Archive for the ‘Chemistry’ Category

Raman Analysis of Pharmaceutical Ingredients

Thursday, September 2nd, 2010

A range of options is available for Raman analysis, including systems suitable for handheld, laboratory and educational applications. Systems typically include a spectrometer, laser, operating software and sampling accessories, while modular options are available for users to configure their own Raman systems. Most applications are handled in the 150-3200 cm-1 range, with resolution of ~6-10 cm-1.

Introduction
Raman spectroscopy offers a number of benefits for testing and characterization. It is rapid and non-destructive, requires only limited sample preparation and allows for sample volumes in the microliter range. In addition, Raman can be used to measure aqueous samples or samples with high moisture content, and allows researchers to capture data from a sample contained in plastic or other materials that are optically transparent to the wavelengths of interest.

Raman is particularly useful for pharmaceutical applications. For example, Raman techniques are used to discern characteristics of pharmaceutical raw materials, including active ingredients, binders, fillers, lubricants and other excipients. Raman is also useful for through-container measurements of pharmaceutical blister packs, pill bottles and vials.

Experimental Conditions
To illustrate the capabilities of our Raman systems we analyzed Paracetamol (acetaminophen) and Carbamazepine, which are pharmaceutical active ingredients, and the excipients alpha and beta lactose. The samples studied consisted of simple organic compounds contained in standard, clear borosilicate scintillation vials. No additional preparation was necessary.

Samples were analyzed using a modular Raman setup comprising our QE65000 Spectrometer, a 785 nm laser with 500 mW output and a fiber optic probe. The spectrometer was set from ~780-940 nm and configured with a 50 µm slit for good optical resolution. High reflectivity optical bench mirrors increased spectrometer sensitivity.

To collect signal, we placed the tip of the probe at the bottom of three glass vials containing the samples. We measured the samples at an integration time of 8 seconds and averaged three spectra.

Results
Our measurements confirmed that this Raman configuration can differentiate various pharmaceutical raw materials based on their spectral fingerprints. Also, the experiment helped demonstrate that, with proper method development and application of chemometric analysis, our Raman setups can be used to obtain semi-quantitative data of active ingredients in a pharmaceutical mixture.

Our experiment also showed that fluorescence occurs in the lactose samples. Fluorescence is a common phenomenon in Raman measurements of some organic compounds and depends on the wavelength of the laser utilized.

Conclusions
The availability of both turnkey and modular Raman systems, complemented by sophisticated chemometric analysis packages and spectral libraries, makes Raman spectroscopy a versatile choice for a host of applications.

Effect of Sandblasting on the Specular Reflection from Encoder Wheels

Friday, July 16th, 2010

Goal:
Determine the impact of sandblasting on specular reflection from different types of encoder wheels

Experimental Conditions:
Several encoder wheels were sent for analysis. The samples are described below. (more…)

Bacillus globigii spores in terbium reagent

Tuesday, February 9th, 2010

Goal:
Illustrate the effect of the variable delay microcode on the shape of the terbium spectrum (more…)

LIBS Analysis of Materials Generated During the Zinc Refinement Process

Tuesday, February 9th, 2010

Goal:
Assess the feasibility of using LIBS to detect various elements in materials generated during the zinc refinement process (more…)

Non-intrusive Reflective pH Sensing in Tubes of Muddied/Sediment Water

Friday, January 15th, 2010

Goal
There was an interest in non-intrusively monitoring pH in tubes containing wet soil samples. This was significant for a number of reasons; this was the first time the reflective patches were to be tested in something other than a cuvette, on a curved surface rather, and this was also the first time an analyte solution was observed that contained sediment or turbidity. (more…)

Measuring Headspace of Organic Solvents

Friday, January 15th, 2010

Abstract
This application note explains how oxygen concentration is measured in the headspace of organic solvents such as Acetonitrile. (more…)

Smart Oxygen Cuvette for Optical Monitoring of Dissolved Oxygen in Biological Blood Samples

Tuesday, January 12th, 2010

A smart Oxygen Cuvette is developed by coating the inner surface of a cuvette with oxygen sensitive thin film material. The coating is glass like sol-gel based sensor that has an embedded ruthenium compound in the glass film. The fluorescence of the ruthenium is quenched depending on the oxygen level. Ocean Optics phase fluorometer, NeoFox is used to measure this rate of fluorescence quenching and computes it for the amount of oxygen present. (more…)

HiOXY Measurement of Methane Gas

Monday, December 28th, 2009

Goal:
To measure oxygen for the purpose of detecting methane gas. (more…)

Measuring Oxygen Concentration in Headspace

Wednesday, December 9th, 2009

Goal:

To measure oxygen concentration is measured in the headspace of organic solvents such as Acetonitrile) using a phase fluorometer system (more…)

PNNL pH Sediment Tubes

Tuesday, December 8th, 2009

Goal:
Non-intrusive Reflective pH Sensing in Tubes of Muddied/Sediment Water (more…)

Effect of fiber diameter on fluorescein fluorescence

Monday, October 26th, 2009

Goal:
Assess the effect of various fiber diameters on fluorescein fluorescence (more…)