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FT-IR - Experiment Setup

The document outlines the experimental setup for obtaining high-quality IR spectra, emphasizing the importance of selecting appropriate parameters such as number of scans, resolution, and background handling. It details various tabs in the setup dialog, including options for file handling, atmospheric suppression, and spectral range adjustments. Additionally, it discusses the impact of noise and resolution on spectral quality and provides guidelines for optimizing these settings for different applications.

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Wilmer Arias
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0% found this document useful (0 votes)
25 views34 pages

FT-IR - Experiment Setup

The document outlines the experimental setup for obtaining high-quality IR spectra, emphasizing the importance of selecting appropriate parameters such as number of scans, resolution, and background handling. It details various tabs in the setup dialog, including options for file handling, atmospheric suppression, and spectral range adjustments. Additionally, it discusses the impact of noise and resolution on spectral quality and provides guidelines for optimizing these settings for different applications.

Uploaded by

Wilmer Arias
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Experiment Setup

The world leader in serving science

Experimental parameters should be carefully selected to achieve IR spectra of satisfactory


quality within a reasonable amount of time for each application.

Experiment Setup 1
Experiment Setup

Collect Tab
Setting Number of Scans and Resolution
Final Format
Saving Files and Interferograms
Background Handling Options
Atmospheric Suppression
Preview Data Collection
Experiment Descriptions and Titles
Bench Tab
Setting Spectral Range, Gain, and Velocity
Quality Tab
Advanced Tab
Zero Filling, Apodization, and Phase Correction
Configure Tab
Diagnostics Tab
Align and Reset
100% Transmission Line Noise Test

Experiment Setup 2
Collect Tab – Setting Number of Scans and Resolution

Experimental parameters are selected in the Experimental Setup dialog box under the Collect
drop down menu.
Collect | Experiment Setup | Collect tab
Setting a sufficient number of scans and appropriate resolution is critical for obtaining an
acceptable spectral quality for each application. There is no one set parameters that works for
all applications.

Experiment Setup 3
Setting Number of Scans

S/N = Signal to Noise Ratio


Instrumental Noise: extraneous and random fluctuation in measured intensity.

S/N ~1.3 S/N >3.0

Signal Averaging
Signal is Constant
Noise is Random

Σ
S nSn Sn
= = n
N nNn Nn
# of Scans S: Signal, N: Noise, n: number of scans

D. A. Skoog and J. J. Leary, Principles of Instrumental Analysis 4th ed. Fort Worth: Saunders College Publishing, 1992.

Number of scans affects signal to noise ratio (S/N). A higher S/N ration leads to a better quality
spectrum. For the final spectrum, spectra are coadded and averaged by the number of scans.
Increasing the number of scans increases the S/N to a point, because signal intensity accumulates
linearly whereas noise intensity accumulates square root of number of scans.
Types Instrumental Noise - Thermal, Shot, Flicker, and environmental Noise
Thermal Noise (Johnson Noise): noise caused by agitation of charge carriers in resistors and
capacitors in an instrument.
Shot Noise: related to statistical fluctuations for random and quantized transfer event of charged
particles through junctions.
Flicker Noise (1/f): Noise with magnitude inversely proportional to frequency; hence the name “1/f
noise”.
Environmental Noise: Noise created from sources other than the instrument, but environment.
Types of Noise Measurements*
Peak-to-peak noise is the difference between the highest and lowest noise peaks in the selected
spectral region. Before measuring the noise, the software corrects any baseline tilt using a least-
squares correction method.
Root mean square (rms) noise measurement is a statistical analysis of the noise variation. The rms
noise level is equal to the square root of the average of the squares of the data points in the selected
spectral region.

Experiment Setup 4
Resolution
ƒ The ability to separate two closely spaced bands.
ƒ Bands with Full Width at Half-Height (FWHH) broader than the resolution
setting are distinguished.
Resolution
Band Separation = FWHH

= 4 cm-1

Absorbance
= 2 cm-1

= 1.25*FWHH

= 1 cm-1

2140 2120 2100 2080 2060 2040

Wavenumbers (cm-1)
IR spectrum of CO(g) band FWHH ~1.5 cm-1, band spacing ~5 cm-1

Resolution is the ability to distinguish two closely spaced bands. According to the FWHH
criterion, two bands with identical intensity and FWHH are considered resolved when the
spacing between the lines is greater than the FWHH.*
*Griffiths, P. R. and De Haseth, J. A., eds. Fourier Transform Infrared Spectroscopy, Wiley: New York 1986.
To distinguish between closely spaced bands, the resolution setting must be less than or equal
to the separation of the bands.
In solids and liquids, many features are naturally overlapping and improving the resolution of
the analysis will not separate these features.

Experiment Setup 5
Resolution (cont.)

ƒ The ability to accurately depict the band shape


• Band width and height can be distorted if system resolution is not
set correctly, affecting quantitative determinations
• The loss of intensity will effect the low level detection limit of a feature
• Sensitivity to small variations in band
intensity are diminished

• Qualitative determinations
can be affected
• Search library resolutions should
match sample resolutions
• Visual interpretation relies on recognition
of band positions and band shapes

A band is detected if the resolution (in cm-1) is less than or equal to the band FWHH.
Therefore, if the resolution were setting for 4 cm-1, a band with a FWHH of 2 cm-1 would not
be resolved and identified.
Beyond simple detection, the true shape of the band is accurately depicted if the resolution
setting is less than 1/7 to 1/10 of the band FWHH.
System resolutions less than this criteria will cause the bands to become broader and less
intense.
The FWHH of a band is a feature of the band in much the same way the position is.
Using better resolution than necessary does not enhance the peak shape further, instead
results in an increase of noise, degrading the quality of the spectrum.
In solids and liquids, resolution better than 4 cm-1 is rarely needed. Gas samples require
higher resolution due to the narrower bands.

Experiment Setup 6
Resolution and Moving Mirror Travel

When a higher resolution is selected, (lower number), the mirror must move farther. This idea
is demonstrated in this example.
Three racing cars that are traveling at three different speeds represent signal with different
frequencies. The red car at the top is traveling at the lowest speed. Two cars at the bottom are
traveling at similar faster speed, but one at the very bottom is slightly faster. If the mirror were
moved only to the distance of the first marker, separation would occur between the lowest
frequency signal and higher frequency signals. But higher velocities still have not separated.
By running the race farther, it is possible to see that eventually cars with the middle and
highest velocities can be separated. This is because the small, undetectable difference at the
first marker is enhanced as the mirror moves further.

Experiment Setup 7
Resolution and Moving Mirror Travel

Increase in Resolution
• Increases Distance mirror moves
• Increases Time required for data acquisition
• Increases Instrumental Noise
• Decreases Throughput due to aperturing of the beam for collimation

ZPD 8 cm-1 4 cm-1 2 cm-1

An increase in the distance the mirror moves increases the time of the experiment, increases
electronic noise and decreases overall intensity throughput because the beam must be
collimated using an aperture.
The relationship between mirror distance from ZPD and resolution is
Resolution = (2 * Mirror distance)-1
Resolution can be reduced but can not be increased at post-collection. Select a resolution that
produces acceptable spectra without overly increasing data acquisition time. Higher resolution
can provide invaluable information in certain applications.
Most commercial libraries have a resolution of 16 or 8 cm-1. There are newer commercial
libraries with a resolution of 4 cm-1. For most applications, 4 or 8 cm-1 is typically used.

Experiment Setup 8
Final Format

Final Format on the Collect tab in the Experiment Setup dialog box determines the units used
for the collected data. The following table shows the available final format settings and the
units used by each format:

Final Format X-Axis Unit Y-Axis Unit


Interferogram data point volt
Single Beam wavenumbers Single Beam
%Transmittance wavenumbers %Transmittance
Absorbance wavenumbers Absorbance

Experiment Setup 9
File Handling Options

To save files automatically enable Save Automatically. You may choose to enter a 4 character
alpha-numeric base file name. Note the location of the “autosave” subdirectory. Recall that
using Edit | Options | File Tab and setting intial autosave subdirectory will allow you to change
the destination subdirectory. Automatically saved files will increment up. In this example,
demo0001.spa, demo0002.spa, demo0003.spa etc. OMNIC always looks for the highest
number to increment, even if you have deleted files from the subdirectory with lower numbers.
Turn on Save Interferograms if you want to include the associated reference and sample
interferograms when a spectrum is saved. The interferograms will be saved in the same file as
the spectrum. The interferograms will be included whether you are saving spectra
automatically or saving them by using Save in the File menu.
Saving interferogram data lets you reprocess a spectrum in case you want to restore the
original data.
When you reprocess the spectrum, you can use a different reference or change some of the
parameter settings used for the transformation. With the abundant storage space available in
current computer’s, it is a good idea to always save interferogram data so that full
reprocessing can occur. An interferogram is raw data that can be processed.

Experiment Setup 10
Background Handling Options

Collect Before Every Sample Most commonly Used


Collect After Every Sample Microscope date collection when
aperture size limits energy
Collect After Specified amount Well purged environments when fast
of time (0 = infinity) data collection is paramount
Collect using specific named Not recommended but useful if
background on hard drive background is well defined

Remember first to match experimental conditions between background collection and sample
collection. Choose appropriate background handling option for each experiment.
Collect background before each sample: This more closely pairs the energy of the background
and environmental contamination to the sample data collection.
Collect background after each sample: This allows some adjustment to be made between
sample and background collection. In the example of the microscope, the aperture is set
based on the sample size and the stage moved to background material to collect background.
Collect background after __ minutes: (setting this to 0 means a new background is only
needed when experimental parameters change or OMNIC is closed). This allows the user to
determine when and if a new background is required. Setting it to a time value reminds the
user to collect a new background periodically.
Use selected background file: If you have collected a background and saved it to your hard
drive as a file with .spa extension you may select this option. However, this can be a
dangerous practice if not changed periodically!

Experiment Setup 11
What does a background represent?

Background- Purged with nothing in Sample Compartment Background - Diamond ATR

Background - Nothing in Sample Compartment, Purge Line Contamination

The single beam of a background is used to ratio against the single beam of a sample to
produce a spectrum (either in transmission or absorbance). It represents a measurement of
the maximum throughput available at each and every wavelength that might be absorbed by a
sample. Because of this, it is important that the background collection represent the
experimental conditions used for sample data collection.
For example, when analyzing a sample with an ATR accessory, you would first clean the ATR
crystal and, with NOTHING on the ATR crystal analyze the background. This will produce a
single beam of the background which represents the maximum energy available using your
ATR crystal. When a sample is placed on the ATR crystal, some of the energy is absorbed by
the sample and is never detected. We know which frequencies and how much of each were
absorbed by the sample by knowing the original amount of energy available (the background).
The background can be thought of as the spectrum of the instrument (and accessory) and
needs to be removed from the instrument plus sample spectrum to see the unique sample
spectrum.
It is tempting to think that the background is subtracted from the sample. This is not the case.
It is ratioed.

Experiment Setup 12
Atmospheric Suppression

Atmospheric Suppression is designed to remove the presence of water and CO2 vapor while
you are collecting data, as opposed to subtracting it from final data. To use this feature you
must load and unzip all the associated quant files that came with OMNIC. Then enable this
feature.
This is considered as a collection parameter and cannot be performed in post-processing as a
correction. To post-collection process the spectrum and remove the water vapor and carbon
dioxide contributions, the H2O and CO2 correction should be used in the Process | Other
Corrections Menu.
When performing quantitative analysis it is probably best not to enable automatic atmospheric
suppression as it will add one additional variable to your method.

Experiment Setup 13
Preview Data Collection

Use preview data collection function if you would like to spend some time repositioning the
sample prior to collection (nice for ATR and Microscope samples). If you use it, be sure to set
an appropriate Background Handling technique (after a fixed amount of time) so that you see
“ratioed” data. Also, do NOT forget to hit the Start Collection Button in the upper right hand
corner of the screen when you are ready for data collection.

Experiment Setup 14
Experiment Description and Title

The experiment title will appear on the experiment title drop down menu in OMNIC. It is good
practice to make the title and the description meaningful before saving.
Multiple experiments may be saved and added to the Experiment drop down list. The only way
to permanently remove an experiment from the list is to delete the experiment file from your
computer hard drive.

Experiment Setup 15
Bench Tab - Setting Spectral Range

Use the Bench Tab of Experiment Setup to set Spectral Range. Setting the appropriate
spectral range for your experiment is important for things like improving the quality of a
commercial library search, or, more important, developing your own spectral library.
Note: When the Smart™ Accessory is inserted into the sample compartment an experiment
file is automatically loaded changing all the collection parameters. You should review these
settings to be sure the meet the needs of your sample.

Experiment Setup 16
Gain

The Gain parameter on the Bench tab in the Experiment Setup dialog box determines how
much the detector signal is amplified electronically. You can set Gain to 1, 2, 4, 8, or Autogain.
The Autogain setting allows the system to optimize the gain automatically. Use a gain setting
that results in a signal intensity of less than 20 volts peak-to-peak +/- 10 volts min/max. Select
the desired setting from the drop-down list box.

Experiment Setup 17
Setting Gain

ƒ Gain Attenuates Electronic Signal prior to Detector


ƒ Detector analog to digital converter becomes saturated
at ±10 volts

Gain = 1.0

Gain = 2.0

Gain = 4.0

ƒ Autogain is recommended for qualitative analysis Gain = 8.0

ƒ Use fixed gain setting for aligning an accessory or microscope

Increasing gain increases the signal from the detector. When the gain is improperly set the
detector electronics can saturate. This occurs when the interferogram measurement is +/- 10
volts (see the Max and Min measurement on the top of Bench Tab).
For qualitative analysis the gain should be set to Autogain. This allows the electronics to select
the most appropriate gain for the experiment. When you are doing sensitive quantitative
analysis you should determine the best gain for your experiment and run using a fixed gain
value.
Because the interferogram display is “live”, it may be used as a tool to monitor energy
throughput while aligning an accessory or a microscope. You should select a fixed gain value
to prevent the interferogram from jumping between gain values during alignment.

Experiment Setup 18
Velocity
• Velocity controls the speed of the moving mirror (cm/s)
• Setting is dependant on type of detector
-For DTGS (room temp), slower (~0.6 cm/s)
-For MCT-B, MCT-A, and MCT-A* (liquid N2 cooled), faster (~1.8 cm/s)

The Velocity parameter in the Bench tab determines the velocity of the moving mirror in the
interferometer. The default value is determined by the detector type and is set when you select
a detector using the Detector parameter. Select the desired setting from the drop-down list box
at the right end of the Velocity row.
Using a faster velocity allows you to collect more scans in a given amount of time; however,
using a velocity that is faster than the default setting will produce a smaller signal intensity.
Using a slower velocity increases the time required for an individual scan, but that does not
mean the total measurement time needs to be longer. The stronger signal obtained (with some
detectors) at the slower velocity can allow you to collect fewer scans, resulting in a shorter
measurement time and better quality spectra.
The velocity is the speed with which the moving mirror moves inside the interferometer. It is
constant on both the forward and reverse stroke. Slowing the mirror down while using a DTGS
detector will improve sensitivity. However, if you are using an MCT detector you may collect
with a higher velocity. This is advantageous because very often experiments that use an MCT
detector are already “low energy” and the number scans is increased to improve the signal to
noise ratio. Increasing the velocity of the moving mirror will decrease the amount of time
required to collect data.

Experiment Setup 19
Aperture

The Aperture parameter on the Bench tab in the Experiment Setup dialog box allows you to set
the size of the optional adjustable aperture to any value from 0, the minimum size, to
approximately 150, the maximum size.
To change the setting, double-click the table cell to the right of Aperture. Then type a value or
click the up and down arrow buttons to the right of the value.
The Aperture parameter is dimmed if the aperture is not installed.

Experiment Setup 20
Quality Tab

To display a category of checks or all the checks on the Quality tab, select the appropriate
option to the right of Select View.
If you want any of the spectral quality checks to be performed when you collect spectra using
the current experiment, turn on Use Spectral Quality Checks near the top of the dialog box.
This makes the various checks available for you to select. If you don't want any checks to be
performed, turn off the check box.
Spectral Quality checks are designed to look for conditions which exist during data collection
and test for the selected feature/error. If the test fails (or nears failing) the Collect Status
indicator (lower right hand corner of the OMNIC Collect window) will turn from a green check
mark to yellow flashing or to red “x”. This indicates that one or more of the quality parameters
is outside limits.
If you choose to use Quality checks you must first set each parameter with the appropriate
sensitivity level. For example, if you want to check for the presence of CO2 vapor, first set the
sensitivity to 100. Collect data. Using View Confirmation Status you can determine the level at
which CO2 as a vapor was recorded. If, in fact, there was an acceptable amount of CO2 in your
environment then you must set the sensitivity setting just below this number. In this way, the
collect will “pass” (a green check mark appears at the Collection Status at the lower right hand
corner).

Experiment Setup 21
Spectral Quality Collection - “Collect Status errors”

When OMNIC performs a check and detects a problem, the Collect Status indicator is
displayed in yellow or red. You can click the indicator (or click the View Collect Status button at
the end of data collection) to see a summary of data collection problems encountered during
the collection and other information about the collection.
In this example there were totally absorbing peaks present, as well as partially absorbing. This
is not a surprise when analyzing polystyrene. The sensitivity values should be reset to lower
numbers for the Collect Status to “pass”.

Experiment Setup 22
Advanced Options – Zero Filling
Artificially improves resolution of spectrum by adding additional data points as zeros
prior to Fourier Transformation

I(δ )= ∫ β( ν)co s2πνδdν
−∞

Advanced options should only be changed if you are confident in your choices. Remember that
a simple right click and choosing discussion on the window that pops up will bring a detailed
explanation of everything related to the window.
The two options changed most frequently in this tab are the Apodization and Phase Correction.
To mathematically improve the data spacing frequency based data, zeros may be added to the
Fourier Transform. One level of Zero Fill adds a number of data points to the end of the
interferogram and sets them to zero. This is then transformed and the results is to add an
interpolated data point in between every real data point in the spectrum.
This is useful in enhancing the peak shapes in the resulting spectrum, allowing for better
interpretation of the information. The spectrum data is not changed by adding zeros and this
should not be used as a substitute for increasing the resolution to meet the needs of the
sample analysis.
A second level zero fill adds a second set of data points to the end of the interferogram. This
will have the effect of inserting 3 interpolated data points in between each real data point in the
frequency spectrum after the Fourier transform, further enhancing the peak shapes.
If you need to collect higher resolution data, it is better to experimentally improve resolution
than artificially.

Experiment Setup 23
Apodization

Apodization removes peak side lobes that can occur because the interferogram is not an
infinite set of data. The apodization types described in the following table are available. Collect
your sample and reference spectra using the same apodization type.
The two most commonly used apodization functions are Happ-Genzel and Triangular.
Triangular apodization is used during the 100% line noise test with infrared microscopes.
Happ-Genzel: This setting is the best choice for most applications. It suppresses side lobes
more effectively than the triangular apodization but with more reduction in resolution than the
triangular and boxcar type apodizations. If you are measuring condensed-phase samples, use
Happ-Genzel apodization.
Triangular: Mathematically weights interferogram data to reduce ringing effects (side lobes),
resulting in lower resolution than that obtained with the boxcar type apodization but higher than
that obtained with the Happ-Genzel apodization.
The other apodization types available are described in the help file accessed by right clicking
on the item of interest.

Experiment Setup 24
Apodization

Mathematically applies limits of integration to Fourier Transform


because we are not collecting data from +/- infinity

Prior to the Fourier Transform, limits of integration must be identified (because we are not
collecting data from negative to positive infinity). The limits are found by applying an
Apodization function to the data. Each apodization function is the description of a
mathematical calculation performed on the interferogram prior to the Fast Fourier Transform.
(ex. Boxcar or Triangular all describe mathematical formulas).
These functions serve to smooth the transitions at the ends of the interferograms and eliminate
the artifacts that could be introduced due to the abrupt discontinuation of the real data in the
interferogram.
From the above picture, it can be seen that more attenuation is applied to regions that are far
from the center burst. These regions have also been shown to contain the higher resolution
information in the data. The application of an apodization function then has the effect of
lowering the resolution slightly in the final spectrum.
Happ-Genzel is recommended for ordinary data collections. Triangular may be better for noisy,
low energy experiments (like working with the a microscope). Whichever you choose, be
consistent. Apodization function impart their own unique peak shapes to the final data. This
can cause problem in analysis and may result in misleading interpretations or quantitative
determinations.

Experiment Setup 25
Advanced Options

Power Spectrum: Always produces a spectrum that is positive. In this correction the power
equals the square root of the sum of the squares of the real and imaginary parts of the Fourier
transform. This is the normal setting for Raman data.
Mertz: Uses the Mertz algorithm to calculate the phase-corrected spectrum.
For more information on the Mertz and Power Spectrum corrections, read
Transformations in Optics by L. Mertz, published by John Wiley and Sons, New York, 1965.
de Haseth: Phase corrects vibrational circular dichroism (VCD) spectra. These spectra can
have both negative and positive peaks, so the correction is designed to accommodate
negative spectral features. For more information, see the article titled "Phase Correction of
Vibrational Circular Dichroic Features" by Colleen A. McCoy and James A. de Haseth in the
Journal Applied Spectroscopy, Volume 42, Number 2, 1988.

Experiment Setup 26
Phase Correction

Corrects the phase angle term of the Fourier Transform


where distortions to the interferogram occur as a result of
noise or laser sampling effects.
Makes the interferogram symmetric around ZPD
-Use Mertz Correction-

Phase correction corrects for any distortions around the centerburst (ZPD) caused by noise or
other sampling effects. It is possible that “imaginary” (-10.5 or i) data is introduced into the
mathematical calculations and this correction removes this effect. The result is that it makes
the interferogram more “symmetric” about the centerburst. Mertz is always recommended for
FTIR data.

Experiment Setup 27
Configure Tab

Configuration tab contains Source Rest Mode, Bench, and Filter Wheel configuration options.
The source can be set to rest (not turned off, but set at lower power) at scheduled times.

Experiment Setup 28
Open, Save and Save As

Experiment files have the .exp extension. Several pre-existing experiments are loaded with
your software. They are located in the OMNIC\Params subdirectory. If you use a pre-existing
experiment be sure to check all settings to ensure they are appropriate for your data collection.
When saving an experiment it may be set as default. This is the experiment which is
automatically loaded when OMNIC is launched (assuming that OMNIC log in feature is not
enabled). You may also write protect experiment files so that they can not be overwritten by
selecting Read Only.
On the lower left side of the Save As Dialog box there are several check boxes. These tie
various collection parameters together as part of your experiment file. Selections made in
Quality, Advanced, and Configuration tabs (discussed later) are also saved with experiment
file.
Note: If the Search checkbox is selected, selected library setup with your experiment is saved
as a part of the experiment file. This function is covered again in the Library Setup section of
this course.

Experiment Setup 29
Diagnostic Tab
Performance Indicator for Power Supply, HeNe Laser, Source, Electronics, and Detector.
Red line across the figure indicates a problem.

Reference signal from the laser


diode for trouble shooting

Freeze: Freezes the interferogram in the live display


Align: Aligns the interferometer to maximize the throughput
Reset Bench: Repositions the ZPD
Verify Smart Accessory: Displays which Smart™ accessory is installed

Above the live display are several icons that can be selected to check the status of the
following spectrometer components: Power, HeNe laser, White Light, Electronics, and
Detector. If an indicator is continuously marked with a red diagonal line for at least one minute,
there may be a problem with the corresponding component in the spectrometer.
You can use the Align button to perform an automatic alignment of the interferometer.
If the interferogram peak has drifted from its normal location, you can click the Reset Bench
button to reposition the peak. If you find that the interferogram peak in the live display tends to
drift from its normal location, turn on Reset Bench At Start Of Collection on the Advanced tab
in the Experiment Setup dialog box. This repositions the peak before data collection starts.
Periodically you should Align your instrument. When you select this button the hardware will
automatically perform this task. It is important that the sample compartment be clear of all
accessories when this task is performed. By adjusting the position of the beam splitter the
amplitude of the interferogram can be maximized.
Reset Bench will flush the electronics of the instrument. This may used in establishing
communication with the instrument.

Experiment Setup 30
100 % Transmission Line Noise Test

A transmission spectrum of the bench with nothing in the beam path is


taken to evaluate noise; therefore, the performance of spectrometer.

10 10 100

%Transmittance
Single Beam

Single Beam
÷
8 8
6 6
99
4 4
2 2
98
4000 3000 2000 1000 4000 3000 2000 1000 4000 3000 2000 1000
Wavenumbers (cm-1) Wavenumbers (cm-1) Wavenumbers (cm-1)

Blank
= Noise
Blank

The 100% Transmission Line spectrum is used to evaluate instrument noise. It is the ratio of
two single beam spectra, with nothing in the sample compartment. This, theoretically, should
produce a straight line. Any instrumental noise may then be calculated using this data.

Experiment Setup 31
100% Transmission Line Collection Parameters

Main Bench Microscope


Scans 64 200
Resolution (cm-1) 4 4
Apodization Happ-Genzel Triangular
Final Format % Transmission % Transmission
Correction None None
Spectral Range (cm-1) 2200-2100 2600-2500

Whichever parameters you choose, always be consistent!

Thermo Fisher Scientific recommends parameters listed above to evaluate the performance of
your instrument over time. Unless you have developed a test for an accessory, be sure to
always clear the sample compartment of any accessories. Whichever collection parameters
you choose, be consistent so that all results obtained can be compared. Final format can be
changed later in OMNIC. Different apodization function can be applied post-collection if
interferograms are saved.

Experiment Setup 32
100% Transmission Display Limits and Noise Result

Set X-Limits
to 2200-2100 cm-1
or 2600-2500 cm-1

Select a display limit range either 2200 to 2100 or 2600 to 2500 cm-1 to ensure that water and
CO2 vapor does not interfere with the noise test.
View | Display Limits
Noise is easily calculated in OMNIC by selecting
Analyze | Noise
The published specification on peak-to-peak (p-p) noise values vary between spectrometer
models. A value less than 0.1 should be expected. Thermo does not recommend the use of a
root mean squared (rms) noise value for this evaluation. You may track p-p noise in your lab
notebooks and watch for trends. If the p-p noise begins to drift up significantly, this may
indicate a problem with the bench. Be sure to align the bench periodically. If a problem occurs,
align the bench and then run this test again.

Experiment Setup 33
Experiment Setup - Review

Collect Tab
Setting Number of Scans and Resolution
Final Format
Saving Files and Interferograms
Background Handling Options
Atmospheric Suppression
Preview Data Collection
Experiment Descriptions and Titles
Bench Tab
Setting Spectral Range, Gain, and Velocity
Quality Tab
Advanced Tab
Zero Filling, Apodization, and Phase Correction
Configure Tab
Diagnostics Tab
Align and Reset
100% Transmission Line Noise Test

Experiment Setup 34

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