Characterization method for polymer molecular weight
A polymer and molecular weight technology, applied in the field of polymers, can solve the problems of increased test cost, chromatographic column replacement, and high cost, and achieve the effects of less sample amount and solvent amount, accurate test results, and low characterization cost.
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[0039] Example 1
[0040] The test instrument is a Bruker Ascend series 400MHZ liquid nuclear magnetic resonance spectrometer, the probe is a BBFO broadband high-resolution liquid probe, and the Z gradient field is 5.35G / mm.
[0041] 1) Instrument calibration
[0042] Use 80% ethylene glycol deuterated DMSO standard to calibrate the temperature in the range of 300-380K.
[0043] Use containing GdCl 3 99% of D 2 O / 1%H 2 The O standard sample repeatedly tests the self-diffusion coefficient of water until the diffusion coefficient of water at 298K is 1.872e-9, thus realizing the correction of the gradient.
[0044] 2) Determination of linear polyethylene molecular weight and molecular distribution
[0045] a) Obtaining the standard curve
[0046] Select a series of linear polyethylenes with known molecular weight and distribution shown in Table 1. Weigh 3 mg of the sample and dissolve it in a 10mm diameter glass tube, add 6 mL of deuterated tetrachloroethane, seal it, and then place it in a...
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[0055] Example 2
[0056] The pulse sequence used by 1D DOSY is still ledbpg2s1d, the diffusion time parameter (D20) is adjusted to 100ms, and the gradient pulse duration varies between 300-1800us with the molecular weight. The pulse gradient intensity is set to 1% and 98% respectively. Do a two-dimensional DOSY experiment on the sample PE4, obtain its 2D DOSY spectrum at 110°C, and then obtain the diffusion coefficient. 2D DOSY spectrum such as Image 6 As shown, where the F1 dimension is the sample’s 1 H NMR spectrum, F2 dimension is the diffusion axis. It can be seen from the figure that 1.40ppm is polyethylene 1 H NMR signal peak, 6.0 ppm is the signal of deuterated reagent. The two signals on the two-dimensional plane correspond to the diffusion signals of the polyethylene sample and the solvent under the experimental conditions, and the diffusion rates are 1.332*10. -9 m 2 / s and 5.32*10 -9 m 2 / s, and figure 2 The DOSY spectrum of PE4 shown is basically the same, and the...
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