26 (2) ◽

pp. 479

Author(s):

Shihan Wang ◽

Yuanshuai Gan ◽

Hong Kan ◽

Xinxin Mao ◽

Yongsheng Wang

Keyword(s):

Fatty Acids ◽

Quantitative Analysis ◽

Unsaturated Fatty Acids ◽

Internal Standard ◽

Active Components ◽

Reliable Determination ◽

External Standard Method ◽

Single Marker ◽

Oviductus Ranae

As one of the featured products in northeast China, Oviductus Ranae has been widely used as a nutritious food, which contains a variety of bioactive unsaturated fatty acids (UFAs). It is necessary to establish a scientific and reliable determination method of UFA contents in Oviductus Ranae. In this work, six principal UFAs in Oviductus Ranae, namely eicosapentaenoic acid (EPA), linolenic acid (ALA), docosahexaenoic acid (DHA), arachidonic acid (ARA), linoleic acid (LA) and oleic acid (OA), were identified using UPLC-MS/MS. The UFAs identified in Oviductus Ranae were further separated based on the optimized RP-HPLC conditions. Quantitative analysis of multi-components by single-marker (QAMS) method was implemented in content determination of EPA, ALA, DHA, ARA and OA, where LA was used as the internal standard. The experiments based on Taguchi design verified the robustness of the QAMS method on different HPLC instruments and chromatographic columns. The QAMS and external standard method (ESM) were used to calculate the UFA content of 15 batches of Oviductus Ranae samples from different regions. The relative error (r < 0.73%) and cosine coefficient showed that the two methods obtained similar contents, and the method validations met the requirements. The results showed that QAMS can comprehensively and effectively control the quality of UFAs in Oviductus Ranae which provides new ideas and solutions for studying the active components in Oviductus Ranae.

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Crystallization of simonkolleite (Zn5Cl2(OH)8 ∙ H2O) in powder samples prepared for mineral composition analysis by quantitative X-ray diffraction (QXRD)

Nafta-Gaz ◽

10.18668/ng.2021.05.02 ◽

2021 ◽

Vol 77 (5) ◽

pp. 293-298

Author(s):

Urszula Zagórska ◽

◽

Sylwia Kowalska ◽

Keyword(s):

Quantitative Analysis ◽

Internal Standard ◽

Mineralogical Composition ◽

Hydrocarbon Exploration ◽

Composition Analysis ◽

Internal Standard Method ◽

X Ray Diffraction ◽

Method Error ◽

X Ray ◽

Significant Difference

The analysis of mineralogical composition by quantitative X-ray diffraction (QXRD) is one of the standard research methods used in hydrocarbon exploration. In order to improve it and to obtain better results, the methodology of quantitative analysis used at Well Logging Department is being periodically (more or less) modified. After the introduction of the improvements, comparative analyses were performed on archival samples. Reflections from an unidentified phase which did not occur in the tested Rotliegend sandstone samples were noticed on X-ray diffractograms of archival samples. Reflections of a mineral called simonkolleite were identified in the X-ray diffraction database. Chemically it is a hydrated zinc chloride of the formula: Zn5Cl2(OH)8 × H2O. Analysis of the composition of samples in which simonkolleite crystallised, indicated that the mineral is being formed in the result of the slow reaction of zinc oxide with halite (NaCl) and water vapour. An attempt was made to determine the influence of the presence of this mineral on the results of the quantitative analysis of mineralogical composition. The above methodology was applied on a group of ten samples. The results of the quantitative analysis conducted for archival samples stored with added zincite standard containing simonkolleite and for new, freshly grinded (without artifact) samples were compared. The comparison of the obtained results showed a slight influence of this mineral on the quantitative composition of the remaining components. The difference between the results usually did not exceed the method error. At the same time a significant difference in the calculated content of the internal standard was noted – on average 1% less in archival than in new samples. This shows that the reaction occurring in the archival samples will affect the evaluation of the quality of the obtained quantitative analysis, at the same time excluding the possibility of determining the rock’s amorphous substance content with the internal standard method.

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Sintering of alumina ceramics reinforced with a bioactive glass of 3CaO.P2O5-SiO2-MgO system

Cerâmica ◽

10.1590/0366-69132015613581887 ◽

2015 ◽

Vol 61 (358) ◽

pp. 160-167 ◽

Cited By ~ 1

Author(s):

A. W. Huang ◽

C. Santos ◽

R. O. Magnago ◽

R. F. F. Silva ◽

K. Strecker ◽

...

Keyword(s):

Fracture Toughness ◽

Relative Density ◽

Transient Liquid Phase ◽

Xrd Analysis ◽

Alumina Ceramics ◽

Crystalline Phases ◽

Powder Mixtures ◽

Solid State Sintering ◽

Sintering Condition

Alumina-based ceramics, Al2O3, exhibit a combination of properties which favor its use as biomaterial, specifically as structural dental prosthesis. Its most important properties as biomaterial are its elevated hardness, chemical stability and biocompatibility. Usually, Al2O3 is processed by solid-state sintering at a temperature of about 1600 oC, but it is very difficult to eliminate the porosity due to its diffusional characteristics. The objective of this work was the development and characterization of sintered Al2O3 ceramics, densified with a transient liquid phase formed by a bioactive 3CaO.P2O5-SiO2-MgO glass. Powder mixtures of 90 wt.% Al2O3 and 10 wt.% bioglass were milled, compacted and sintered at 1200 oC to 1450 oC. Comparatively, monolithic Al2O3 samples were sintered at 1600 oC/120 min. The sintered specimens were characterized by relative density, crystalline phases, microstructure and mechanical properties. The results indicate that the specimen sintered at 1450 oC/120 min present the best properties. Under this sintering condition, a relative density of 95% was reached, besides hardness higher than 9 GPa and fracture toughness of 6.2 MPa.m1/2. XRD analysis indicate alumina (αAl2O3), whitlockite (3CaO.P2O5) and diopsite [3(Ca,Mg)O.P2O5], as crystalline phases. Comparatively, monolithic sintered Al2O3 samples presented 92% of relative density with 17.4 GPa and 3.8 MPa.m1/2 of hardness and fracture toughness respectively.

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