Foreword
This document is drafted in accordance with the provisions of GB/T 1.1-2020 "Guidelines for standardization work Part 1: Structure and drafting rules of standardization documents".
Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility of identifying patents.
This document is proposed by the China Petroleum and Chemical Industry Federation.
This document is attributed to the National Technical Committee for Standardization of Plastics (SAC/TC15).
1 Scope
This document specifies the technical requirements, test methods, testing rules, marking, packaging, transportation and storage of polyphenylene ether (PPE).
This document applies to 2,6-dimethylphenol and oxygen in the role of the catalyst polymerization of polyphenylene ether (PPE) products.
Note: Polyphenylene ether (PPE) is also known as PPO.
2 Normative references
The contents of the following documents constitute the essential provisions of this standard through the normative references in the text. Among them, note the date of the reference document, only the date of the corresponding version applies to this standard; do not note the date of the reference document, its latest version (including all the revision of the list) applies to this standard.
GB/T 1632.1 Plastics Determination of viscosity of dilute polymer solutions using capillary viscometer Part 1: General rules
GB/T 6678 General rules for sampling chemical products
GB/T 6679 General rules for sampling of solid chemical products
GB/T 8170 Numerical modification rules and limit values of the representation and determination
GB/T 30514 Glass capillary motion viscometer Specifications and operating instructions
JJG 694 Atomic absorption spectrophotometer
3 Terminology and definitions
There are no terms and definitions that need to be defined in this document.
4 Product classification
According to its characteristic viscosity, volatile matter, copper content index is divided into superior and qualified products.
5 Technical requirements
5.1 Appearance
The appearance of polyphenylene ether (PPE) should be milky white to light yellow uniform particles or powder.
5.2 Performance
Performance indicators of polyphenylene ether (PPE) should be in accordance with the provisions of Table 1.
6 Test methods
6.1 Appearance
Take 100g of particles or powder, visual inspection under natural light.
6.2 Characteristic viscosity
6.2.1 Principle
According to GB / T 1632.1, the determination of 25 ℃ trichloromethane solvent and concentration of 0.005g / mL of the outflow time of the sample, calculate the characteristic
viscosity.
6.2.2 Apparatus and reagents
Safety tips: the test method used in the trichloromethane, chromic acid washing solution is toxic, the operator should take appropriate safety and health protection measures to avoid contact with the skin and inhalation of its vapor, and in the fume hood.
6.2.2.1 Usher viscometer: GB/T 30514 in line with the provisions of the gas-bearing liquid column viscometer, model 0C, viscometer capillary diameter 0.36mm ~ 0.40mm, solvent flow time of 70s ~ 200s; can also use www.GB-GBT.cn GB/T 30514 listed in other types of viscometer, should ensure that the results of its determination and the above The provisions of the U. Viscometer equal; controversial, should use the U. Viscometer.
6.2.2.2 Analytical balance: accuracy 0.1mg.
6.2.2.3 volumetric flask: 50mL.
6.2.2.4 Glass sand core funnel: microporous diameter 40μm~100μm.
6.2.2.5 Timer: precision 0.01s.
6.2.2.6 Constant temperature water tank: temperature can be controlled at (25.0±0.1)℃.
6.2.2.7 Trichloromethane: analytical purity.
6.2.2.8 Chromic acid washing solution.
6.2.3 Test procedure
6.2.3.1 Solution preparation
Weigh (0.250±0.002)g of dry specimen, transfer to a 50mL volumetric flask, add 15mL of trichloromethane, shake to dissolve the specimen.
Then dilute to the scale with trichloromethane at 25℃ and shake well.
6.2.3.2 Test
6.2.3.2.1 Before measurement, filter the solution with a glass sand core funnel, and rinse the filtering device and the UVM with a small amount of solution, and add the filtered solution into the UVM, so that the liquid level is between the loading line. Install the viscometer into the constant temperature water bath (25.0±0.1)℃, ensure that the viscosity tube is vertical, and the upper line is at least 30mm below the surface of the water bath, constant temperature of 15min, determine the flow time of the sample.
6.2.3.2.2 each repeatedly measured 3 times, take the average value of the flow time, the extreme difference should not be greater than 0.2s.
6.2.3.2.3 Use the same Ushian viscometer to measure the average flow time of pure solvent in the same way, repeat the measurement 5 times, the extreme difference should not be greater than 0.2s, if the difference between the average flow time of two consecutive measurements is greater than 0.4s, the application of chromic acid washing solution to clean Ushian viscometer.
6.2.4 Calculation
6.3 Volatile matter
6.3.1 Instrument
6.3.1.1 Analytical balance: accuracy 0.1mg.
6.3.1.2 Weighing bottle: flat with cap.
6.3.1.3 Dry box: the use of the range of room temperature ~ 200 ℃, accuracy ± 1 ℃.
6.3.1.4 Desiccator: containing appropriate desiccant (such as discolored silica gel, etc.).
6.3.2 Operation steps
Weigh accurately (10.0±0.5)g specimen into the weighing bottle which has been baked to constant weight at (120±1)℃. The sample should be spread flat in the weighing bottle, and the height should not exceed 5mm. put the weighing bottle into the drying oven, dry it at 120℃ for 1h, then move it into the desiccator quickly, cool it for 45min and then weigh it, accurate to 0.1mg.
6.4 Copper content
6.4.1 Apparatus and reagents
6.4.1.1 Atomic absorption spectrophotometer: in accordance with the requirements of JJG694 calibration, with a copper hollow cathode lamp, wavelength set at 324.7nm, using air-acetylene flame for determination.
6.4.1.2 analytical balance: precision 0.1mg.
6.4.1.3 Volumetric flask: 100mL, 50mL.
6.4.1.4 Porcelain crucible: 100mL.
6.4.1.5 Copper ion standard solution mass concentration: 100mg/L.
6.4.1.6 1:1HNO3 aqueous solution.
6.4.1.7 graduated pipette: minimum accuracy of 0.1mL.
6.4.2 Sample processing
6.4.2.1 Weigh (5.0 ± 0.5) g of the sample in a porcelain crucible, placed on the electric furnace charring to non-smoking and placed in the (700 ± 50) ℃ muffle furnace ashing 2h, removed and cooled.
6.4.2.2 Add 1.5 mL of 1:1HNO3 to the crucible, heat it on the electric furnace until it boils, cool it down and fix the volume with deionized water in a 50 mL volumetric flask, shake well and set aside.
6.4.3 Preparation of standard solution
Pipette 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL, 3.0mL of copper ion standard solution (6.4.1.5) with a graduated pipette.
The solution was injected into a set of 100mL volumetric flasks. In the above-mentioned volumetric flasks, add 3 mL of L1:1HNO3 aqueous solution and dilute to the scale with deionized water to obtain the copper ion standard solutions with mass concentrations of 0.5 mg/L, 1.0 mg/L, 1.5 mg/L, 2.0 mg/L, 2.5 mg/L and 3.0 mg/L, respectively.
6.4.4 Test procedure
6.4.4.1 The absorbance of the standard solution was measured at 324.7 nm using an atomic absorption spectrometer and a copper elemental lamp with an air-acetylene flame, and zeroed with deionized water. The standard working curve was established with the concentration of copper ions as the horizontal coordinate and absorbance as the vertical coordinate.
6.4.4.2 The absorbance of the specimen was measured at 324.7 nm using an atomic absorption spectrometer and a copper elemental lamp with an air-acetylene flame, and zeroed with deionized water. According to the standard working curve to measure the content of copper in the sample.
7 test rules
7.1 Test batch
The same production line, the same raw materials, the same process produced by the same grade of polyphenylene ether (PPE) products as the test batch, the maximum batch does not exceed 100t.
7.2 Factory inspection
The technical items specified in Chapter 5 are factory inspection items, sampling methods and sampling volume according to GB / T 6678, GB / T 6679 of the provisions of the implementation. Each production batch of products by the production plant quality inspection department for inspection, inspection before leaving the factory, the factory products should be accompanied by a quality inspection certificate.
7.3 Judgment rules
The test results are determined by GB/T 8170 in the revision of the value of the comparison method, according to the lowest level to determine the level of the batch. Test results all pass, the batch of products is judged to be qualified. Test results, such as indicators do not meet the requirements of this document, should be re-sampled from twice the amount of packaging test, re-examination of the results of an indicator does not meet the requirements of this document, that is, the entire batch of products for failure. If qualified, determine the batch of products qualified.
8 Sign, packaging, transportation and storage
8.1 Logo
The bag should indicate the product name, specification, grade, batch number, net content, production date, the document number, trademark, the name of the manufacturer, address and other signs.
8.2 Packaging
The product is usually packed in round shape, and the small package is usually packed in plastic bags, or other forms of packaging can be used according to the needs of users.
8.3 Transportation
Product transportation and loading and unloading should be carried out in accordance with the provisions of the transport of goods, should take precautions. Transportation should be lightly moved, lightly placed, to prevent damage to the packaging.
Foreword
1 Scope
2 Normative references
3 Terminology and definitions
4 Product classification
5 Technical requirements
6 Test methods
7 test rules
8 Sign, packaging, transportation and storage
