New Quantitative Technique for Attenuated Total Reflection (ATR) Spectrophotometry; Calibration of the “CIRCLE” ATR Device in the Infrared

1986 ◽  
Vol 40 (7) ◽  
pp. 1019-1022 ◽  
Author(s):  
R. P. Sperline ◽  
S. Muralidharan ◽  
H. Freiser

A general method for spectroscopic determination of the incidence angle and number of reflections in ATR devices is described. This technique extends the inherent advantages of ATR by simplifying general quantitative spectroscopic measurements. Effects of polarization, beam focusing, errors of alignment, indices of refraction, handling of the optical elements, and surface activity of internal standard are discussed. Measured ATR absorbances are fitted mathematically with the use of incidence angle as a parameter. A standardizing solution, molar absorptivities for that solution, and knowledge of the dimensions of the internal reflection optical element are required. Application of the method to a cylindrical internal reflection (CIR) device gives the averaged incidence angle in the CIR with greater accuracy than is otherwise obtainable. With the use of a side-focusing Fourier transform spectrophotometer, the average incidence angle in the Spectra-Tech, Inc. “Micro-cell” “CIRCLE” CIR was 49.68 degrees ± 0.78%, and the number of solution-sensing internal reflections was 7.52 ± 1.95%.

Author(s):  
Meguya Ryu ◽  
Soon Hock Ng ◽  
Vijayakumar Anand ◽  
Stefan Lundgaard ◽  
Jingwen Hu ◽  
...  

Capabilities of the Attenuated Total Reflection (ATR) at THz wavelengths for increased sub-surface depth characterisation of (bio-)materials is presented. The penetration depth of a THz evanescent wave in biological samples is dependent on the wavelength and temperature and can reach 0.1-0.5 mm depth due to strong refractive index change ∼0.4 of the ice-water transition; this is quite significant and important when studying biological samples. Technical challenges are discussed when using ATR for uneven, heterogeneous, high refractive index samples with possibility of frustrated total internal reflection (a breakdown of the ATR reflection-mode into transmission-mode). Local field enhancements at the interface are discussed with numerical/analytical examples. Maxwell’s scaling was used to model behaviour of absorber-scatterer inside materials at the interface with ATR prism for realistic complex refractive indices of bio-materials. Modality of ATR with polarisation analysis is proposed and its principle illustrated, opening an invitation for its experimental validation. The sensitivity of the polarised ATR mode to the refractive index between the sample and ATR prism is revealed. Design principles of polarisation active optical elements and spectral filters are outlined. The results and concepts are based on experiments carried out at the THz beamline of the Australian Synchrotron.


2003 ◽  
Vol 0 (8) ◽  
pp. 2961-2965 ◽  
Author(s):  
N. Rochat ◽  
K. Dabertrand ◽  
V. Cosnier ◽  
S. Zoll ◽  
P. Besson ◽  
...  

2020 ◽  
pp. 000370282096971
Author(s):  
Nataša Radosavljević Stevanović ◽  
Milena Jovanović ◽  
Federico Marini ◽  
Slavica Ražić

Heroin is one of the most frequently seized drugs in Southeastern Europe. Due to the position in the Balkan route, the Republic of Serbia keeps important role in suppression of the trafficking of heroin for domestic and foreign illegal market. This research is aimed to provide a good scientific approach in the field of seized heroin analysis. Two different forms of heroin are present in the illegal market, mostly in mixtures with typical “cutting” agents: caffeine, paracetamol, and sugars. It was observed that the quantity of pure heroin in seized samples slightly increases from year to year. The aim of this study was to produce a reliable and fast procedure for classification of illicit heroin samples and determination of the concentration range of heroin in the samples. For that purpose, the attenuated total reflection Fourier transform infrared spectroscopy (ATR FT-IR) technique was used and combined with such chemometric methods as principal component analysis, cluster analysis, and partial least squares. Principal component analysis (PCA) as an unsupervised model was used for exploratory purposes to identify trends, similarities, and differences between samples by reducing the dimensionality of the data. The cluster classification of examined samples turned out to be extremely useful to evaluate the possibilities of the ATR FT-IR technique to classify the samples appropriately into the patterns, the constituted clusters. Additionally, partial least square was the suitable method for the purpose of determination of the heroin hydrochloride concentration range in examined samples. It is proved that the joined application of spectroscopy and chemometrics can be extremely convenient and useful for forensic and drugs control laboratories.


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