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Related Concept Videos

Spectrophotometry: Introduction01:16

Spectrophotometry: Introduction

Spectrophotometry is the quantitative measurement of the absorption, reflection, diffraction, or transmission of electromagnetic radiation through a material as a function of the intensity and wavelength of the radiation. A spectrophotometer is a device used to measure the change in the radiation intensity caused by its interaction with the material.
The essential components of a spectrophotometer include a source of electromagnetic radiation, a slot for placing a material to be analyzed, and a...
IR and UV–Vis Spectroscopy of Aldehydes and Ketones01:29

IR and UV–Vis Spectroscopy of Aldehydes and Ketones

Infrared spectroscopy, also known as vibrational spectroscopy, is mainly used to determine the types of bonds and functional groups in molecules. In aldehydes and ketones, the carbonyl (C=O) bond shows an absorption around 1710 cm-1. The C=O bond vibration of an aldehyde occurs at lower frequencies than that of a ketone. In addition to the C=O absorption in an aldehyde, the aldehydic C–H bond also gives two peaks in the 2700–2800 cm-1 range. This absorption, coupled with the C=O stretching, is...
UV–Vis Spectroscopy: Woodward–Fieser Rules01:29

UV–Vis Spectroscopy: Woodward–Fieser Rules

UV–Visible absorption spectra of conjugated dienes arise from the lowest energy π → π* transitions. The light-absorbing part of the molecule is called the chromophore, and the substituents directly attached to the chromophore are called auxochromes. A strong correlation exists between the absorption maxima, λmax, and the structure of a conjugated π system. The Woodward–Fieser rules predict the value of λmax for a given structure by adding the contributions...
IR Spectroscopy: Hooke's Law Approximation of Molecular Vibration01:16

IR Spectroscopy: Hooke's Law Approximation of Molecular Vibration

A covalently bonded heteronuclear diatomic molecule can be modeled as two vibrating masses connected by a spring. The vibrational frequency of the bond can be expressed using an equation derived from Hooke's law, which describes how the force applied to stretch or compress a spring is proportional to the displacement of the spring. In this case, the atoms behave like masses, and the bond acts like a spring.
According to Hooke's law, the vibrational frequency is directly proportional to the...
UV–Vis Spectroscopy of Conjugated Systems01:32

UV–Vis Spectroscopy of Conjugated Systems

Organic compounds with conjugated double bonds show strong absorption features in the UV–visible region of the electromagnetic spectrum attributed to π → π* electronic excitations. Generally, a UV–vis absorption spectrum is recorded as a plot of absorbance vs wavelength. The wavelength of maximum absorbance, which manifests as a peak in the absorption spectrum, is denoted as λmax.
One of the factors influencing λmax is the extent of conjugation in the...
IR Spectroscopy: Molecular Vibration Overview01:24

IR Spectroscopy: Molecular Vibration Overview

When Infrared (IR) radiation passes through a covalently bonded molecule, the bonds transition from lower to higher vibrational levels. The fundamental vibrational motions that result in infrared absorption can be classified as stretching or bending vibrations.
Stretching vibrations are vibrational motions that occur along the bond line, changing the bond length or distance between two bonded atoms. They are further distinguished as symmetric or asymmetric. In symmetric stretching, the...

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Characterization of Biological Absorption Spectra Spanning the Visible to the Short-Wave Infrared
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Characterization of moisture-sensitive raw materials with simple spectroscopic techniques.

L Pan1, R Lobrutto, G Zhou

  • 1Merck and Co., Inc., Merck Research Laboratories, P.O. Box 2000, RY818-C306 Rahway, NJ 07065, USA.

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Summary

Spectroscopic techniques offer efficient analysis of air and water-sensitive raw materials. This study demonstrates FT-IR and NIRS methods for quantifying critical reagents in chemical synthesis, ensuring product quality and reaction efficiency.

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Area of Science:

  • Analytical Chemistry
  • Process Chemistry
  • Spectroscopy

Background:

  • Controlling raw material quality is crucial for synthetic processes.
  • Air and water-sensitive materials present significant quantitative analysis challenges.
  • Spectroscopic methods offer rapid, cost-effective analysis for reactive materials.

Purpose of the Study:

  • To demonstrate the utility of spectroscopic techniques for analyzing air and water-sensitive raw materials.
  • To develop and validate methods for quantifying specific reactive impurities and reagents.
  • To ensure optimal reaction conversion and product quality in chemical synthesis.

Main Methods:

  • Fourier Transform Infrared (FT-IR) spectroscopy for acetic acid quantification in acetic anhydride.
  • Near-Infrared Reflectance Spectroscopy (NIRS) for diisobutyl aluminum hydride (DIBAL-H) concentration in toluene.
  • NIRS with Partial Least Squares (PLS) regression for p-toluenesulfonic acid in p-toluenesulfonic anhydride.

Main Results:

  • A one-frequency calibration method accurately quantified 2-35 wt.% acetic acid in acetic anhydride.
  • A one-frequency calibration method determined 0-1.5 mol/L DIBAL-H in toluene.
  • A PLS-NIRS method was developed for quantifying p-toluenesulfonic acid, which is not suitable for chromatography.

Conclusions:

  • Spectroscopic methods provide effective solutions for analyzing challenging air and water-sensitive raw materials.
  • Developed methods ensure accurate quantification, preventing issues like reaction quenching and incomplete conversion.
  • These techniques enhance process control and product quality in chemical manufacturing.