Semi-Quantitative X-Ray Diffraction Analysis of Fly Ash by the Reference Intensity Ratio Method

1988 ◽  
Vol 136 ◽  
Author(s):  
Gregory J. McCarthy ◽  
A. Thedchanamoorthy

ABSTRACTA protocol for relatively inexpensive and rapid semi-quantitative x-ray diffraction analysis of fly ash mineralogy by the Reference Intensity Ratio (RIR) method is described. RIR's for the common crystalline phases in fly ashes derived from low rank and bituminous coal are given. The method is semi-quantitative for some phases because of unavoidable overlaps of the stronger peaks suitable for quantitation. Use of the protocol is illustrated with the four fly ash Standard Reference Materials supplied by the National Institute of Standards and Technology. Recommendations for implementation of this protocol in other laboratories and for improvements in quantitation of fly ash mineralogy are given.

2000 ◽  
Vol 15 (3) ◽  
pp. 163-172 ◽  
Author(s):  
Ryan S. Winburn ◽  
Dean G. Grier ◽  
Gregory J. McCarthy ◽  
Renee B. Peterson

Rietveld quantitative X-ray diffraction analysis of the fly ash Standard Reference Materials (SRMs) issued by the National Institute of Standards and Technologies was performed. A rutile (TiO2) internal standard was used to enable quantitation of the glass content, which ranged from 65% to 78% by weight. TheGSASRietveld code was employed. Precision was obtained by performing six replicates of an analysis, and accuracy was estimated using mixtures of fly ash crystalline phases and an amorphous phase. The three low-calcium (ASTM Class F) fly ashes (SRM 1633b, 2689 and 2690) contained four crystalline phases: quartz, mullite, hematite, and magnetite. SRM 1633b also contained a detectable level of gypsum, which is not common for this type of fly ash. The high-calcium (ASTM Class C) fly ash, SRM 2691, had eleven crystalline phases and presented a challenge for the version ofGSASemployed, which permits refinement of only nine crystalline phases. A method of analyzing different groups of nine phases and averaging the results was developed, and tested satisfactorily with an eleven-phase simulated fly ash. The results were compared to reference intensity ratio method semiquantitative analyses reported for most of these SRMs a decade ago.


1987 ◽  
Vol 31 ◽  
pp. 331-342 ◽  
Author(s):  
G.J. McCarthy ◽  
D.M. Johansen ◽  
S.J. Steinwand ◽  
A. Thedchanamoorthy

AbstractMethods for, and results from, x-ray diffraction analysis of large numbers of fly ash samples obtained from U.S. power plants are described. Qualitative XRD indicates that low-calcium/Class F fly ash (usually derived from bituminous coal) consists typically of the crystalline phases quartz, mullite, hematite and magnetite in a matrix of aluminosilicate glass. Highcalcium fly ash (derived from low-rank coal) has a much more complex assemblage of crystalline phases that typically includes these four phases plus lime, periclase, anhydrite, alkali sulfates, tricalcium aluminate, dicalcium silicate, melilite, merwinlte and a sodalite-structure phase. Glass compositions among the particles are more heterogeneous and range from calcium aluminate to sodium calcium aluminosilicate, Every ash studied Is mixed with an internal Intensity standard (rutile) so that Intensity ratios can be used to make comparisons of the relative amounts of crystalline phases. An error analysis was performed to define the level of uncertainty in making these comparisons. These intensity ratios will be used for quantitative XRD phase analyses when reference intensity ratios for each fly ash phase become available.


2019 ◽  
Vol 49 (2) ◽  
pp. 20170609
Author(s):  
M. N. Ervina Efzan ◽  
N. Siti Syazwani ◽  
A. M. Mustafa Al Bakri ◽  
Wai Liew Kia

1996 ◽  
Vol 51 (5) ◽  
pp. 744-746 ◽  
Author(s):  
A. Franken ◽  
H. Thomsen ◽  
W. P reetz

By reaction of conjuncto-[B6H6-B6H6]2- in alkaline solution with excess bromine the heptabromo-closo-heptaborate, [B7Br7]2 is formed. The crystal structure of [(CsH3N)2CH2][B7Br7] has been determined by single crystal X-ray diffraction analysis (monoclinic, space group P21/a with a = 15.0843(14), b = 9.8882(14), c = 17.057(2) Å, β = 114.039°(7)). In accordance with the D5h point symmetry, the anion shows two singlets at -23.3 and -0.1 ppm with the intensity ratio 2:5 in its 11B NMR spectrum.


1990 ◽  
Vol 34 ◽  
pp. 387-394 ◽  
Author(s):  
G. J. McCarthy ◽  
J. K. Solem

AbstractA protocol for semi-quantitative XRD analysis of fly ash has been applied to 178 ashes in studies of the typical mineralogy of high-calcium and iow-calcium fly ash, the consistency of fly ash mineralogy from a typical power station, the partitioning of chemical constituents into crystalline phases, and the crystalline phases relevant to the use of fly ash in concrete.


1986 ◽  
Vol 86 ◽  
Author(s):  
G. J. McCarthy ◽  
O. E. Manz ◽  
D. M. Johansen ◽  
S. J. Steinwand ◽  
R. J. Stevenson

Fly ashes derived from low-rank coals mined principally in Montana, Wyoming and North Dakota are being studied by the Western Fly Ash Research, Development and Data Center [1]. Previous studies of the mineralogy of western U.S. fly ash by McCarthy et al. [1–3] using x-ray diffraction (XRD) form the framework of the present study. A database of chemical, mineralogical and physical properties, along with precursor coal characteristics, is being assembled. Based on studies to date of several hundred fly ash samples derived from lignite and subbituminous coals, as well as from several bituminous ashes, correlations of chemistry and mineralogy have been hypothesized and are being tested. These correlations are discussed below.


Sign in / Sign up

Export Citation Format

Share Document