Apparatus and method for analyzing samples with NMR

Patent metadata

Field	Value
Publication number	US-10042014-B2
Application number	US-201615132903-A
Country	US
Kind code	B2
Filing date	Apr 19, 2016
Priority date	Apr 20, 2015
Publication date	Aug 7, 2018
Grant date	Aug 7, 2018

Abstract

An apparatus and method for testing and analyzing the molecular structure of a sample material in an NMR device are described. A sample is held in a pre-determined stretched state in an apparatus that includes the sample arranged between two body components that are secured together with one or more retaining members that fit around the bodies or portions thereof. The apparatus is inserted into an NMR device to obtain NMR spectrums for analyzing the molecular structure of the samples, for instance, identifying strain-induced crystallinity and quantifying the same at pre-determined stretch ratios of a sample material.

First claim

What is claimed is:

1. An apparatus for testing a sample with NMR comprising: a. a first body comprising a sample contact surface along its length and a second body comprising a sample contact surface along its length for holding a sample comprising a stretched elastomer having a pre-determined stretch ratio; b. the sample arranged between the contact surface of the first body and the contact surface of the second body, wherein the sample contact surface of the first body and the sample contact surface of the second body press on the sample; c. a retaining member positioned around a portion of the sample, the portion of the sample arranged between a portion of the first body and a portion of the second body, wherein the retaining member secures the sample pressed between the first body and the second body.

2. The apparatus of claim 1 , the sample being a stretched sample of an elastomer.

3. The apparatus of claim 1 , the sample having a stretch ratio of greater than 4.

4. The apparatus of claim 1 , the sample containing rubber.

5. The apparatus of claim 1 , the first body and the second body being in direct contact with the sample.

6. The apparatus of claim 1 , the first body, the second body, or the retaining member being made of plastic.

7. The apparatus of claim 1 , the plastic being a thermoplastic.

8. The apparatus of claim 1 , the retaining member being positioned around the entire length of the first body and the second body.

9. The apparatus of claim 1 , further comprising a second retaining member, the second retaining member being positioned around an end portion of the first body and an end portion of the second body.

10. The apparatus of claim 9 , the first retaining member and the second retaining member being removably fixed to the first body and the second body.

11. The apparatus of claim 9 , the first retaining member and the second retaining member having same shape and dimensions.

12. The apparatus of claim 1 , the sample contact surface of the first body and the sample contact surface of the second body being in direct contact with the sample.

13. The apparatus of claim 1 , the first body and the second body having the same shape and dimensions.

14. The apparatus of claim 1 , wherein the sample being in a sample receiving space of an NMR device for rotating or analyzing the sample.

15. The apparatus of claim 14 , a solid state NMR spectrum of the sample being measured while the sample is rotated by the NMR device.

16. The apparatus of claim 15 , the sample being rotated in the NMR device at a frequency of 2 to 10 kHz.

17. The apparatus of claim 15 , the sample being positioned parallel to the axis of rotation.

18. A method for analyzing the molecular structure of a sample comprising: a. introducing the apparatus of claim 1 into a sample receiving space of an NMR device; b. rotating the sample in the apparatus in the NMR device; c. obtaining a NMR spectrum of the sample; d. calculating the amount of strain-induced crystallinity in the sample for the pre-determined stretch ratio.

19. The method of claim 18 , the sample being rotated in the NMR device at a frequency of 2 to 10 kHz.

20. The method of claim 18 , the sample being rotated in the NMR device at the magic angle of 54.74.degree. with respect to the external magnetic field to detect an NMR spectrum.

21. The method of claim 18 , the sample being a stretched sample of an elastomer.

22. The method of claim 18 , the sample having a stretch ratio of greater than 4.

23. The method of claim 18 , further comprising identifying strain-induced crystalline structure in the sample.

24. The method of claim 18 , further comprising positioning the first body against a first surface of the sample and the second body against a second surface of the sample.

25. The method of claim 24 , further comprising arranging a second retaining member over a portion of the first body and the second body.

26. The method of claim 18 , further comprising portions of the stretched sample being arranged within a second retaining member.

27. The method of claim 18 , further comprising the retaining member being positioned around the entire length of the first body and the second body.

28. The method of claim 18 , the sample being positioned in the apparatus such that the sample is rotated parallel to the axis of rotation.

Assignees

• Bridgestone Corp
• Univ Akron

Inventors

• Miyoshi Toshikazu
• Davis Michael C
• Hu Jiahuan

Classifications

• G01R33/307

  specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer · CPC title

• G01N24/08

  by using nuclear magnetic resonance (G01N24/12 takes precedence) · CPC title

• G01R33/30 Primary

  Sample handling arrangements, e.g. sample cells, spinning mechanisms · CPC title