Solid State Nuclear Magnetic Resonance Spectroscopy
Solid state Nuclear Magnetic Resonance (NMR) spectroscopy enables molecular level analysis of solid polymers. Using magnetic resonance of certain magnetic nuclei with an applied electromagnetic (EM) wave, NMR can identify and quantify the Hydrogen, Carbon and other elements along with associated functional groups. Solid state NMR spectroscopy of polymers is industrially significant, as most applications of polymers are in the solid state.
The Nuclear Magnetic Resonance (NMR) technique utilizes the fact that certain atomic nuclei have magnetic moments related to their spin and mass number. Isotopes of elements having odd mass numbers often have magnetic nuclei. When subjected to an external magnetic field, these magnetic nuclei absorb electromagnetic energy. Maximum energy is absorbed by the nuclei at their resonant frequency. When the eternal magnetic field is removed, the nuclei return to lower energy levels, emitting excess energy which is measured as absorption peaks in the NMR spectrum. The relative height of each peak correlates with the strength of absorption and area under the peaks is proportionate to the number of Hydrogen atoms contributing to that peak. This is the principle of NMR spectroscopy.
NMR experiments can provide valuable insights in studies of molecular structure and topology. Typically, organic compounds need field strengths ranging from about 1.4 to 18.0 teslas (T) and are subjected to electromagnetic radiation in the radio frequency range. NMR can be applied to substances in liquid solution or in solid state. When NMR spectroscopy is performed on solids, it is termed Solid State NMR.
Solid state NMR spectroscopy of polymers is industrially significant, as most applications of polymers are in the solid state. Magnetic isotopes of elements such as 1H, 13C, 19F, 29Si, 15N, yield high-resolution NMR spectra at their resonant frequencies. These elements are important constituents of plastics, elastomers and adhesives.
When studying molecular structures in solid polymers, NMR spectroscopy targets the magnetic 13C nucleus in the Carbon backbone. However only a small percentage of Carbon atoms in a polymer molecule comprises 13C isotope and they are surrounded by 1H atoms (protons). The resulting dipolar interactions with magnetized protons distort the 13C signal. This is resolved by heteronuclear dipolar decoupling (DD) which involves sending a strong radiofrequency pulse at the 1H frequency, during the period when the 13C signal is observed. Another necessary technique to be used in conjunction with Solid state NMR of polymers is magic angle spinning (MAS) which is used to deal with Chemical shift anisotropy that distorts signals. Chemical shift refers to the position of a peak relative to the peak of a reference chemical. Atoms in a molecule have different chemical shifts because they experience slightly different local magnetic fields owing to the presence of nearby electrons. The MAS procedure involves spinning the solid sample, at rates of a few thousand hertz and an angle of precisely 54.74° relative to the static magnetic field.
Polyethylene-co-vinyl acetate or EVA is an important elastomeric polymer. It is a random copolymer with vinyl acetate percentage varying from 10 % to 40% depending on end use. The molecular structure of EVA copolymer is as below:
In this case study, solid state 13 C NMR with MAS was used to analyse a powdered sample of EVA co-polymer. Figure 1 shows the 13C MAS NMR spectrum. The peak at 30.2 ppm is the CH2 backbone and a smaller peak at 14.3 ppm shows the CH3 radical of the acetate branch. Two small signals at about 21 and 25 ppm, are interpreted as CH2 from the ethylene branching.
Figure 1: Solid-state MAS NMR 13C spectrum of EVA polymer in powder form showing peaks and relative quantities of Hydrocarbon functional groups.
ASTM E572 test method covers the analysis of stainless and alloy steels by Wavelength Dispersive X-ray Fluorescence Spectrometry (WDXRF). It provides rapid, multi-element determinations with sufficient accuracy to assure product quality.
The ASTM D2674 test is a standard test method for the analysis of sulfochromate etch solutions used in the surface preparation of aluminum. The ASTM D2674 standard specifies a method for determining the efficacy of an etchant used to prepare the surface of aluminum alloys for subsequent adhesive bonding.
An immunological method for quantization of Hevea Natural Rubber (HNRL) proteins using rabbit anti-HNRL serum. Rabbits immunized with HNRL proteins react to the majority of the proteins present, and their sera have the capability to detect most if not all the proteins in HNRL.
ASTM G65 measures the resistance of metallic materials to abrasion using the dry sand/rubber wheel apparatus. The quality, durability, and toughness of the sample are determined using this test. Metallic materials are ranked in their resistance to scratching abrasion under a controlled environment.
ASTM E2141 test methods provide accelerated aging and monitoring of the performance of time-dependent electrochromic devices (ECD) integrated in insulating glass units (IGU). This test helps to understand the relative serviceability of electrochromic glazings applied on ECD.
ASTM C724 test method is used in analyzing the quality and ease of maintenance of a ceramic decoration on architectural-type glass. This test method is useful in the acknowledgment of technical standards.
Send us a request
Process for testing
You share material and testing requirements with us
You ship your sample to us or arrange for us to pick it up.
We deliver the test report to your email.
Just share your testing requirements and leave the rest on us!
Free, no-obligation consultation
Quick turnaround time
Let us combine our capabilities to achieve success!!