1、GM DAEWOO Auto & Technology EDS Engineering, GM DAEWOO Auto & Technology Standards TEST METHOD FOR MATERIAL ANALYSIS OF PLASTIC & RUBBER USING FTIR EDS-T-7826 ISSUED DATE: 1996. 05. 09 REVISED DATE: 2006. 06. 19 VERSION: 3 EDS-T-7826TEST METHOD FOR MATERIAL ANALYSIS OF PLASTIC & RUBBER USING FTIR PA
2、GE: 1/3 ISSUED DATE: 1996. 05. 09 REVISED DATE: 2006. 06. 19 VERSION: 3 GM DAEWOO Auto & Technology 1. PURPOSE This standard aims at specifying the analysis method of plastic and rubber parts used for automobiles using FTIR. 2. EQUIPMENT 2.1. FTIR (Fourier transform infrared spectroscopy) 2.2. Centr
3、ifugal separator 2.3. Hot plate 2.4. 50 ml, 100 ml beakers 2.5. Toluene, Chloroform 2.6. Test tube 2.7. Pyrolyzer 2.8. KRS window 3. PRINCIPLE OF TEST FTIR is a method of performing qualitative and quantitative analysis with the infrared absorption spectrum obtained by measuring the absorbed quantit
4、y of the gas, liquid or solid sample for each frequency when the infrared beam (frequency: 4,000 400 cm) passes through them. The infrared beam absorption spectrum is expressed by a graph with the frequency in the x-axis and the trasmittance or absorbance in the y-axis. The peculiar molecule of the
5、plastic and rubber always repeats movement. Its kinetic energy remains in the similar wavelength range of the infrared beam. When the infrared beam is scanned, the infrared beam wavelength corresponding to the kinetic energy of the molecule is absorbed or transmitted to show a peculiar wavelength ba
6、nd. The peculiar infrared beam wavelength band resulting from the molecular movement confirms the molecular structure of the sample to allow qualitative analysis of the sample. 4. SAMPLE PREPARATION 4.1. Pre-conditioning of plastic parts 4.1.1. Melting Take a portion of the part free from defected m
7、atters and insert it between two glass plates. Raising the temperature to above the melting point of the plastic and pressing the piece between two glass plates produces a sample that has the transparency to permit transmission of light. 4.1.2. Purification EDS-T-7826TEST METHOD FOR MATERIAL ANALYSI
8、S OF PLASTIC & RUBBER USING FTIR PAGE: 2/3 ISSUED DATE: 1996. 05. 09 REVISED DATE: 2006. 06. 19 VERSION: 3 GM DAEWOO Auto & Technology Put some 1 mg of the sample into a mortar together with some 200 mg of potassium bromide powder for infrared beam spectrum. While cautioning not to get it damp, comp
9、letely blend it by swiftly making into small granules, put it into the hand press and apply pressure to effect molding for 3 5 minutes. 4.1.3. Solvent Select a solvent capable of melting the sample to solve the sample in it. After taking a proper amount sample, put it into a 100 ml beaker and pour t
10、he solvent. Apply heat of 120 150 to the hot plate and check that the sample solves. If inorganic additives, such as talc, are mixed, separate them with a centrifugal separator and filter it. Apply the filtered solution on the KRS window and dry the solvent to get the sample. 4.2. Pre-conditioning o
11、f rubber parts The rubber part sample is made by the following method. 4.2.1. Sap extraction After preparing a heat-resistant test tube, cut the rubber into small pieces and fill the test tube bottom with them. Heat the test tube bottom with an alcohol lamp and observe if white smoke comes out. Once
12、 the sap of the rubber starts to form as a result of continued heating, tilt the test tube and apply it to the KRS window to get the sample. 4.2.2. Pyrolyzer It is mainly used when the rubber part is of a small amount. Take some 1 mg of rubber and wrap it with a PYRO foil of proper temperature range
13、 (500 800 ) to seal it. The pyrolyzer is a system to check the quality with FTIR by making rubber into vapor using the PYRO foil, a foil for sampling, and separating each component by GC (gas chromatography). 5. TEST PROCEDURES 5.1. Before using the FTIR, check the coolant and input air pressure fir
14、st. 5.2. After turning on the equipment, wait until the Interferogram is stabilized. 5.3. Input the user name. 5.4. Press F1 key in the menu to run SET UP PARAMETER. 5.5. After confirming that Interferogram got stabilized, perform calibration. 5.6. Exit to the menu and press F3 key to run SCAN AND D
15、ISPLAY. 5.7. In SPECTRUM TYPE, select TRANSMITTANCE or ABSORBANCE to run it. 5.8. Mount the sample made in clause 4 in the sample chamber of FTIR. 5.9. In SPECTRUM TYPE, select TRANSMITTANCE or ABSORBANCE to run it. EDS-T-7826TEST METHOD FOR MATERIAL ANALYSIS OF PLASTIC & RUBBER USING FTIR PAGE: 3/3
16、 ISSUED DATE: 1996. 05. 09 REVISED DATE: 2006. 06. 19 VERSION: 3 GM DAEWOO Auto & Technology 5.10. For the infrared ray absorption spectrum thus obtained, determine the type of material by running the searching program stored in IR program to or by using the established IR spectrum hand book through
17、 comparison. 5.11. If the transmittance or absorbance is so bad as to make it impossible to determine the material by spectrum, make a sample in another method and perform measuring. When two or more materials are combined to form a copolymer and thus make decision difficult, use PGC/FTIR system to analyze the material. 6. ABSORPTION FREQUENCY BY MOLECULAR STRUCTURE USEFUL FOR MATERIAL DETERMINATION OH : 3600 cm Carbon triple bonding: 2150 cm NH : 3500 cm C=O : 1715 cm C-H : 3000 cm Carbon double bonding: 1650 cm CN : 2250 cm C- O : 1100 cm
