SN/T 3011.1-2020X-ray diffraction method to identify the phases of imported solid wastes of metal minerals - Part 1: General rules (English PDF)
X射线衍射法鉴别金属矿产类进口固体废物物相 第1部分:通则
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Issued by
General Administration of Customs
Level / Type
National · Recommended
Issue date
August 27, 2020
Implementation date
March 1, 2021
Scope
SN/T 3011.1-2020 is the English-translated version of X射线衍射法鉴别金属矿产类进口固体废物物相 第1部分:通则.
SN/T 3011.1-2020 — This part of SN/T 3011 specifies the general rules for the identification of imported solid wastes of metal minerals by X-ray diffraction. This part is applicable to the phase identification of imported solid wastes of metal minerals by X-ray diffraction method.
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Document preview — SN/T 3011.1-2020
National Standard of the People's Republic of China
- ICS
- 77-010
- Classification
- H 10
- Replacing
- SN/T 3011.1-2011
Issued by: General Administration of Customs
Contents
- Foreword
- 1 Scope
- 2 Normative references
- 3 Terms and definitions
- 4 Method summary
- 5 Apparatus and equipment
- 6 Sampling and sample preparation
- 7 Sample test
- 7.1 Preparation of test pieces
- 7.2 Determination
- 7.3 Data analysis
- 8 Result analysis
Foreword
This part is the first part of the series of standards of SN/T 3011 "Identification of the Phases of Imported Solid Wastes of Metal Minerals by X-ray Diffraction Method".
This part was drafted in accordance with the rules given in GB/T 1.1-2009.
This part replaces SN/T 3011.1-2011 "Identification of Imported Solid Wastes of Metal Minerals by X-ray Diffraction Method Part 1: General then".
Compared with SN/T 3011.1-2011, the main technical changes in this part are as follows.
--Modified and added equipment;
--Added and improved the content of sampling and sample preparation;
--Improved the result analysis.
This part is proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organizations of this section. Shenzhen Customs of the People's Republic of China, Shenzhen Institute of Inspection and Quarantine, and People's Republic of China City Customs/Shenzhen Vocational and Technical College.
1 Scope
This part of SN/T 3011 specifies the general rules for the identification of imported solid wastes of metal minerals by X-ray diffraction.
This part is applicable to the phase identification of imported solid wastes of metal minerals by X-ray diffraction method.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB.2007.1 General Rules for Sampling and Sample Preparation of Bulk Mineral Products
3 Terms and definitions
The following terms and definitions apply to this document.
Loss of original use value or abandoned or abandoned although it has not lost the use value generated in production, life and other activities Solid, semi-solid, and gaseous articles and substances placed in containers, as well as articles that are included in solid waste management by laws and administrative regulations, substance.
Metal minerals
Through mining, beneficiation and smelting processes, one or more metal element or compound minerals can be extracted from it.
4 Method summary
The sample was tested with an X-ray diffractometer, and the interplanar spacing (d) and relative intensity (I) of the various diffraction peaks in the diffraction spectrum were compared with Compare the d value and I value of the standard minerals in the diffraction spectrum library to determine whether the sample contains a certain mineral or multiple minerals.
5 Apparatus and equipment
5.1 X-ray diffractometer. equipped with inorganic standard powder diffraction database and mineral standard powder diffraction database.
5.2 Grinding machine.
5.3 Agate mortar.
5.4 Standard sieve. 147 µm, 75 µm.
5.5 Blast drying oven. the temperature can reach 105 °C, and the temperature control accuracy is ±2 °C.
Solid wastes
6 Sampling and sample preparation
Sampling and sample preparation are carried out in accordance with the provisions of GB.2007.1.All samples shall pass through a 147 µm standard sieve (5.4) and be kept at 105 °C ±2 °C After drying for at least 2 hours, put it in a desiccator for later use.
7 Sample test
7.1 Preparation of test pieces
Place the sample in an agate mortar (5.3) and grind until all of it passes through a 75 µm standard sieve (5.4), and take an appropriate amount of analysis sample and load it evenly in the sample frame, use a glass sheet to compress and flatten the powder to a plane with the surface of the sample frame.
7.2 Determination
Place the sample piece on the sample table of the X-ray diffractometer (5.1), and use appropriate measurement conditions to collect the X-ray diffraction pattern of the sample.
Refer to the X-ray diffractometer measurement conditions in Appendix A.
7.3 Data analysis
Use the processing program configured with the X-ray diffractometer to analyze the X-ray diffraction pattern obtained in 7.2 to obtain the crystal plane of the sample Spacing (d) and relative diffraction intensity (I/I0). The relative deviation of d value measurement should be less than 1%.
Use Hanawalt qualitative phase analysis method or computer search qualitative phase analysis method to determine the phase composition of the sample. Hanawalt Qualitative refer to the figure B.1 in Appendix B for the determination procedure of the phase analysis method, and refer to the figure in Appendix B for the determination procedure of the computer retrieval qualitative phase analysis method B.2.
Note. Phase analysis generally needs to determine the elemental composition information of the sample in advance. The technical means to determine the elemental composition include X-ray fluorescence spectroscopy, inductance Coupled plasma emission spectroscopy, etc.
8 Result analysis
8.1 If the main phase of the sample is a certain metallic mineral phase (that is, the strongest diffraction peak in the diffraction pattern of the sample is the strongest diffraction of a certain metallic mineral phase) Line), or contains other metal minerals, or contains a small amount of gangue phase, then the sample is determined to be the metal mineral.
8.2 If the main phase of the sample is a certain metallic mineral phase (that is, the strongest diffraction peak in the diffraction pattern of the sample is the strongest diffraction of a certain metallic mineral phase) Line), the non-mineral phase containing the metal or other metals is determined to contain the mineral phase of the metal and the non-mineral phase containing the metal Phase, or non-mineral phase containing other metals.
8.3 If a certain metal mineral phase does not exist in the phase composition of the sample (that is, the strongest diffraction peak in the diffraction pattern of the sample is not a certain metal mineral phase) the strongest diffraction line), or the non-mineral phase containing other metals, it is determined that the sample is not the metal mineral, or the non-mineral containing other metals Physical phase.
Appendix A
(Informative appendix) X-ray diffractometer measurement conditions Due to the different instruments used, the optimal analysis conditions may also be different, so it is impossible to give the general parameters of the X-ray diffractometer.
The set parameters should ensure the effective collection of the X-ray diffraction pattern of the sample. The parameters given in Table A.1 have been proved to be feasible.
Note. In the measurement process, it is recommended to use an anti-air scatter shovel to remove the air scatter background in the diffraction pattern.
Appendix B
(Informative appendix) X-ray diffraction qualitative phase analysis method B.1 Hanawalt method the most classic method of phase analysis is the Hanawalt method. The principle is to select three diffraction lines with the highest intensity from the diffraction lines of a substance (with in order of decreasing intensity) and its corresponding crystal plane spacing, find the corresponding set of data in the index, and then obtain the JCPDS card Number, find out the JCPDS card, carefully compare and compare to determine whether it contains the substance. The qualitative phase analysis steps are shown in Figure B.1.
B.2 Computer retrieval qualitative phase analysis method with the increasing number of JCPDS cards, Hanawalt method identification takes a long time. At present, almost all X-ray diffractometers are compatible with the computer is online, which can realize computer automatic determination and automatic retrieval, but in the end, human judgment of the retrieval result is required. Computer search the steps of sexual phase analysis are shown in Figure B.2.
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