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SH/T 1826-2019: (Plastics-Determination of melting enthalpy and crystallinity and melting temperature of ultra-high molecular weight polyethylene (PE-UHMW) materials and products Differential scanning calorimetry (DSC))
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(Plastics-Determination of melting enthalpy and crystallinity and melting temperature of ultra-high molecular weight polyethylene (PE-UHMW) materials and products Differential scanning calorimetry (DSC))
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SH/T 1826-2019
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Basic data | Standard ID | SH/T 1826-2019 (SH/T1826-2019) | | Description (Translated English) | (Plastics-Determination of melting enthalpy and crystallinity and melting temperature of ultra-high molecular weight polyethylene (PE-UHMW) materials and products Differential scanning calorimetry (DSC)) | | Sector / Industry | Petrochemical Industry Standard (Recommended) | | Classification of Chinese Standard | G31 | | Classification of International Standard | 83.080.20 | | Word Count Estimation | 10,128 | | 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 the test methods for the determination of melting enthalpy and melting temperature of ultra-high molecular weight polyethylene (PE-UHMW) materials and products by differential scanning calorimetry (DSC), and the calculation method for crystallinity. This standard applies to powders, molded materials, finished or used PE-UHMW, as well as irradiated or chemically cross-linked PE-UHMW. | SH/T 1826-2019: (Plastics-Determination of melting enthalpy and crystallinity and melting temperature of ultra-high molecular weight polyethylene (PE-UHMW) materials and products Differential scanning calorimetry (DSC))
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Plastics-Determination of melting enthalpy and crystallinity and melting temperature of ultra-high molecular weight polyethylene (PE-UHMW)
materials and products Differential scanning calorimetry (DSC)
Petrochemical Industry Standards of the People's Republic of China
SH/T 1826-2019
Plastic ultra-high molecular weight polyethylene (PE-UHMW)
Material and product melting enthalpy and crystallinity and melting
Determination of temperature Differential scanning calorimetry (DSC)
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).
The organization responsible for drafting this standard. Beijing Yanshan Petrochemical High-Tech Technology Co., Ltd.
Participated in the drafting of this standard. Shanghai Research Institute of Chemical Industry Co., Ltd., China Petroleum & Chemical Corporation Qilu Branch Research Institute,
China National Petroleum Corporation Liaoyang Petrochemical Company, Waters Technology (Shanghai) Co., Ltd.
The main drafters of this standard. Zheng Huiqin, Ye Chunlin, Li Zhenhuan, Hou Bin, Shi Hongbo, Huang Heliu, Shen Xianting, Yang Shengying, Duan
slight.
This standard is issued for the first time.
SH/T 1826-2019
Plastic ultra-high molecular weight polyethylene (PE-UHMW) materials and products melting enthalpy and
Determination of crystallinity and melting temperature Differential scanning calorimetry (DSC)
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 is responsible for taking appropriate safety and health measures. And to ensure that it meets the requirements of the relevant national laws and regulations.
1 Scope
This standard specifies the Differential Scanning Calorimetry (DSC) method for the determination of the enthalpy of fusion of ultra-high molecular weight polyethylene (PE-UHMW) materials and products,
Test method for melting temperature. And the calculation method of crystallinity.
This standard applies to powders, molded materials, finished products or used PE-UHMW. Also suitable for irradiated or chemically cross-linked
PE-UHMW.
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
Pieces. All undated reference documents. The latest version (including all amendments) is applicable to this document.
GB/T 2035 Plastic Terms and Definitions
GB/T 19466.1-2004 Plastic Differential Scanning Calorimetry (DSC) Part 1.General
GB/T 19466.3-2004 Plastic Differential Scanning Calorimetry (DSC) Part 3.Melting and crystallization temperature and enthalpy
Determination
3 Terms and definitions
The following terms and definitions defined in GB/T 2035, GB/T 19466.1-2004 and 19466.3-2004 apply to this document.
3.1
Degree of crystallinity
The mass fraction of the crystalline phase in a semi-crystalline polymer. XC. The unit is expressed as a percentage (%).
4 Method summary
Put a known mass of PE-UHMW in the sample dish. Heat to the melting end temperature at a certain heating rate under protective gas
Degree above. Record the melting temperature curve. Simultaneously measure the heat flow of the sample vessel and the blank reference vessel. The area enclosed by the melting peak curve and the baseline
Represents the enthalpy of fusion. The sample quality is used for normalization. Then use the theoretical melting enthalpy of 100% crystalline polyethylene for normalization. which is
Obtain the crystallinity of the sample.
5 Apparatus and materials
5.1 Differential scanning calorimeter
See GB/T 19466.1-2004 5.1.
SH/T 1826-2019
5.2 Sample dishes
Aluminum DSC sample pan. Used to hold the sample and reference sample. Press the lid on the sample dish. And made of the same material of the same quality. Is measuring
Condition. The sample cuvette does not physically or chemically change with the sample and atmosphere.
5.3 Analytical balance
Weighing accuracy. ±0.01mg.
Note. When using a balance with an accuracy of 0.01 mg. The repeatability standard deviation of polyethylene fusion enthalpy is 1.2% [1].
5.4 Standard sample
See Appendix A of GB/T 19466.1-2004.Use standard samples of indium and tin.
5.5 Air source
Nitrogen or other inert gases. The purity is at least 99.9%.
6 Specimen
6.1 The PE-UHMW sample can be powder or fine particles. It can also be fragments of films or flakes. Recommended fine particle size or fragment thickness
The degree is not more than 0.25mm.
6.2 The machining process will affect the crystal structure of the material. If sampling from a large piece of PE-UHMW sample. It is recommended to use clean and sharp
A blade or other similar tool to cut thin slices. Tools that can generate heat to melt PE-UHMW should not be used to cut samples. Holes can also be used
The drill or puncher cuts the sample from the PE-UHMW film.
6.3 The sample should be flat. Ensure good contact with the sample cuvette.
6.4 It is recommended to take at least three samples from each test position for testing.
Note. The location in the sample where DSC analysis is required is defined as the "test location".
7 Test conditions and state adjustment of samples
See Chapter 7 of GB/T 19466.1-2004.
8 Calibration
See Chapter 8 of GB/T 19466.1-2004.
9 Test procedure
9.1 Instrument preparation
9.1.1 Before the test. Power on the instrument. Make it balanced for at least 30min.
9.1.2 Place two empty sample dishes with the same mass on the sample holder. Adjust to the actual measurement conditions. At the required temperature
Within range. The DSC curve should be a straight line. When you can't get a straight line. Record the DSC curve after confirming the repeatability.
9.1.3 During the entire test. The DSC test chamber should be filled with dry nitrogen or other inert gases. Flow at 50mL/min±5mL/min
Purge at speed. And all calibrations and tests should use the same gas and purge rate.
9.2 Placement of the sample
9.2.1 Select a sample vessel with an appropriate volume. And make sure it is clean.
9.2.2 Use two identical sample dishes. One is used as a sample cuvette. (Sample cuvette where the sample is placed). The other serves as a reference cuvette (without placing the sample
Sample dish) ꎻ
9.2.3 Weigh the sample vessel and lid. Accurate to 0.01 mg.
9.2.4 Place the sample in the sample cuvette. Seal the sample dish with the lid. Check the bottom of the sample cuvette to make sure it is flat. If it's not level. Then re-standard
Sample preparation
9.2.5 Weigh the sample cuvette after placing the sample. The mass of the sample should be between 5 mg and 10 mg. Accurate to 0.01 mg. The quality of the repeated test samples
The amount deviation is not more than 2mg. For materials or products containing additives. The sample mass refers to the polymer matrix after subtracting the additive mass
quality.
9.3 Placement of sample dishes
Use tweezers or other suitable tools to place the sample cuvette into the sample holder. Close the cover of the sample holder. Ensure that between the sample and the dish,
The contact between the dish and the support is good.
9.4 Test
9.4.1 Stable the sample at room temperature for at least 3min.
9.4.2 Heat the sample from room temperature to.200°C at a heating rate of 10°C/min. Record the enthalpy curve of the first heating process
9.4.3 Keep at this temperature for 5 minutes, if necessary. Re-cooling-heating cycle operation can be performed.
9.4.4 Decrease to room temperature at a cooling rate of 10°C/min. Keep it for 5min.
9.4.5 Repeat 9.4.2.Record the enthalpy curve of the second heating process.
Note. The information obtained from the first heating scan can indicate the thermal history of the polymer (such as processing and sample preparation). If you want to get unaffected by thermal history
The crystallinity of the sample can use the result of the second heating scan. Generally, the second temperature rise is used for the raw materials. For products to reflect their processing heat history
Impact. Use the first heating up more often.
9.4.6 During the test, if any weight loss is found due to chemical reaction. The upper temperature limit should be lowered. And it should be noted in the report.
10 Test results
10.1 Result calculation
10.1.1 In a heating cycle, connect the points corresponding to 50°C and 160°C on the curve to establish a straight baseline. If the melting process is
160°C does not end. You can move the baseline to a higher temperature. But this change must be recorded.
10.1.2 Integrate the area under the melting endothermic curve from the beginning of the heating cycle to the heat transition enthalpy. Get the heat of the endothermic process
Variety. Divide the heat by the mass of the sample. Obtain the enthalpy of fusion per unit mass of the sample. That is, the enthalpy of fusion of the sample ΔHm.
10.1.3 See formula (1) for calculation of crystallinity.
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