CN112724485A - Standard substance for self-detection of differential scanning calorimeter and application thereof - Google Patents
Standard substance for self-detection of differential scanning calorimeter and application thereof Download PDFInfo
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- CN112724485A CN112724485A CN202011488789.1A CN202011488789A CN112724485A CN 112724485 A CN112724485 A CN 112724485A CN 202011488789 A CN202011488789 A CN 202011488789A CN 112724485 A CN112724485 A CN 112724485A
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- 239000000126 substance Substances 0.000 title claims abstract description 68
- 238000001514 detection method Methods 0.000 title claims abstract description 15
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 33
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 15
- 150000008301 phosphite esters Chemical class 0.000 claims description 6
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical group CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- 239000002530 phenolic antioxidant Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 abstract description 19
- 230000003647 oxidation Effects 0.000 abstract description 17
- 238000007254 oxidation reaction Methods 0.000 abstract description 17
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 238000007689 inspection Methods 0.000 description 5
- 238000012937 correction Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000010421 standard material Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention provides a standard substance for self-detection of a differential scanning calorimeter. The standard substance comprises the following components in parts by weight: 99.4-99.8 parts of PE resin; 0.1-0.3 part of hindered phenol antioxidant; 0.1-0.3 part of phosphite antioxidant; the PE resin has a measured OIT of less than or equal to 2min at 200 ℃. The standard substance can well replace standard metal to serve as a standard substance of a differential scanning calorimeter, is low in cost, high in detection accuracy, short in detection time and high in stability, can serve as a rapid test means, and assists in monitoring the stability and data accuracy of the equipment under a fixed temperature in the oxidation induction period test.
Description
Technical Field
The invention relates to the field of instrument correction, in particular to a standard substance for self-detection of equipment for measuring an oxidation induction period by a differential thermal analysis method and application thereof.
Background
The oxidation induction period is one of important performance indexes of the existing cable material, the existing equipment for testing the oxidation induction period is mainly a differential scanning calorimeter, the existing domestic common test brand still has some defects in equipment stability, and the accuracy of test data of equipment oxidation induction period items needs to be monitored regularly. Since there is no relevant standard substance for daily self-test of the equipment on the market at present, the common means for self-test of the equipment is to use standard metals of indium (In, melting point 156.61 ℃) and tin (Sn, melting point 231.89 ℃) to test the temperature stability and accuracy.
However, the temperature test conditions commonly used in the oxidation induction period test are 200 ℃, 210 ℃ and 220 ℃, the temperature is a main influence factor of the oxidation induction period, and experiments show that the oxidation induction period test values of the same material under different temperature sections are greatly different. Taking MDPE-5105 as an example, the oxidation induction period is 68.4min at 200 ℃, 41.0min at 210 ℃ and 19.5min at 220 ℃. It can be seen that the effect of the change in temperature on the oxidative induction period is very significant. In addition, instrument self-inspection using standard metals indium and tin cannot be accurate to the required test temperature, and the influence of temperature range fluctuation may exist. Meanwhile, atmosphere, gas flow rate, sample size, sample shape, temperature rise rate and the like all have certain influence on the sample, so that the instrument self-inspection is carried out by using standard metal, and the problem that the accuracy self-inspection characterization of the oxidation induction period project test cannot be comprehensively carried out exists.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a standard substance for self-checking of a differential scanning calorimeter, which can more accurately perform self-checking on the differential scanning calorimeter compared with a standard metal.
The invention also aims to provide a method for using the standard substance for the self-detection of the differential scanning calorimeter in the self-detection of the differential scanning calorimeter.
The above purpose of the invention is realized by the following technical scheme:
a standard substance for self-detection of a differential scanning calorimeter comprises the following components in parts by weight:
99.4-99.8 parts of PE resin;
0.1-0.3 part of hindered phenol antioxidant;
0.1-0.3 part of phosphite antioxidant;
the OIT value of the PE resin is less than or equal to 2min at 200 ℃.
Compared with the standard metal with only one melting point, a plurality of standard substances suitable for different detection temperatures can be obtained by slightly adjusting the formula of the PE resin standard substance, the oxidation induction period of the self-detection standard substance can be controlled within a reasonable range, and the problems of inaccuracy and overlong detection time of the conventional standard substance are solved. If the OIT value of the PE resin is too high, the condition that the quality of a sample is floated and unstable easily occurs, the PE resin with the OIT value less than or equal to 2min is selected, the banburying process can be better controlled, and a standard substance with the oxidation induction period of 10-20 min can be obtained more easily.
More preferably, the OIT of the PE resin is measured at 200 ℃ for 1-2 min.
Preferably, the PE resin is recycled. The PE resin of the reclaimed material has lower cost and is more easily obtained.
Preferably, the standard substance is prepared by adopting an internal mixing method. The banburying condition can affect the dispersion condition of the antioxidant in the system, and meanwhile, because the addition amount of the antioxidant is small, if the banburying time is insufficient, the OIT value fluctuation of sample quality inspection is easy to cause. More preferably, the banburying conditions are that the banburying time is 8-10 min and the banburying temperature is 180 +/-5 ℃.
Most preferably, the mixing condition is most preferably mixing time 10min and mixing temperature 180 ℃. Under the condition, different formulas are adjusted to obtain the standard substance with proper oxidation induction period suitable for the temperature of more than 200 ℃.
The hindered phenolic antioxidant is a commonly used antioxidant, most preferably, the hindered phenolic antioxidant is most preferably antioxidant 1010.
Phosphite antioxidants are one of the commonly used antioxidants, most preferably, the phosphite antioxidant is most preferably antioxidant 168.
More preferably, the hindered phenol antioxidant and the phosphite antioxidant are preferably mixed in equal proportion.
More preferably, the preparation method of the standard substance comprises the following steps: mixing and shaking the components uniformly, then pouring the mixed sample into an internal mixing module, keeping the temperature of the internal mixing module constant at 180 ℃, and carrying out internal mixing for 10min to obtain the standard substance.
As mentioned above, the OIT value is closely related to temperature, and in order for the standard substance to meet the self-test requirements for OIT, it is preferred that the OIT value of the standard substance fluctuate by less than 10%, and that there be shorter OIT values at different test temperatures. More preferably, aiming at the common self-test of 200 ℃, 210 ℃ and 220 ℃, the invention adopts the following corresponding preferred scheme:
a method of self-testing a differential scanning calorimeter using the standard substance, replacing a standard metal substance with the standard substance, and using a standard substance formulation for OIT values at 200 ℃ of the apparatus:
99.8 parts of PE resin;
0.1 part of hindered phenol antioxidant;
0.1 part of phosphite ester antioxidant.
Under the method, the standard value of the standard substance tested under the temperature condition of 200 ℃ is (18.3 +/-1.8) min.
A method for self-testing a differential scanning calorimeter using the standard substance, the standard substance replacing a standard metallic substance, and using a standard substance formulation for OIT values at 210 ℃ of the equipment:
99.6 parts of PE resin;
0.2 part of hindered phenol antioxidant;
0.2 part of phosphite ester antioxidant.
Under the method, the standard value of the standard substance tested under the temperature condition of 200 ℃ is (20.4 +/-2) min.
A method for self-testing a differential scanning calorimeter using the standard substance, wherein the standard substance is used in place of a standard metal substance, and the standard substance formula is as follows for OIT value at 220 ℃ of equipment:
99.6 parts of PE resin;
0.3 part of hindered phenol antioxidant;
0.3 part of phosphite ester antioxidant.
Under the method, the standard value of the standard substance tested under the temperature condition of 200 ℃ is (16.0 +/-1.6) min.
The standard substance of the invention can still meet the requirement of tolerance after long-term storage (more than half a year).
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a standard substance for differential scanning calorimeter self-inspection, which takes PE resin as a base material, is matched with an antioxidant and a proper processing method, can well replace standard metal as the standard substance of the differential scanning calorimeter, has low cost, higher detection accuracy, short detection time and high stability, and can be used as a rapid test means to assist in monitoring the stability of equipment under a fixed temperature and testing the oxidation induction period and the data accuracy.
Detailed Description
The present invention will be described in further detail with reference to specific examples and comparative examples, but the present invention is not limited to the examples.
In the examples, the starting materials not specifically mentioned are all conventional commercial products.
PE resin reclaimed material A: trade mark, source (trade mark: PE-LT17BK01ML source: Japanese miscellaneous feeds)
PE resin reclaimed material B: brand and source (source of YBL-PE01ZK is produced by self-mixing)
Antioxidant 1010 and antioxidant 168 are commercially available.
The oxidation induction period of the PE resin reclaimed material A is 1.3 +/-0.2 min at the temperature of 200 ℃. The oxidation induction period of the PE resin reclaimed material B is 3.4-7.2 min. The oxidation induction period of the recovered PE resin B itself is unstable, and therefore, it is not suitable for preparing a standard substance.
And (3) exploring a proper formula and banburying conditions to prepare the standard substance by using the PE resin reclaimed material A. Specifically, the process according to table 1 comprises the following steps: mixing and shaking up the components with the total amount of 50g, then pouring the mixed sample into an internal mixing module, setting the temperature of the internal mixing module at a constant value, and adjusting the internal mixing time to obtain different standard substances. And OIT of the standard substance at 200 ℃ was measured as shown in Table 1.
TABLE 1
From the conditions shown in Table 1, the mixing conditions have a strong influence on the OIT of the standard material, and when the mixing temperature is too low, the OIT time is longer, and when the mixing time is too short, the dispersion of the antioxidant is affected. In addition, the banburying temperature is increased, the OIT value is obviously reduced, and the antioxidant is more prone to lose efficacy at higher temperature.
In addition, in order to improve the correction accuracy, the standard substance with the OIT time of 10-20 min is more suitable. At 190 ℃ the OIT value of the standard material is already close to 10min, which is not supposed to be suitable for the correction above 200 ℃.
Therefore, most preferably, the banburying conditions are that the banburying temperature is 180 ℃ and the banburying time is 10 min.
According to the above-mentioned mixing conditions, 3 sets of sample formulations are provided, as shown in table 2:
TABLE 2
The samples of each example were specifically prepared as follows:
(1) weighing: the mass of each component of each formula is accurately calculated by taking 50g as the total amount, and the components are weighed according to the required mass.
(2) Uniformly mixing: pouring all weighed samples into a transparent self-sealing bag, sealing, and then shaking up by hand for at least 10min to ensure that the samples and the antioxidant are distributed uniformly;
(3) standby: after 3 samples with different formulas are mixed uniformly in sequence, marking for later use;
(4) heating to 180 ℃ by using an internal mixing module, and stabilizing the temperature of each module for at least 10 min;
(5) and pouring the standby mixed sample into an internal mixing module, carrying out internal mixing for 10min to ensure that the sample is uniformly mixed, and then taking out the sample. I.e. the standard substance.
Testing of each standard substance: taking samples prepared in the same batch in the above examples 1 to 3, respectively taking 5 groups of balance samples, raising the temperature to a specified test temperature (200 ℃/210 ℃/220 ℃ in sequence in examples 1 to 3) at a heating rate of 20 ℃/min in a nitrogen (99.99 percent and 50mL/min) atmosphere, switching to an oxygen (99.5 percent and above and 50mL/min) atmosphere, and keeping the temperature for 30 min; the oxidative induction period OIT of the standard substance of each example was measured and is shown in Table 3.
TABLE 3
Standard substance rating: combining OIT characteristics, the sample fluctuation is required to be less than 10%, and the PE-OIT-200 of example 1 is tested under the temperature condition of 200 ℃ for standard value of (18.3 +/-1.8) min; the PE-OIT-210 of example 2 has a standard value (20.4 +/-2) min under the temperature condition of 210 ℃; the PE-OIT-220 of example 3 was tested at 220 ℃ for the standard value of (16.0. + -. 1.6) min. All meet the requirements
Data tracking: the sample is sealed and stored in dark, and the verification test is carried out after half a year, and the test data is still stable within the range.
Table 4 is the validation test data after half a year storage:
TABLE 4 verification test half a year later
It can be seen that the standard sample prepared by the invention is still very stable after long-term storage, and meets the use requirement.
Claims (10)
1. A standard substance for self-detection of a differential scanning calorimeter is characterized by comprising the following components in parts by weight:
99.4-99.8 parts of PE resin;
0.1-0.3 part of hindered phenol antioxidant;
0.1-0.3 part of phosphite antioxidant;
the OIT value of the PE resin is less than or equal to 2min at 200 ℃.
2. The standard substance of claim 1, wherein the PE resin is recycled.
3. The standard substance according to claim 1, wherein the standard substance is prepared by adopting an internal mixing method, the internal mixing condition is that the internal mixing time is 8-10 min, and the internal mixing temperature is 180 +/-5 ℃.
4. The standard substance as claimed in claim 1 or 3, wherein the mixing conditions are a mixing time of 10min and a mixing temperature of 180 ℃.
5. The standard substance according to claim 1, wherein the hindered phenolic antioxidant is antioxidant 1010.
6. The standard substance of claim 1, wherein the phosphite antioxidant is antioxidant 168.
7. The standard substance according to claim 1, wherein the hindered phenol antioxidant is mixed with the phosphite antioxidant in equal proportion.
8. A method of self-testing a differential scanning calorimeter using a standard substance according to any one of claims 1 to 7, wherein the standard substance is used in place of a standard metal substance and the standard substance is formulated as follows for the OIT value at 200 ℃ of the apparatus:
99.8 parts of PE resin;
0.1 part of hindered phenol antioxidant;
0.1 part of phosphite ester antioxidant.
9. A method of self-testing a differential scanning calorimeter using a standard substance according to any one of claims 1 to 7, wherein the standard substance is used in place of a standard metal substance and the standard substance is formulated as follows for the OIT value at 210 ℃ of the apparatus:
99.6 parts of PE resin;
0.2 part of hindered phenol antioxidant;
0.2 part of phosphite ester antioxidant.
10. A method of self-testing a differential scanning calorimeter using a standard substance according to any one of claims 1 to 7, wherein the standard substance is used in place of a standard metal substance and the standard substance is formulated as follows for the OIT value at 220 ℃ of the apparatus:
99.6 parts of PE resin;
0.3 part of hindered phenol antioxidant;
0.3 part of phosphite ester antioxidant.
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CN202011488789.1A CN112724485A (en) | 2020-12-16 | 2020-12-16 | Standard substance for self-detection of differential scanning calorimeter and application thereof |
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CN202011488789.1A CN112724485A (en) | 2020-12-16 | 2020-12-16 | Standard substance for self-detection of differential scanning calorimeter and application thereof |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114933751A (en) * | 2022-05-06 | 2022-08-23 | 山东非金属材料研究所 | Polyethylene ferric oxide standard substance and preparation method thereof |
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US4797511A (en) * | 1987-09-25 | 1989-01-10 | Uniroyal Chemical Company, Inc. | Polyethylene stabilized by mixture of hindered phenol and amine antioxidants |
JPH09157577A (en) * | 1995-12-06 | 1997-06-17 | Kawasaki Steel Corp | Metal-coating polyolefin resin composition excellent in durability |
CN111849055A (en) * | 2019-04-25 | 2020-10-30 | 中国石油化工股份有限公司 | Polyethylene resin composition, polyethylene resin pellet, polyethylene expanded bead, method for producing same, and molded article |
CN111925358A (en) * | 2020-06-22 | 2020-11-13 | 宿迁联盛科技股份有限公司 | Light stabilizer and preparation process thereof |
-
2020
- 2020-12-16 CN CN202011488789.1A patent/CN112724485A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4797511A (en) * | 1987-09-25 | 1989-01-10 | Uniroyal Chemical Company, Inc. | Polyethylene stabilized by mixture of hindered phenol and amine antioxidants |
JPH09157577A (en) * | 1995-12-06 | 1997-06-17 | Kawasaki Steel Corp | Metal-coating polyolefin resin composition excellent in durability |
CN111849055A (en) * | 2019-04-25 | 2020-10-30 | 中国石油化工股份有限公司 | Polyethylene resin composition, polyethylene resin pellet, polyethylene expanded bead, method for producing same, and molded article |
CN111925358A (en) * | 2020-06-22 | 2020-11-13 | 宿迁联盛科技股份有限公司 | Light stabilizer and preparation process thereof |
Non-Patent Citations (1)
Title |
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丁延伟主编: "《热分析基础》", 29 February 2020, 中国科学技术大学出版社 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114933751A (en) * | 2022-05-06 | 2022-08-23 | 山东非金属材料研究所 | Polyethylene ferric oxide standard substance and preparation method thereof |
CN114933751B (en) * | 2022-05-06 | 2023-09-12 | 山东非金属材料研究所 | Polyethylene ferric oxide standard substance and preparation method thereof |
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Application publication date: 20210430 |