Comparative Variable Temperature Studies of Polyamide II with a Benchtop Fourier Transform and a Miniature Handheld Near-Infrared Spectrometer Using 2D-COS and PCMW-2D Analysis

Abstract

The main objective of this communication is to compare the performance of a miniaturized handheld near-infrared (NIR) spectrometer with a benchtop Fourier transform near-infrared (FT-NIR) spectrometer. Generally, NIR spectroscopy is an extremely powerful analytical tool to study hydrogen-bonding changes of amide functionalities in solid and liquid materials and therefore variable temperature NIR measurements of polyamide II (PAII) have been selected as a case study. The information content of the measurement data has been further enhanced by exploiting the potential of two-dimensional correlation spectroscopy (2D-COS) and the perturbation correlation moving window two-dimensional (PCMW2D) evaluation technique. The data provide valuable insights not only into the changes of the hydrogen-bonding structure and the recrystallization of the hydrocarbon segments of the investigated PAII but also in their sequential order. Furthermore, it has been demonstrated that the 2D-COS and PCMW2D results derived from the spectra measured with the miniaturized NIR instrument are equivalent to the information extracted from the data obtained with the high-performance FT-NIR instrument.

Keywords

Near-infrared (NIR)Fourier transform infrared spectroscopy (FT-IR)Fourier transform near-infrared spectroscopy (FT-NIR)handheld NIR spectrometer hydrogen bonding perturbation correlation moving window two-dimensional (PCMW2D) analyses Polyamide II recrystallization two-dimensional correlation spectroscopy (2D-COS)variable temperature NIR spectroscopy

Get full access to this article

View all access options for this article.

References

Trifan

D.S.

Terenzi

J.F.

“Extents of Hydrogen Bonding in Polyamides and Polyurethanes”. J. Polym. Sci 1958; 28(117): 443–445.

Painter

P.C.

Coleman

M.M.

Fundamentals of Polymer Science, Lancaster, PA: Technomic Publishing Company, 1994, pp. 156–159.

R.J. Palmer. Encyclopedia of Polymer Science and Technology. Polyamides, Plastics. Hoboken, NJ: John Wiley and Sons, 2001. Pp. 618–642.

Siesler

H.W.

Dal Maso

Zanier

“Rheo-Optical Fourier-Transform NIR Spectroscopy of Polyamide 11”. Analusis Magazine 1998; 26(4): 61–64.

Yeh

Hsiao

B.S.

Sauer

B.B.

Michel

Siesler

H.W.

“In-Situ Studies of Structure Development During Deformation of a segmented Poly(urethane-urea) Elastomer”. Macromolecules 2003; 36(6): 1940–1954.

Skrovanek

D.J.

Painter

P.C.

Coleman

M.M.

“Hydrogen Bonding in Polymers. 2. Infrared Temperature Studies of Nylon 11”. Macromolecules 1986; 19(3): 699–705.

Serpe

Chaupart

“Relaxation-Structure Relationship in Bulk and Plasticized Polyamide 11”. J. Polym. Sci. Part B: Polym. Phys 1996; 34(14): 2351–2365.

Kinoshita

“An Investigation of the Structures of Polyamide Series”. Die Makromolekulare Chemie 1959; 33(1): 1–20.

Miyake

“Infrared Spectra and Crystal Structures of Polyamides”. J. Polym. Sci 1960; 44(143): 223–232.

10.

Noda

“Generalized Two-Dimensional Correlation Method Applicable to Infrared, Raman, and Other Types of Spectroscopy”. Appl. Spectrosc 1993; 47(9): 1329–1336.

11.

Noda

Dowrey

A.E.

Marcott

Story

G.M.

Ozaki

“Generalized Two-Dimensional Correlation Spectroscopy”. Appl. Spectrosc 2000; 54(7): 236A–248A.

12.

Noda

Ozaki

“Principle of Two-dimensional Correlation Spectroscopy”. In: Noda

Ozaki

(eds). Two-dimensional Correlation Spectroscopy–Applications in Vibrational and Optical Spectroscopy, Chichester, UK: John Wiley and Sons, 2004, pp. 15–38.

13.

Morita

Shinzawa

Noda

Ozaki

“Perturbation-Correlation Moving-Window Two-Dimensional Correlation Spectroscopy”. Appl. Spectrosc 2006; 60(4): 398–406.

14.

Thomas

Richardson

H.H.

“Two-Dimensional FT-IR Correlation Analysis of the Phase Transitions in a Liquid Crystal, 40-n-octyl-4-cyanobiphenyl(8CB)”. Vib. Spectrosc 2000; 24(1): 137–146.

15.

Jia

Wang

“An Insight into Sequential Order in Two-Dimensional Correlation Spectroscopy”. Appl. Spectrosc 2009; 63(3): 344–353.

16.

Sorak

Herberholz

Iwascek

Altinpinar

Pfeifer

Siesler

H.W.

“New Developments and Applications of Handheld Raman, Mid-Infrared, and Near-Infrared Spectrometers”. Applied Spectroscopy Reviews 2012; 47(2): 83–115.

17.

N.A. O’Brien, C.A. Hulse, D.M. Friedrich, F.J. Van Milligen, M.K. Von Gunten, F. Pfeifer, H.W. Siesler. “Miniature Near-Infrared (NIR) Spectrometer Engine for Handheld Applications”. Proceedings of SPIE - The International Society for Optical Engineering. 2012. 8374: 837404-1-837404-8.

18.

M. Pfirzer, K. Sawatski. “Method and Device for Correcting a Spectrum”. US Patent 7359815. Filed 2006. Issued 2008.

19.

Wartewig

“Manipulating”. IR and Raman Spectroscopy–Fundamental Processing, Weinheim, Germany: Wiley-VCH GmbH, 2003, Chap. 10, pp. 77–79.

20.

Siesler

H.W.

“Two-Dimensional Correlation Analysis of Variable-Temperature Fourier-Transform Mid- and Near-Infrared Spectra of Polyamide 11”. Journal of Molecular Structure 2000; 521(1–3): 37–47.

21.

Brill

“Über das Verhalten von Polyamiden beim Erhitzen”. J. Prakt. Chem 1942; 161(1–3): 49–64.

22.

Feldman

Wachtel

Vaughan

G.B.M.

Weinberg

Marom

“The Brill Transition in Transcrystalline Nylon-66”. Macromolecules 2006; 39(13): 4455–4459.

23.

Hirschinger

Miura

Gardner

K.H.

English

A.D.

“Segmental Dynamics in the Crystalline Phase of Nylon 66: Solid-State 2H NMR”. Macromolecules 1990; 23(8): 2153–2169.

24.

Murthy

N.S.

Curran

S.A.

Aharoni

S.M.

Minor

“Premelting Crystalline Relaxations and Phase Transitions in Nylon 6 and 6,6”. Macromolecules 1991; 24(11): 3215–3220.

25.

Cui

Yan

“Preparation, Characterization and Crystalline Transitions of Odd Even Polyamides 11,12 and 11,10”. European Polymer Journal 2005; 41(4): 863–870.