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YB/T 5320-2006: Metal materials - Quantitative phase analysis - Value K method of X-ray diffraction Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
YB/T 5320-2006: Metal materials - Quantitative phase analysis - Value K method of X-ray diffraction---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/YBT5320-2006 YB FERROUS METALLURGY INDUSTRY STANDARD (Adjusted from GB/T 5225-1985) Metal materials - Quantitative phase analysis - "Value K" method of X-ray diffraction Issued on. JULY 27, 2006 Implemented on. OCTOBER 11, 2006 Issued by. National Development and Reform Commission of PRC Table of Contents1 Principles... 3 2 Requirements and preparation of specimens... 4 3 Test instruments and test conditions... 6 4 Test procedure and result calculation... 7 Appendix A (Supplementary)... 9 Appendix B (Supplementary)... 12 Additional information... 14 Metal materials - Quantitative phase analysis - "Value K" method of X-ray diffraction This standard applies to the measurement of phase content in polycrystalline powders of metallic materials. It can also be used as a reference for quantitative phase analysis of polycrystalline powder specimens of other materials.1 PrinciplesThe X-ray diffraction pattern of a phase is a characterization of the crystal structure of the phase. When using the K value method to perform X-ray diffraction quantitative analysis on a multiphase specimen, the cumulative intensity of a phase’s diffraction line AND the content of the phase in the specimen have the relationship of formulas (1) and (2) (see Appendix A for derivation). Where. Xa - The weight content of the α phase in the powder to be tested; - The constant of proportionality. For the same radiation, the constant is related to the αphase to be tested AND the reference substance; Ia(hikili) - The cumulative intensity of diffraction lines of α phase on the (hikili) crystal plane, after adding the reference substance to the powder to be tested; Ir(hjkjlj) - The cumulative intensity of diffraction lines of the reference material on the crystal plane (hjkjlj), after adding the reference substance to the powder to be tested; (hikili) - The cumulative intensity of diffraction lines of the α phase on the crystal plane (hikili), in the reference specimen; (hjkjlj) - The cumulative intensity of diffraction lines of the reference material from the crystal plane (hjkjlj), in the reference specimen; Wr - The weight of the reference substance, after adding the powder to be tested into the reference substance; Wo - The weight of the powder to be tested, when adding the powder to be tested into the reference substance; - The weight of the reference substance, in the reference specimen; - The weight of the powder to be tested, in the reference specimen. The characteristic of this method is to calculate the first AND finally determine the Xa. Note. The reference specimen refers to the specimen, which is prepared when the value is calculated.2 Requirements and preparation of specimens2.1 Sampling 2.1.1 Weighing When weighing the sample, the relative deviation of the weight shall not exceed 0.1%. 2.1.2 Reference materials and reference specimens 2.1.2.1 Selection of reference materials The principles for selecting reference materials are. 2.1.2.2 The linear absorption coefficient and particle radius of the reference material and the phase to be measured shall satisfy the formula (3). 2.1.2.3 When calculating the value, the recommended ratio of the reference specimen, which is formed by mixing the pure reference material and the pure phase to be measured, is as follows. When the cumulative intensity of the measured diffraction lines of the reference material and the phase to be measured differ greatly, it shall change the ratio, to increase the cumulative intensity of the weak diffraction lines. 2.1.4 Mixing of sample Use an agate mortar to grind the powders, which are prepared in 2.1.2.3 and 2.1.2.4, for 30 ~ 40 minutes; mix well. 2.2 Preparation of specimens 2.2.1 Size and thickness of reference specimen and mixed specimen In any selected diffraction position, the X-ray's irradiation area shall not exceed the surface area of the specimen. The thickness of the specimen shall satisfy formula (4). 2.2.2 Sample preparation 2.2.2.1 Use a commonly used specimen frame. Place a piece of about No.300 metallographic sandpaper, which is larger than the frame, under the frame (corresponding rough ground glass can also be used). 2.2.2.2 Pour the ground mixed powder into the specimen frame. Compact vertically to shape it. 2.2.2.3 Turn the pressed specimen over at an angle of 180°. Remove the sandpaper. Use the surface of the specimen, which is in contact with the sandpaper (or ground glass), as the test surface.3 Test instruments and test conditions3.1 Diffractometer The overall stability of the diffractometer1 is better than 1%. 3.2 Test conditions 3.3 Requirements for diffraction peak shape The peak height shall be 4 times larger than the fluctuation range of the background; The peak height should be about 4 times the half-height width.4 Test procedure and result calculationBefore the quantitative determination, the intensity of the diffraction lines of the reference specimen and the mixed specimen shall first be calibrated with the JCPDS standard card, to check whether the reference material and the phase to be measured have a preferred orientation. 4.1 Determination of value of reference specimen 4.1.1 To calculate the pure phase to be measured of the value, it shall first carry out qualitative analysis of the X-ray diffraction line, to check the purity; there shall be no impurity diffraction lines. 4.1.2 For the pure reference material selected according to 2.1.2, it shall check its purity according to 4.1.1. 4.1.7 Calculate value according to formula (2). 4.2 Determination of the content of the phase to be measured 4.2.1 According to 2.1.2.4, add a reference substance to the powder to be tested. Prepare the sample according to 2.2.2, so that the selected diffraction lines of the measured phase conform to 3.3. 4.2.2 According to 4.1.6, record the cumulative intensity of each corresponding diffraction line. 4.3 If the above requirements are met, the relative deviation of Xa is ≤ 5%.Appendix A(Supplementary) A.1 Derivation of formula (1) in this standard The cumulative intensity of powder diffraction lines can be expressed as.Appendix B(Supplementary) B.1 If the preferred orientation is not serious, the following formula can be used to correct the cumulative intensity of the diffraction line. YB/T 5320-2006 YB FERROUS METALLURGY INDUSTRY STANDARD (Adjusted from GB/T 5225-1985) Metal materials - Quantitative phase analysis - "Value K" method of X-ray diffraction Issued on. JULY 27, 2006 Implemented on. OCTOBER 11, 2006 Issued by. National Development and Reform Commission of PRCTable of Contents1 Principles... 3 2 Requirements and preparation of specimens... 4 3 Test instruments and test conditions... 6 4 Test procedure and result calculation... 7 Appendix A (Supplementary)... 9 Appendix B (Supplementary)... 12 Additional information... 14 Metal materials - Quantitative phase analysis - "Value K" method of X-ray diffraction This standard applies to the measurement of phase content in polycrystalline powders of metallic materials. It can also be used as a reference for quantitative phase analysis of polycrystalline powder specimens of other materials.1 PrinciplesThe X-ray diffraction pattern of a phase is a characterization of the crystal structure of the phase. When using the K value method to perform X-ray diffraction quantitative analysis on a multiphase specimen, the cumulative intensity of a phase’s diffraction line AND the content of the phase in the specimen have the relationship of formulas (1) and (2) (see Appendix A for derivation). Where. Xa - The weight content of the α phase in the powder to be tested; - The constant of proportionality. For the same radiation, the constant is related to the αphase to be tested AND the reference substance; Ia(hikili) - The cumulative intensity of diffraction lines of α phase on the (hikili) crystal plane, after adding the reference substance to the powder to be tested; Ir(hjkjlj) - The cumulative intensity of diffraction lines of the reference material on the crystal plane (hjkjlj), after adding the reference substance to the powder to be tested; (hikili) - The cumulative intensity of diffraction lines of the α phase on the crystal plane (hikili), in the reference specimen; (hjkjlj) - The cumulative intensity of diffraction lines of the reference material from the crystal plane (hjkjlj), in the reference specimen; Wr - The weight of the reference substance, after adding the powder to be tested into the reference substance; Wo - The weight of the powder to be tested, when adding the powder to be tested into the reference substance; - The weight of the reference substance, in the reference specimen; - The weight of the powder to be tested, in the reference specimen. The characteristic of this method is to calculate the first AND finally determine the Xa. Note. The reference specimen refers to the specimen, which is prepared when the value is calculated.2 Requirements and preparation of specimens2.1 Sampling 2.1.1 Weighing When weighing the sample, the relative deviation of the weight shall not exceed 0.1%. 2.1.2 Reference materials and reference specimens 2.1.2.1 Selection of reference materials The principles for selecting reference materials are. 2.1.2.2 The linear absorption coefficient and particle radius of the reference material and the phase to be measured shall satisfy the formula (3). 2.1.2.3 When calculating the value, the recommended ratio of the reference specimen, which is formed by mixing the pure reference material and the pure phase to be measured, is as follows. When the cumulative intensity of the measured diffraction lines of the reference material and the phase to be measured differ greatly, it shall change the ratio, to increase the cumulative intensity of the weak diffraction lines. 2.1.4 Mixing of sample Use an agate mortar to grind the powders, which are prepared in 2.1.2.3 and 2.1.2.4, for 30 ~ 40 minutes; mix well. 2.2 Preparation of specimens 2.2.1 Size and thickness of reference specimen and mixed specimen In any selected diffraction position, the X-ray's irradiation area shall not exceed the surface area of the specimen. The thickness of the specimen shall satisfy formula (4). 2.2.2 Sample preparation 2.2.2.1 Use a commonly used specimen frame. Place a piece of about No.300 metallographic sandpaper, which is larger than the frame, under the frame (corresponding rough ground glass can also be used). 2.2.2.2 Pour the ground mixed powder into the specimen frame. Compact vertically to shape it. 2.2.2.3 Turn the pressed specimen over at an angle of 180°. Remove the sandpaper. Use the surface of the specimen, which is in contact with the sandpaper (or ground glass), as the test surface.3 Test instruments and test conditions3.1 Diffractometer The overall stability of the diffractometer1 is better than 1%. 3.2 Test conditions 3.3 Requirements for diffraction peak shape The peak height shall be 4 times larger than the fluctuation range of the background; The peak height should be about 4 times the half-height width.4 Test procedure and result calculationBefore the quantitative determination, the intensity of the diffraction lines of the reference specimen and the mixed specimen shall first be calibrated with the JCPDS standard card, to check whether the reference material and the phase to be measured have a preferred orientation. 4.1 Determination of value of reference specimen 4.1.1 To calculate the pure phase to be measured of the value, it shall first carry out qualitative analysis of the X-ray diffraction line, to check the purity; there shall be no impurity diffraction lines. 4.1.2 For the pure reference material selected according to 2.1.2, it shall check its purity according to 4.1.1. 4.1.7 Calculate value according to formula (2). 4.2 Determination of the content of the phase to be measured 4.2.1 According to 2.1.2.4, add a reference substance to the powder to be tested. Prepare the sample according to 2.2.2, so that the selected diffraction lines of the measured phase conform to 3.3. 4.2.2 According to 4.1.6, record the cumulative intensity of each corresponding diffraction line. 4.3 If the above requirements are met, the relative deviation of Xa is ≤ 5%.Appendix A(Supplementary) A.1 Derivation of formula (1) in this standard The cumulative intensity of powder diffraction lines can be expressed as.Appendix B(Supplementary) B.1 If the preferred orientation is not serious, the following formula can be used to correct the cumulative intensity of the diffraction line. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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