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SH/T 1827-2019: (Plastics. Determination of crystallinity. X-ray diffraction)
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| SH/T 1827-2019 | English | 279 |
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(Plastics. Determination of crystallinity. X-ray diffraction)
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SH/T 1827-2019
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Basic data | Standard ID | SH/T 1827-2019 (SH/T1827-2019) | | Description (Translated English) | (Plastics. Determination of crystallinity. X-ray diffraction) | | Sector / Industry | Petrochemical Industry Standard (Recommended) | | Classification of Chinese Standard | G31 | | Classification of International Standard | 83.080.01 | | Word Count Estimation | 12,171 | | Date of Issue | 2019-12-24 | | Date of Implementation | 2020-07-01 | | Issuing agency(ies) | Ministry of Industry and Information Technology | | Summary | This standard specifies a method for the determination of the crystallinity of polyethylene (PE) and polypropylene (PP) by X-ray diffraction. This standard is applicable to the determination of the crystallinity of granulated or powdered polyethylene and polypropylene (�� crystal form, ��+�� crystal form) compression or injection molding samples, but not applicable to the determination of the crystallinity of filled polyethylene and polypropylene. | SH/T 1827-2019: (Plastics. Determination of crystallinity. X-ray diffraction)---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Plastics.Determination of crystallinity.X-ray diffraction)
Petrochemical Industry Standards of the People's Republic of China
Determination of crystallinity of plastics by X-ray diffractometry
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009
This standard was proposed by China Petrochemical Corporation
This standard is under the jurisdiction of the Petrochemical Plastic Resin Products Branch of the National Plastics Standardization Technical Committee (SAC/TC15/SC1)
Responsible for drafting this standard. China National Petroleum Corporation Petrochemical Research Institute, Beijing Yanshan Petrochemical High-tech Technology Company
Limited liability company
Participated in the drafting of this standard. Tianjin University, Shanghai Jiaotong University, China Petroleum & Chemical Corporation Beijing Research Institute of Chemical Industry,
China Petroleum & Chemical Corporation Zhenhai Refining & Chemical Company, China National Petroleum Corporation Liaoyang Petrochemical Company, Bruker
(Beijing) Technology Co., Ltd., Thermo Fisher Scientific (China) Co., Ltd., Dandong Haoyuan Instrument Co., Ltd., Dandong Tongda Technology Co., Ltd.
Co., Ltd., Shanghai Ruoyi New Material Technology Co., Ltd.
The main drafters of this standard. Li Ruifeng, Zheng Huiqin, Wang Zhengyuan, Wang Weizhong, Wu Yanjin, Zhang Lijun, Ren Minqiao, Jin Wenren, Ju
Wei Cai, Wang Tong, Du Haiyan, Jiang Chuanhai, Meng Hongcheng, Shi Hongbo, Zhong Zhe, Wei Liming
This standard is issued for the first time
Determination of crystallinity of plastics by X-ray diffractometry
Warning. The personnel using this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues.
The user has the responsibility to take appropriate safety and health measures and to ensure compliance with the conditions stipulated by relevant national laws and regulations
1 Scope
This standard specifies the method for determining the crystallinity of polyethylene (PE) and polypropylene (PP) by X-ray diffraction
This standard is applicable to the determination of crystallinity of granular or powdered polyethylene and polypropylene (α crystal form, β＋α crystal form) compression-molded or injection-molded specimens
This standard does not apply to the determination of the crystallinity of filled polyethylene and polypropylene
Note. The determination of the crystallinity of polyethylene and polypropylene products can refer to this standard. The high ethylene content ethylene-propylene copolymer polypropylene can also refer to this standard.
2 Normative references
The following documents are indispensable for the application of this document. All dated reference documents only the dated version applies to this article
The latest version (including all amendments) of undated reference documents is applicable to this document
GB/T 1845.2 Plastic Polyethylene (PE) Molding and Extrusion Materials Part 2.Sample Preparation and Performance Determination
GB/T 2546.2 Plastic polypropylene (PP) Moulding and extrusion materials Part 2.Sample preparation and performance measurement
GB/T 2918 Standard environment for condition adjustment and testing of plastic samples
JJG 629-2014 Polycrystalline X-ray Diffractometer
3 Terms and definitions
The following terms and definitions apply to this document
3.1
Crystallinity (X-ray diffraction method)
The degree of crystallinity calculated based on the percentage of the contribution of the crystal region in the total area of the X-ray diffraction intensity peaks of the partially crystalline polymer[1]Xc
4 Method summary
The crystallinity of the polymer is proportional to the integrated area of the X-ray diffraction peaks of the crystalline phase. Collect 2θ at an angle of 5° under the specified test conditions.
The copper Kα X-ray diffraction data of the sample within the range of 35° is obtained by using the chemometric peak analysis software to obtain the measured crystal plane diffraction peak and amorphous scattering
The peak 2θ angle and peak area count value are calculated by the ratio of the sum of the peak area of the crystalline peak and the sum of the sum of the peak area of the amorphous peak.
Kind of crystallinity
5 Reference materials
Powder α-SiO2 or Si standard material that meets the technical requirements of JJG 629-2014
6 Equipment
6.1 X-ray diffractometer
The X-ray diffractometer that meets the technical requirements of JJG 629-2014 is equipped with a copper target (Kα radiation). The rotating sample stage instrument is as per JJG
The stability of the diffraction intensity measured in 629-2014 for 8 hours is not more than 1.5% (expressed as relative range)
Note. If the instrument's optical system configuration or adjustment is improper, the scattered light will enter the detector at a low angle and a bun peak will appear on the background, and the instrument cannot be completed.
Determination of crystallinity
6.2 Software
X-ray diffraction data processing software with Pearson Ⅶ peak splitting program
7 samples
7.1 Sample preparation
7.1.1 Preparation of PE sample
Use compression molding (Q) or injection molding (M) methods to prepare specimens according to GB/T 1845.The specimen thickness is 1.0mm ± 0.1mm
7.1.2 Preparation of PP sample
Use compression molding (Q) or injection molding (M) methods to prepare specimens according to GB/T 2546.The specimen thickness is 1.0 mm ± 0.1 mm
7.2 Sampling
Use punching equipment or ruler and blade to cut a test piece in the middle of the sample prepared by compression molding (Q) or injection molding (M) method. The test piece is required.
Flat as a mirror surface without bending The test surface is clean and free from dust and other mechanical impurities and kept dry. The size of the test piece is as specified by the instrument used.
Note. When sampling from the product, machine processing or other suitable methods can be used to prepare a slice of 1.0mm ± 0.1mm from the product and then sample according to the above method
8 Condition adjustment
According to GB/T 2918, the state is adjusted at a temperature of 23°C ± 2°C. The state adjustment time is in accordance with GB/T
1845.2 and GB/T 2546.2.
9 Test procedure
9.1 Test conditions
Test according to GB/T 2918 at a temperature of 23℃±2℃
9.2 Calibration instrument
Start the X-ray diffractometer (6.1) and use the standard material (5) to verify that the diffraction intensity of the instrument is not greater than the stability of the instrument
1.5%/8 hours (expressed in relative range)
9.3 Set the working conditions of the instrument
Set the working conditions of X-ray diffractometer (see Table 1)
9.4 Test
Do two tests in parallel, install the debugging film on the X-ray diffractometer sample table, close the sample room and start the test
10 Test data processing
10.1 Get the 2θ value of the peak position and the count value of the peak area
Use the data processing software configured with the X-ray diffractometer to first perform the Save-Golay 9 points or the X-ray diffraction data of the sample.
11-point parabolic smooth stripping Kα2 subtracts the background (B.G.), and then uses the Pearson-Ⅶ peak splitting program to perform peak shape fitting.
The peak shape of the radiation curve is divided into the crystal diffraction peak and the amorphous scattering peak to obtain the 2θ value of the peak position of the crystal diffraction peak and the amorphous scattering peak of the tested sample.
Amorphous scattering peaks and symmetrical crystal diffraction peaks should be symmetrically fitted to the peak area count value. If the measured crystal diffraction peaks are asymmetric
The asymmetric fitting is performed according to its peak shape
Note 1.The 2θ value of the peak position of the amorphous scattering peak in the literature is not uniform, and there is an unreasonable phenomenon in some literature that the asymmetrical splitting of the amorphous scattering peak
Note 2.For the typical stoichiometry of PE and PP (α crystal form, β＋α crystal form) (Pearson-Ⅶ), see Appendix A for the peak shape fitting diagram
10.2 Calculation
Calculate the crystallinity of the tested sample according to formula (1). Appendix B is the factor in formula (1) and the calculation method of the coefficient in the calculated formula.
10.3 Presentation of results
Take the arithmetic average of the two parallel determination results as the determination result data and keep one decimal place
11 Precision
In.2018, X-ray diffraction method was carried out to determine the crystallinity of 3 typical PE and 4 typical PP compression molded samples in 8 laboratories.
The precision test of each laboratory repeats the measurement for each sample twice. The precision calculation results are shown in Table 2.
Note 1.The precision of this standard is calculated according to GB/T 6379.2-2004[2], where Sr is the repeatability standard deviation, and SR is the reproducibility standard deviation and r is the repeatability.
Limit R is the limit of reproducibility
Note 2.The samples for the precision test are selected from samples with a crystallinity of 37.8% to 81.2%
The test report should include the following.
a) Indicate the reference to this standard.
b) All data and information of the test sample.
c) The working conditions of the instrument.
d) Details of sample preparation, sampling and sample state adjustment, test conditions, etc.
e) Sample size,
f) The test results include the two test results and the arithmetic mean value.
g) Details of any abnormal phenomena observed in the measurement and their descriptions, such as unqualified background, inconsistent crystal form of the sample, etc.
h) Date of analysis, etc.
Appendix A
(Informative appendix)
PE and PP (α crystal form, β＋α crystal form) typical stoichiometry (Pearson-Ⅶ) peak shape fitting graph
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