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3 using an integrating sphere – Ocean Optics DTS User Manual

Page 51

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Measuring the Spectrum of a Sample

Polychromix DTS

TM

Near-Infrared Spectrometer

6-5

Operator’s Manual

Document Number 04-91-0201-00 Rev A

6.3

Using an Integrating Sphere

An integrating sphere is normally used when the analyst wants to obtain the
spectrum of the surface of a solid or a turbid solution. The sample is placed
on the orifice of the sphere and is an integral part of the optical pathway.

6.3.1

The Sample

The following points regarding sample handling should be noted to ensure
the fidelity of collected spectra:

Do not get fingerprints on the surface of the sample. If you accidentally

touch the surface, wipe it off with a lint free tissue saturated with methanol
and allow the methanol to evaporate.

If a sample is contained in a bottle (flask, etc.) make certain that the

surface through which the infrared radiation passes is clean and is not
scratched, chipped or cloudy.

If the sample is believed to be homogeneous, collect spectra at a few

positions on the sample to ensure that you are viewing a representative
sample.

If the sample contains imperfections due to handling (e.g. scratches on a

piece of plastic) avoid the areas containing the imperfections.

6.3.2

Collecting a Reflectance Spectrum

To collect a spectrum:

a) Collect the background scan of an appropriate high reflectance material

such as “Spectralon” polymer or roughened gold as described in Section
5.2.

b) Place the sample on the integrating sphere and measure the reflectance.

6.3.3

Standards

The spectrum of a standard should be collected on a periodic basis. The
standard should have a number of absorbance bands spread across the
spectral region. When the spectrum of a standard is collected, the analyst
should check that the intensity of the bands and the wavelength remains
constant over time.

If difficulties are observed with the system, the spectrum of a standard should
be collected and compared to spectra that have been previously collected
using the same conditions.