Quantitative Phase Analysis of Devonian Shales by Computer Controlled X-Ray Diffraction of Spray Dried Samples

Smith, Steven T.; Snyder, Robert L.; Brownell, Wayne Ernest

doi:10.1007/978-1-4613-9987-2_17

Cited by 10 publications

(6 citation statements)

References 3 publications

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“…Using as the criterion the departure of totals from 100%, our results compare favorably with the technique of Smith et al (1979), who used 00l clay reflections, spray drying and calculated p~* from the ma-jot element chemical analysis. Our sample preparation technique is better than spray drying (Hiller, 1999) if a sample changer is used, because it produces rigid specimens, resistant to mechanical deformation that can occur during loading.…”

Section: Conclusion and Further Perspectivesmentioning

confidence: 55%

“…The first ( Figure 2) compares diffraction data obtained from side-loaded preparations with those from splits of the same sample prepared by spray-freeze-drying. This technique is a variation (driving water off by sublimation instead of heating) of spray drying, which was shown to produce perfectly random orientation (Smith et al, 1979;Hillier, 1999). The second test tions of platy vs. isometric particles using different amounts of kaolinite and quartz.…”

Section: Sample Preparationmentioning

confidence: 99%

“…Orientation-related problems can be avoided by using a random preparation. Techniques for producing such preparations from clay-rich rocks have been described previously (Smith et al, 1979;Moore and Reynolds, 1997;Hillier, 1999 and references therein).…”

Section: Introductionmentioning

confidence: 99%

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Quantitative X-Ray Diffraction Analysis of Clay-Bearing Rocks From Random Preparations

Środoń¹

2001

Clays and clay miner.

415

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Abstract--An internal standard X-ray diffraction (XRD) analysis technique permits reproducible and accurate calculation of the mineral contents of rocks, including the major clay mineral families: Fe-rich chlorites + berthierine, Mg-rich chlorites, Fe-rich dioctahedral 2:1 clays and micas, Al-rich dioctahedral 2:1 clays and micas, and kaolinites. A single XRD pattern from an air-dried random specimen is used. Clays are quantified from their 060 reflections which are well resolved and insensitive to structural defects. Zincite is used as the internal standard instead of corundum, because its reflections are more conveniently located and stronger, allowing for a smaller amount of spike (10%). The grinding technique used produces powders free of grains coarser than 20 ixm and suitable for obtaining random and rigid specimens.Errors in accuracy are low, <2 wt. % deviation from actual values for individual minerals, as tested on artificial shale mixtures. No normalization is applied and thus, for natural rocks, the analysis is tested by the departure of the sum of the measured components from 100%. Our approach compares favorably with other quantitative analysis techniques, including a Rietveld-based technique.

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Section: Conclusion and Further Perspectivesmentioning

confidence: 55%

Section: Sample Preparationmentioning

confidence: 99%

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Quantitative X-Ray Diffraction Analysis of Clay-Bearing Rocks From Random Preparations

Środoń¹

2001

Clays and clay miner.

415

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“…In addition, line overlap may reduce the number of measurable lines, particularly with complex diffraction patterns. Typically, few reflections from each phase are used which limits the precision of the results and makes analyses more susceptible to the effects of primary extinction and preferred orientation (Chung, 1974a, b;Smith, Snyder & Brownell, 1979b;Goehner, 1982;Hubbard, Robbins & Snyder, 1983;Pawloski, 1985).…”

Section: Introductionmentioning

confidence: 99%

Quantitative phase analysis using the Rietveld method

Bish¹,

Howard²

1988

J Appl Crystallogr

916

516

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Quantitative phase analysis of multicomponent mixtures using X-ray powder diffraction data has been approached with a modified version of the Rietveld computer program of Wiles & Young [ J. Appl. Cryst. (1981), 14, 149-151]. This new method does not require measurement of calibration data nor the use of an internal standard; however, the approximate crystal structure of each phase of interest in a mixture is necessary. The use of an internal standard will allow the determination of total amorphous phase content in a mixture. Analysis of synthetic mixtures yielded high-precision results, with errors generally less than 1.0% absolute. Since this technique fits the complete diffraction pattern, it is less susceptible to primary extinction effects and minor amounts of preferred orientation. Additional benefits of this technique over traditional quantitative analysis methods include the determination of precise cell parameters and approximate chemical compositions, and the potential for the correction of preferred orientation and microabsorption effects.

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“…Quando pós com cristalitos de tamanhos da ordem de 10 μm não podem ser obtidos diretamente por peneiramento, podem ser usados métodos como sedimentação ou outros meios de fracionamento ou pode ainda ser usada moagem ou trituração, caso a microestrutura da amostra não seja de interesse. Entretanto, deve-se ter em mente que algumas substâncias podem sofrer mudanças de fase, quando submetidas a tratamentos mecânicos [19] . Na determinação ou refinamento de estruturas, a sobreposição dos perfis de linha pode, às vezes, ser diminuída e, consequentemente, melhorada a qualidade dos dados, através de tratamentos térmicos da amostra.…”

Section: -Preparação De Amostrasunclassified

Desenvolvimento de amostras padrão de referência para difratometria

Galvao¹

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Manifesto meus sinceros agradecimentos àqueles que colaboraram de alguma forma com a execução deste trabalho:Ao Dr. Luis Gallego Martinez pela oportunidade, orientação e paciência.Aos professores do programa que muito contribuíram para o meu crescimento técnico, científico e intelectual.Ao Dr. Hidetoshi Takiishi pela colaboração e incentivo.A Dra. Dolores R. R. Lazar pela atenção e gentileza. DEVELOPMENT OF STANDART REFERENCE SAMPLES FOR DIFFRACTOMETRY

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Quantitative Phase Analysis of Devonian Shales by Computer Controlled X-Ray Diffraction of Spray Dried Samples

Cited by 10 publications

References 3 publications

Quantitative X-Ray Diffraction Analysis of Clay-Bearing Rocks From Random Preparations

Quantitative X-Ray Diffraction Analysis of Clay-Bearing Rocks From Random Preparations

Quantitative phase analysis using the Rietveld method

Desenvolvimento de amostras padrão de referência para difratometria

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