Mantis 5000 Specifications

Mantis 5000 Specifications
Diffuse Reflectance Accessory (external)
Note: This document is also available in PDF format for improved print quality.
PDF files are stored in the "\Manuals" folder on the Help & Videos CD-ROM.
For the Cary 4000, 5000 and 6000i
Part Numbers: External DRA 900: 00-100818-00
External DRA 1800: 00-100819-00
External DRA 2500: 00-100820-00
Last updated:
Installation category II
Pollution degree 2
Safety class 1 (EN 61010-1)
Overvoltage category I
Refer to the Safety section of the online Help for an explanation of the warnings and
cautions used in this document.
Table of Contents
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Introduction
Theory
o Reflectance measurements
o Transmittance measurements
o Factors affecting accuracy or precision
Description of the accessory
o Accessory design
o Integrating sphere
o Optics
o Detector chamber
o Reflectance standards
o Transmission sample holder
Specifications
Getting started
o Unpacking
o Installation
o Alignment
o Error checks
o Attachment options
o Transmission Port Cuvette Holder
o Center-Mount Sample Holders
o Small spot kit
o Polarizer
o Double aperture accessory
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•
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Operation
o Routine DRA installation
o Removing the DRA from the instrument
o Collecting baseline scans
o 8°/h Reflectance Factor Measurements (Comparison Method)
o 8°/d Reflectance Factor Measurements (Comparison Method)
o 8°/h Reflectance Factor Measurements (Single Beam Mode)
o 0°/h Transmission Measurements (Comparison Method)
o 0°/d Transmission Measurements (Comparison Method)
o Variable Angle Reflectance Measurements (Center-Mount Sample
Holder)
o Absorbance Measurements (Cuvette Center-Mount Sample Holder)
o Using the Small Spot Kit
o Small Sample Masking Techniques
o Applying a Nitrogen Purge
o NIR reflectance measurements (Cary 5000 only)
o Specular-only reflectance measurements
Measurement calibration and corrections
o Calibration
o When should I perform a Calibration?
o Diagnostic scans
ƒ Energy scans
ƒ Baseline scans
ƒ Other scans
Maintenance
o Cleaning and Inspection
o Energy Scans
o Light Trap Zeroline Scan
o Mirror Cleaning Procedure
Standards
Troubleshooting
Spare parts
References
Alignment targets
Sample Mounting Kits
Introduction
The traditional use of the spectrophotometer is to measure the absorbance or transmission
of a clear or translucent liquid or solid. Typically UV/VIS/NIR spectroscopy applications
include reaction kinetics, quantitative analysis or the identification of the chemical
constituents in a substance. The measurement of reflectance offers an added dimension to
the spectroscopy capabilities of your spectrophotometer, the analysis is no longer limited
to the portion of the beam that penetrates the sample. Accordingly, the analysis is no
longer limited to samples that are clear or translucent. The DRA provides the means of
measuring absorbance or transmission of opaque, turbid and reflecting substances.
Figure 1. The external DRA.
Figure 2. The external DRA viewed from
the back.
There are three versions of the diffuse reflectance accessory that operate over different
wavelength ranges.These are specified below. While all of the following variations are
available, the configurations indicated by ticks in the table below offer optimal operation.
(External DRA
900)
(External DRA
1800)
(External DRA
2500)
Cary
4000
Cary
5000
Cary
6000i
The Varian 900, 1800, 2500 External Diffuse Reflectance accessory (DRA) consists of a
150 mm diameter integrating sphere. The sphere is easily installed in the sample
compartment of the instrument and features an inbuilt high performance photomultiplier
tube (PMT). The DRA also has a Lead Sulfide (PbS) or InGaAs detectors which become
active Varian 2500 External DRA. The coating is Polytetrafluoroethylene (PTFE), which
exhibits NIR performance that is superior to traditional coatings(1), whilst maintaining
UV-Vis performance.
Warning
If the DRA is not used in the manner specified by the manufacturer, the protection
provided by the accessory may be impaired.
Theory
Reflection consists of two components: specular and diffuse. Specular reflectance is the
mirror-like reflection off a sample surface. Diffuse reflectance occurs when the surface
reflects light in many different directions, giving the surface a matt finish.
Figure 3: The two components of reflection: specular and diffuse reflection. n represents
the surface normal, an imaginary line at 90° to the sample surface.
Traditionally, the accessory used to measure diffuse reflectance is the integrating sphere.
Applications include characterizing solar materials, color measurement and
characterization, and obtaining reflectance spectra of a painted surface. Integrating
spheres have also proven ideal for measuring the transmission of turbid, translucent or
opaque refractory materials where standard techniques proved inadequate due to loss of
light resulting from the scattering effects of the sample. Samples which distort the beam
of the instrument, such as a lens, can also be studied with the Diffuse Reflectance
accessory.
The DRA is an integrating sphere accessory that replaces the sample compartment of the
spectrophotometer instrument. An integrating sphere is a hollow optical device, either
constructed from or coated internally with a white diffusing material and fitted with the
same detector configuration as the host spectrophotometer. The coatings used in an
integrating sphere usually depends on the wavelength capabilities demanded by the
reflectance application.
The integrating sphere configuration offers some distinct advantages over the standard
sample compartment. The changes made in sample beam and reference beam geometry
on your accessory do not compromise the transmission and absorption measurement
capabilities already inherent to the spectrophotometer the traditional sample transmission
and absorbance measurements can be performed in the same manner, with or without the
DRA. Because of the geometry of the integrating sphere, it has the ability to collect most
reflected or transmitted radiation, remove any directional preferences, and present an
integrated signal to the detector.
The DRA accessories each include an optical bench composed of double beam transfer
optics in combination with a six-inch (150 mm) diameter integrating sphere. The
integrating spheres are machined from SpectralonTM a highly diffuse reflectance
material. The accessory is equipped with a movable mirror in the sample beam optics to
allow the beam to be focused at the transmission, reflectance, or centre-mount sample
positions. This feature adds versatility for measuring various size samples. The external
DRA accessories are designed to perform reflectance, transmission, or absorbance
measurements of diffuse, specular, or mixed samples. The Scan application of the Cary
WinUV software is usually used when operating the accessory.
Reflectance measurements
First, a baseline is recorded with the PTFE reference disk covering the reflectance port.
The sample is then mounted over the port and the reflection off the sample surface is
collected by the sphere. The reflectance is therefore measured relative to the PTFE disk.
This is the ’substitution’ method.
The total (diffuse and specular) or the diffuse-only reflectance may be measured by using
either the specular plug (specular included) or the light trap (specular excluded). The
specular component may be calculated from the difference of these two, or the Cary
Absolute Specular Reflectance Accessory (SRA) may be used to give an absolute value
of the specular component.
A variety of sample types and sizes may be used with the accessory, in conjunction with
different sample holders. For powders, pastes or other material requiring a sample
container, a powder cell is available for use in the DRA.
If only very small amounts of powder or paste are available, or if measurements
extending beyond the range of 250–2500 nm are required, the DRA cannot be used. The
'Praying Mantis' accessory (P/N 00 100469 00) is used for these measurements.
Transmittance measurements
Figure 4: Collection of scattered light by an integrating sphere. Io = incident light, Is =
scattered light.
In order to perform useful measurements on scattering samples, it is necessary to collect a
high proportion of the scattered radiation. The integrating sphere is a highly efficient
collector of scattered radiation. Because of its design, the Diffuse Reflectance accessory
overcomes many of the problems associated with measuring turbid or scattering samples,
which include sloping baseline, poor signal-to-noise ratio and high background
absorbance.
Whilst the DRA should be used when measuring the transmission of opaque or diffusing
solid samples, the accessory may also be used when measuring turbid liquids.
Because the cuvette is located so as to be part of the wall of the sphere, a greater
proportion of the scattered radiation transmitted by the sample is collected by the sphere,
as shown in Figure 3 above.
With the PTFE reference disk in position, a sample is placed in the cuvette, and light is
passed through the sample.
Factors affecting accuracy or precision
Below are the major factors that may affect the accuracy of measurements when using the
DRA.
Aperture area/total surface area ratio
Some of the reflected light escapes through the ports. This has the effect of reducing the
signal to noise ratio, and thus the precision of the measurement.
The Commission Internationale de l’ Eclairage (CIE) recommendation is a ratio of <10%.
This figure is < 10% for the Cary External DRA.
Coating non-uniformity, ageing, or contamination
This accessory has been coated with PTFE via a unique process that ensures both a
uniform coating on the inside of the sphere and the correct powder density. PTFE is
durable, and does not yellow. The reflectivity of the PTFE is above 96% between 200–
2500 nm, and greater than 99% between 350–1800 nm. The sphere will maintain its
reflectivity indefinitely if not subjected to smoke or other contaminants. Contact with
plastic materials may also contaminate the coating.
Incorrect sample placement
Theory assumes that the sample placement will coincide with the inside of the sphere
wall. The sample is normally placed at a port on the outside of the sphere wall. Spacing
between the sample and the sphere wall can lead to large errors due to loss of reflected
light.
Figure 5: Some of the wide-angle scatter is lost when there is a space between the
sample and the sphere wall
Sample recess
Theory assumes that the sample is placed coincident with the inside of the sphere wall,
however the sample is placed against the outside of the sphere wall. The porthole edges
have a finite thickness, and some part of the beam reflected at wide angles may be
intercepted by the sphere wall.
Figure 6: Some of the wide-angle reflection is intercepted by the sphere wall
The edges of the reflectance port are feathered to reduce this error.
Reference beam attenuation
Reference beam attenuation is most useful when the accessory or sample in the sample
beam attenuates the light beam considerably. In such situations, attenuation of the
reference beam will increase noise and considerably increase the dynamic range of the
instrument, as the detector is not then ’seeing’ two dramatically different signals. Clips are
provided at the reference beam window for this purpose. Metallic mesh screens are
recommended if reference beam attenuation is required (part number: 0110677500).
Stray light
If the irradiating beam overfills the reflectance port, a proportion of sphere wall
reflectance is mixed with that of the sample. This gives a high reading if this is not
consistent between the baseline and the sample measurement.
Gloss trap error
Gloss trap error is produced when the gloss trap is unable to completely absorb the
specular component. In the measurement of diffuse-only reflectance, a ’gloss trap’ is often
used to absorb the specular component. Gloss traps are typically glossy black pyramidal
light traps, matt black-coated cavities, or razor blade Fresnel light traps. However, the
reflectance of many samples has broadened the specular peaks which cannot be excluded
by standard sized light traps.
Differences between the standard and sample
It is important that the reference material be of a similar reflectivity and have similar
properties to the sample. Otherwise large errors can be introduced, if for example a
poorly reflecting material is measured relative to a highly reflective PTFE reference
plate. The table below lists the appropriate reference materials that are recommended for
use.
Surface type
Reflectivity
Reference
Matt
High
PTFE reference plate
Matt
Low
Labsphere diffuse
reflectance standards
Glossy
High
PTFE reference plate
Glossy
Low
NIST SRM 2021
The Troubleshooting section contains information on the available reference surfaces.
Figure 7: Highly diffuse samples are measured against a flat PTFE reference plate
Inaccuracy in the standard
If the standard material used to calculate a value is not accurate, this will hamper the
determination of the reflectance of the sample. Great care must be taken to keep reference
materials clean and unscratched.
For a detailed discussion on the factors affecting the measurement of diffuse reflectance
and transmission with integrating spheres, refer to reference (2).
Description of the accessory
Accessory design
The DRA accessories are designed specifically to measure the reflectance or transmission
of solids, liquids, powders, or other small objects that can fit at the transmission or
sample reflectance ports. Except for the sphere detectors, the construction of each version
of the DRA is identical. Basic components of the accessory include the base plate,
integrating sphere, optics chamber and detector chamber. The basic components are
illustrated in the figure below.
Figure 9: A schematic view of the external DRA.
The optics chamber contains the transfer optics that direct the spectrophotometer beams
to their final destinations. The integrating sphere collects and measures the radiation
transmitted or reflected from the sample surface. A removable cover fits over the DRA to
provide a light-tight operating environment. The sample reflectance and reference ports
each are fitted with a separate magnetic port cover. The purposes of the covers are to
reduce the potential for stray light when the accessory is in use and to keep the
integrating sphere and standards clean when not in use.
Beam paths within the accessory are illustrated in the next figure. Light entering the
accessory is directed to one of two entrance ports on the sphere: the reference beam and
sample beam entrance ports. The sample beam entrance port is usually called the
transmission port.
Figure 10: The optical design of the external DRA.
Integrating sphere
An integrating sphere is an optical device used to collect and measure electromagnetic
radiation. The radiation sampled by the DRA integrating sphere is provided by the
spectrophotometer reference and sample beams present inside the sample compartment.
Upon entering the sphere, the light strikes the sample surface and the highly reflective
walls of the cavity, undergoing many diffuse reflections. Radiation trapped inside the
sphere cavity can dissipate by a combination of three ways. Most of the light eventually
is absorbed into the sphere walls. Some of the light exits the cavity through one of the
empty ports, and a small portion of the trapped radiation strikes the active surface of the
sphere detector. A steady state radiant flux distribution is established almost
instantaneously within the sphere and remains as long as the beam source is active. All
integrating spheres possess one unique property with regard to a steady-state flux: the
radiance all along the wall surface of the sphere is uniform and proportional to the flux of
the source input. The sphere detector samples the radiance at the wall surface and relays
the detector signal to the spectrophotometer for processing.
Optics
The optics chamber houses the transfer optics of the DRA accessory that direct the
spectrophotometer reference and sample beams to their respective ports on the integrating
sphere. The sample beam is the rear beam in the accessory. Mirrors labelled M1, M2 and
M3 guide the sample beam through the sample transmission port of the integrating sphere
and onto the sample reflectance port at an 8° angle of incidence. Mirrors M4 and M5
direct the reference beam through the reference beam entrance port onto the reference
port.
Figure 11: Mirror M1.
Figure 12: Mirror M5.
Mirrors M1 and M5 are fixed mounted mirrors that are adjustable in the vertical and
horizontal planes. Mirror M1, illustrated in the figure above, holds a flat mirror that helps
direct the instrument sample beam into the integrating sphere transmission port. M5 holds
a concave mirror surface that reflects the reference beam into the integrating sphere. The
design of mirror M5, shown in the figure below, is very similar to mirror M1. The fixed
mirrors are mounted to the base plate by two M5 bolts that can be adjusted using a 4 mm
hex wrench. All mirror surfaces are coated with a Al/MgF2 thin film.
Mirror M2 is a pivoting mirror assembly that positions a flat mirror surface into the
sample beam path, directing the beam onto the movable mirror, M3. The mirror mount
pivots about a fixed point. To rotate the mirror assembly horizontally, loosen the two
screws shown in the figure and rotate the floor adjustment with a large flathead screw
driver. To adjust the mirror surface vertically, use a 3 mm allen wrench.
Figure 13: Mirror M2.
Figure 14: Mirror M3.
Mirror M3 is a spherical mirror that condenses the sample beam onto the target sample.
The mirror can be mounted at any of three different positions on the base plate of the
DRA. These positions correspond to the transmission port, centre mount sample holder
and sample reflectance port, and are labelled "T", "C" and "R" respectively. M3 features
a knurled mounting screw for convenient installation and removal as well as the standard
vertical and horizontal adjustments. The mirror is illustrated below.
Note
If you move M3 to a different position, you will need to realign the transfer optics.
Mirror M4 directs the raw reference beam through the collimating optic and onto mirror
M5. The mirror mount is constructed in a manner to prevent stray light scattered from
mirror M1 from reaching the integrating sphere. The mirror has a single adjustment in the
vertical plane. If beam adjustment is required in the horizontal plane, loosen the cap
screws at the base of the mirror mount and rotate the device slightly in either direction.
Figure 15: Mirror M4.
The accessory is shipped from in a protective wooden case. The accessory should be
stored in the case when the DRA is not being used.
Detector
The detector chamber attaches to the bottom of the base plate and is located directly
underneath the integrating sphere.
Reflectance standards
The DRA is shipped with three Spectralon reflectance standards. If a standard is
calibrated, a calibration certificate that lists the reflectance data across the wavelength
spectrum will be included. The typical reflectance values may be very close to the actual
spectral reflectance of the standards, but the typical data is not traceable to NIST. The
uncalibrated standards should be loaded at the reference and sample ports to protect the
internal surfaces of the sphere when the accessory is installed but not in use.
Cleaning instructions for uncalibrated reflectance standards are provided when the
standards are purchased. Calibrated standards can be returned to Labsphere for
recalibration yearly, or whenever the reflective surface of the standard is soiled or
damaged.
You may want to convert the reflectance values for your standards to a file compatible
with Cary WinUV. This can be accomplished by copying the calibrated or uncalibrated
reflectance data and pasting it into a spreadsheet such as Microsoft EXCEL. Save the
data in the comma separated variable format (.CSV) and paste the file into the Scan data
directory. Consult the online help for more details.
Transmission sample holder
The external DRA accessory uses either a clasp-style or cuvette-style sample holder that
fits over the dovetail mount at the transmission port of the integrating sphere. The claspstyle device, shown below, is best suited for solid samples large enough to completely fill
the transmission port. The optional cuvette sample holder mounts a liquid filled cuvette at
the transmission port.
Specifications
Wavelength
range
DRA 900
DRA 1800
DRA 2500
Cary 4000
200 nm to
900 nm *
200 nm to
900 nm
200 nm to
900 nm
Cary 5000
200 nm to
900 nm *
200 nm to
1800 nm *
200 nm to
2500 nm *
Cary 6000i
200 nm to
900 nm *
200 nm to
1800 nm *
200 nm to
1800 nm
UV/VIS
R928 PMT
R928 PMT
R928 PMT
TE* cooled
InGaAs
TE* cooled
PbS
Detectors
NIR
Sphere diameter
150 mm
Internal coating
Polytetrafluoroethylene
Coating density
1 g/cm3
Coating thickness
4 mm
Port area/total surface area ratio
<10% (CIE recommendation: <10%)
Minimum sample size#
~ 20 mm (3/4")
Maximum sample size
Unlimited
Power input
Sample compartment DRA connector
15-pin D-range connector with two high
voltage pins: -1000 volts DC.
Purge gas connections
Clean flexible tubing of 6 mm (1/4") inside
diameter (Tygon PVC or equivalent).
Size packed
W x L x H, 500 mm x 840 mm x 470 mm
Size unpacked
W x L x H, 330 mm x 660 mm x 300 mm
Weight packed
35 kg
Weight unpacked
12 kg
* Thermoelectrically cooled.
#
The optional small spot kit, with the aperture kit, permits the measurement of samples
down to approximately 5mm.
The accessory is suitable for indoor use only. Suitable for Installation Category I and
Pollution Degree 2. Environmental conditions are the same as for the Cary
spectrophotometer.
Getting started
This section describes how to unpack, install, and align your Diffuse Reflectance
accessory.
Caution
This accessory includes mirrors, lenses and other fragile parts.
Treat the packaging and accessory with care. Do not jar the accessory. Avoid finger
contact with mirrors and lenses. Do not attempt to clean or repair damaged surfaces.
Caution
If the equipment is not used in a manner not specified by the manufacturer, the protection
provided by the equipment may be imparied.
Unpacking
Open the shipping case and the enclosed packages with care.
Warning
Do not touch the mirrors or other transfer optics mounted on the accessory. Fingerprints
will induce optical scattering and may reduce reflectance or transmission of these
components at certain wavelengths.
As well as the particular external DRA that you have ordered, included in the package are
the following:
Item
Description
Part number
3 x Uncalibrated PTFE Three PTFE plates for collecting baselines and
XXXX
reference plates
performing calibrations.
1 x Accessory cover
(installed)
XXXX
2 x Magnetic sample
port covers (installed)
Magnetic covers for the reflectance and
reference ports.
XXXX
1 x Light seal/guillotine
I metal plate to seal the join between the DRA
and the sample compartment.
XXXX
1 x Lockdown pin
Metal pin to hold DRA into place.
XXXX
2 x Dovetail sample
ledge (installed)
Metal ledges to assist in mounting of samples
and holders.
XXXX
2 x Spring loaded
sample holder
Round sample holder on a spring loaded base
for use at the reflectance and reference ports.
XXXX
1 x Specular port plug
XXXX
1 x Specular light trap
Metal plate with PTFE cut-out to seal the
specular port.
XXXX
1 x Centre port plug
Round PTFE plate to fit into the centre mount
port.
XXXX
1 x Transmission port
holder
Metal plate with two clips, for mounting of
solid samples and the cuvette holder.
79 100479 00
1 x M3 moveable
mirror
Mirror that can be mounted in the Centre,
Reflectance or Transmission position
depending on the type of measurement being
taken.
XXXX
1 x Purge adaptor
Stainless steel adaptor for applying a nitrogen
purge to the DRA.
XXXX
1 x 5/32 Hex driver
XXXX
1 x Allen key
XXXX
1 x Test results
Results of factory tests on the DRA.
Not applicable
1 x Cary WinUV Help
and Video CD Rom
85 101953 00
1 x Patches CD ROM
XXXX
XXXX These part numbers were not available at the time of publishing, please refer to
the Varian website, for the most up to date information. See www.varianinc.com
Inspect all parts for damage in transit. Any damage should be reported immediately.
Please refer to the accessory by model and serial number.
1. Unpack M3 and screw it into the "R" position. Set the mirror alignment pins into the
correct locator holes and secure the mount with the mounting screw. Refer to figure 19.
2. Remove the accessory cover.
Figure 16. Removing the accessory cover.
3. Remove the light seal/guillotine.
Figure 17. Removing the light seal.
4. Remove the magnetized covers from the reference and reflectance ports.
5. Install the centre mount port plug into the top of the sphere. Refer to figure 19.
6. Install the specular port plug. Refer to figure 19.
7. Use the "T" handle and the corner (marked "Lift Here") to lift the DRA out of the
box. See figure 18.
Warning
The accessory is heavy (32.5 kg). Safe lifting procedures should be used.
When the accessory is in its box, two people are required to do the lifting.
There is a handle at each end of the box to assist in the lifting.
Figure 18. Lift the DRA from the wooden packing case as shown. One hand on the "T"
handle, the other under the corner marked "Lift here".
If you have also ordered any of the specialized sample mount options you must also
inspect these kits. The Standard Sample Holder kit is included as standard with each
DRA.
Installation
The DRA fits into the spectrophotometer sample compartment using the lockdown
mechanism.
Warning
Do not touch the mirrors or other transfer optics mounted on the accessory. Fingerprints
will induce optical scattering and may reduce reflectance or transmission of these
components at certain wavelengths.
1. Turn off the spectrophotometer and remove any cell holders or other accessories
from the sample compartment (the PC can be left on).
2. Turn the power to the spectrophotometer on and allow time for the instrument to
warm up (about two hours).
3. Fully open the sample compartment lid and remove the front panel.
4. Make sure mirror M3 is set to the position in the DRA required for the intended
application. The reflectance position "R" is the one closest to the front of the accessory;
the transmission position "T" is the position furthest back. To move the mirror, loosen its
mounting screw, lift the mirror off the base plate and move it to the position required. Set
the mirror alignment pins into the correct locator holes and secure the mount with the
mounting screw. See figure
19.
Figure 19: The Varian 900, 1800, 2500 Diffuse Reflectance accessory with the optics
cover removed. The large reference plate is clamped over the sample port at the centre of
the sphere cap.
5. If not installed already fit the centre mount port plug into the top of the sphere.
6. If not installed already install the specular port plug.
Figure 20. Install the specular port plug.
7. Remove the accessory from the wooden container by lifting the accessory by the "T"
handle and the corner marked "Lift Here".
Figure 21. Lift the DRA from the wooden packing case as shown. One hand on the "T"
handle, the other under the corner marked "Lift here".
8. Slide the DRA into the sample compartment at a 20° angle.
9. Take care to align the metal edges of the DRA with the guide tabs on the edge of the
instrument sample compartment. This will correctly align and engage the rear lockdown
pins into the the sample compartment floor. The following two photos illustrate how to
line up the tabs, note inparticular the red circle indicating where the tabs should sit.
Figure 22. Align the tabs on the DRA with those on the instrument sample compartment.
Figure 23. Place the front lock down pin into position.
10. Place the front lockdown pin into the hole in the DRA floor next to the "T" handle.
11. Gently manoeuvre the DRA until the pin falls into place.
12. Flick the lockdown lever on the front instrument panel to the left. Do not connect the
accessory cable to the instrument.
Caution
The spectrophotometer must be turned off before plugging in the DRA, or serious
damage may result.
13. Install the light seal.
14. Slide the adjustable sample ledge on to the dovetail ledges at the reflectance and
reference ports.
15. Fit the spring loaded sample holders onto the ledges at the reflectance and reference
ports. Load a reflectance standard at each port and install the magnetic covers at each
port.
Figure 24. The sample holder fits onto the dovetail at either the reference or reflectance
port.
16. Install the transmission sample holder at the transmission port, it should slide easily
into the dovetail cut-out (just behind the sphere) with the metal clips pointing up.
17. Click the Windows Start button, then Programs, then Cary WinUV, and then Align.
18. The first time you install the DRA you must check the optical alignment of the
accessory as described in the Alignment check section. If the accessory fails the
alignment check, proceed to the Aligning the DRA procedure.
19. If the DRA is correctly aligned close the sample compartment lid and turn the
spectrophotometer instrument OFF.
Caution
The spectrophotometer must be turned off before plugging in the DRA, or serious
damage may result.
20. Connect the accessory detector cable to the matching connector at the rear of the
sample compartment, refer to the figure below.. Make sure the detector cable does not
obstruct the beam path inside the optical chamber of the accessory. Close the sample
compartment lid.
Figure 25: DRA socket
21. Click the Windows Start button, then Programs, then Cary WinUV, and then
Validate. Turn on the spectrophotometer. If the instrument will not initialize, proceed to
the Troubleshooting section.
22. Close the Validate application.
23. If desired, confirm the proper operation of the accessory by performing the
diagnostic scans described in the Diagnostic Scans section of the online help. You may
wish to perform these tests on the initial installation of the DRA.
24. Run the Calibration checks.
Warning
This accessory contains electrical circuits, devices, and components
operating at dangerous voltages. Contact with these circuits, devices and
components can cause death, serious injury, or painful electrical shock.
To prevent electric shocks, operators and other unauthorized personnel
must never remove the main cover. This must be opened only by Variantrained, Varian-qualified, or Varian-approved service engineers.
Alignment
Warning
To prevent eye damage use care when looking into the various ports during
the alignment process. Do not look into the light beams.
After installing the DRA it is necessary to check the alignment of the accessory. In some
cases it will then be necessary to Align the DRA.
You will need:
•
•
A flat blade screw-driver
3mm Allen key (provided)
Alignment check
This procedure can be used to check the optical alignment of the accessory without
disturbing any mirror adjustments. A one inch square of translucent paper (e.g., tissue) is
required.
1. Open the Align (if it is not already running) by clicking the Windows Start button,
then Programs, then Cary WinUV, and then Align.
2. Darken the room and set the instrument for white light operation as follows:
Cary tab
Beam Mode
Double
Y Mode
%R
Ave Time
0.1
SBW
Slit Height
2
Full
Select the Zero Order checkbox and click Apply.
2. Remove the cover to the accessory and remove the centre mount plug.
3. Slide the piece of translucent paper (e.g., tissue) into the reflectance port just behind
the port opening. Looking through the centre mount port, examine the location of the
sample beam relative to the port. Check that the beam is centred, and falls completely
within the port surface area. The beam should not overfill the port.
Figure 26. Checking the beam at the reflectance port.
4. Repeat the previous step for the reference beam at the reference port.
Figure 27. Checking the beam at the reference port.
5. Mount or hold the translucent paper directly in front of the transmission port. Check
that the sample beam is confined to the surface area inside the transmission port.
6. Repeat the previous step for the reference beam at the reference beam entrance port.
7. If the reference and sample beam profiles meet the criteria specified in the previous
steps, the accessory optics are aligned properly and no further alignment is necessary.
Return to Step 16 of the Installation procedure. If the accessory alignment does not meet
the criteria, proceed to the following section.
Aligning the DRA
This procedure is used to align the transfer mirrors in the accessory optical chamber. A
one inch square of translucent paper is required that clearly displays the outline of the
sample or reference beam when illuminated. The following procedure should be
performed using white light operation. Refer to the illustration in the figure below when
performing the optics alignment.
Figure 28: The optics of the DRA.
1. Click the Windows Start button, then Programs, Cary WinUV and then Align.
2.
Click the Setup button.
3. Darken the room and set the instrument for white light operation by setting the
following parameters:
Cary tab
Beam Mode Double
Y Mode
%R
Ave Time
0.1
SBW
2
Slit Height
Full
4. Select the Zero Order checkbox and click Apply.
Place a piece of translucent paper in the sample beam path in front of M1 to check that
the beam is centreed. If the beam is not centreed:
•
•
Check that that DRA is correctly locked down onto the instrument sample
compartment floor.
If the DRA is correctly installed, and misalignment persists, contact your local
Varian service representative.
Place a piece of translucent paper in the sample beam path in front of M2. Turn the
adjustment screws of mirror M1 until the beam is centred on M2.
7. Place the translucent paper in the sample beam path in front of M3. Adjust M2 until
the beam is centreed on M3. Use the hex ball screw driver to loosen the locking nut on
M2. Use the flat blade screw driver to adjust M2 until the beam is centreed on M3.
8. Remove the cover to the accessory.
8. Make adjustments to mirror M3 using the translucent paper and one of the following
steps.
a. For reflectance measurements, slide the piece of translucent paper into the reflectance
port just behind the port opening. Examine the location of the sample beam relative to the
port. Check that the beam is centred, and falls completely within the port surface area. If
necessary, turn the adjustment screws of mirror M3 until the beam is centred on the
opening at the sample reflectance port. Hold the piece of translucent paper at the
transmission port just in front of the port opening. The beam should not overfill the
reflectance or clip the transmission port. The sample beam is now aligned.
b. For transmission measurements, hold the piece of translucent paper at the transmission
port just in front of the port opening. Turn the adjustment screws of mirror M3 until the
sample beam is centred on the transmission port. In this configuration, the sample beam
may overfill the reflectance port, but it should be tightly focused at the transmission port.
The sample beam is now aligned.
c. For centre mount use, load the translucent paper into one of the centre mount sample
holders and load the entire assembly into the sphere. Block the reference beam with a
plate and remove the reference port plug. View the centre mount holder through the
reference port. Turn the adjustment screws of mirror M3 until the beam is centred on the
sample area but does not clip the edges of the transmission port. When finished remove
the blocking plate.
9. Place the paper in the beam path in front of M5. Turn the adjustment screws of mirror
M4 until the reference beam is centred on M5.
10. Turn the adjustment screws of mirror M5 until the beam is centred on the reference
port. If using a centre mount sample holder, the reference beam should pass directly in
front of the centre mount device.
11. Alternately adjust mirrors M4 and M5 to centre the reference beam on both the
reference beam entrance and the reference ports such that the beam is not clipped by the
cente mount sample holder. The reference beam is now aligned.
12. Return to Step 7 of Installation.
Error checks and diagnostic scans
The following section describes the procedures for a series of diagnostic scans or error
checking. The scans should be performed as part of the installation procedure and
routinely as part of a preventive maintenance program. The successful performance of the
diagnostic scans validates the operation of the accessory. The accessory optics should be
aligned and the electronics calibrated before proceeding with the diagnostic scans.
Hot Tip
It may be useful to construct a method file for each of these scan procedures. The
scan results should be retained for future use. If problems develop with the
accessory in the future, the diagnostic scans can be repeated with copies sent to
Varian for analysis. All diagnostic scans are set up and executed from the WinUV
Scan application.
In the normal spectrophotometer configuration, the front beam serves as the sample beam
and the rear beam is the reference beam. The DRA units all use the reverse beam
configuration, where the rear beam is the sample beam and the front beam path serves as
the reference beam. When a DRA is installed in the spectrophotometer, beam reversal is
applied automatically during system initialization. Therefore, the Beam mode—Double
checkbox should be selected.
Note
Parameters activated by a radio button that are not specifically mentioned in the
following procedure should be set to ’Off’ (e.g., the Signal-to-noise mode radio
button). These parameters will not affect the procedure.
1.
Click the Windows Start button, then Programs, then Cary WinUV, and then Scan.
2.
Click the Setup button.
3.
From the Setup menu, set the following parameters to carry out the error checking.
Cary tab
X mode: Mode
X mode: Start/Stop
Nanometers
User-set range
Y mode: Mode
%R
Y mode: Y min
-5.00
Y mode: Y max
110.00
Scan controls:
Ave time (s)
1.000
Scan controls:
Data interval (nm)
0.500
Scan controls:
Scan rate (nm/min)
30.000
Options tab
SBW/Energy: Fixed SBW
ON
SBW/Energy: SBW (nm)
2.00
SBW/Energy: Beam
mode
Double
SBW/Energy: Slit height
Reduced
Source: Lamps
UV-Vis
Source: Source
changeover (nm)
350.0
Baseline tab
Correction
None
Autostore tab
File Storage: Storage
OFF
4. Click the ’Goto’ button to open the ’Goto wavelength’ dialog box box. Enter ’500’ in
the wavelength field and click OK. The instrument will then drive to 500 nm.
Zero %R error check - alignment check
1. With the transmission ports uncovered, place the large reference plate over the
reflectance port.
2. From the main ’Scan’ dialog box box, click the Zero button and wait for the
instrument to zero.
3. Remove the reference plate so the beam is going straight through the sphere into the
sample cover. Close the sample compartment, the reading should not be greater than
0.5%R. If it is then check the alignment of the beam through the sphere (adjust M2 as
necessary), check that the lens is clean and free from dust, and ensure that the beam is not
clipping the reflectance port.
Zero %T error check - Electronic calibration check
1. Place the large reference plate over the reflectance port, close the sample
compartment and then zero the instrument
2. Block the beam with a blanking plate (a large solid object) placed in front of the
transmission port of the sphere.
3. The reading should be less than 0.01%R. If it is not, use the Calibration menu item
in the Validate application. Refer to the Calibration section for further details.
Zero Abs error check - photometric noise check
1. Open the Validate application and select noise test under instrument performance
tests.
2.
Enter a tolerance of 0.00012 Abs for UV-Vis and 0.00016 Abs for NIR test.
3. Run the test. If the test fails, use the Calibration menu item in the Validate
application. Refer to the Calibration section for further details. Also run the noise tests
without the DRA installed. If necessary align the visible lamp in the instrument.
Specular component exclusion check
1. Position the specular light trap over the specular port.
2. Place the large reference plate over the reflectance port.
3. Click the Goto button to open the Goto wavelength dialog box box. Enter ’500’ in the
Wavelength field and click OK. The instrument will then drive to 500 nm. Close the
sample compartment lid.
4. Click the Zero button and wait for the instrument to zero.
5. Place a mirror over the reflectance port, and close the sample compartment. Note the
reading. If the reading is greater than 1.5%R, then either the specularly reflected beam is
not entering the light trap, dirt on the lens is scattering the beam and creating a ’halo’
effect on the reflectance port, or the sample mirror does not have a good specular surface.
If the reading is greater than 1.5%R, you should repeat the check for the specular
component as detailed in the Checking for the specular component section.
6. Remove the specular light trap and replace the specular port plug. When the sample
compartment is closed, the reading should be approximately 90%.
Attachment options
There are several different attachments options available for use with the external DRA.
These greatly increase the versatility of the accessory. The attachment options are:
•
•
•
•
•
•
•
Transmission port cuvette holder
Centre-Mount Sample Holders
Small spot kit
Double aperture accessory
Polarizer
Powder cell
Apertures
Transmission Port Cuvette Holder
The transmission port cuvette sample holder mounts a standard 1 cm cuvette directly in
front of the transmission port. Transmission measurements made with this device at the
transmission port will include the a portion of the scattered component of radiation in the
transmission scan data. The sample holder is mounted into the clip style transmission port
and is illustrated below.
Figure 29: The cuvette holder
Installation and alignment
To install the cuvette holder:
Slide the cuvette holder over the dovetail so that it fits securely into the clips.
Check the sample beam alignment before proceeding with transmission measurements.
To record transmission data with the cuvette holder, refer to the 0°/d Transmission
Measurements Using the Comparison Method.
Centre-Mount Sample Holders
A centre-mount sample holder offers two distinct advantages over the external sphere
sample holders on the DRA. One is the ability to vary the angle of incidence for
reflectance and transmission measurements. The other advantage is the ability to measure
the transmission and reflectance of a sample together (transflectance).
There are several centre-mount designs, depending on the reflectance or transmission
application intended.
•
•
A variable angle sample holder mounts a solid sample at the centre of the sphere
at specified angles of incidence from the sample beam. The variable angle sample
holders may be clip or jaw style.
A cuvette centre-mount sample holder positions a cuvette inside the sphere at a
fixed angle normal to the sample beam.
Installation and alignment
To install a centre mount sample holder:
1. Remove the sphere cap from the top of the sphere.
2. Lower the centre mount through the opening in the sphere.
3. Fit the two posts on the centre mount onto the sphere by using the two locating holes
in the top of the sphere.
Figure 30. Lower the centre mount through the opening in the sphere, user the locating
holes in the top of the sphere to secure the centre mount.
4. Align the centre mount sample holder.
Alignment
Occasionally, the requirement exists to conduct fine tune alignment of the beam inside
the integrating sphere. Use white light operation and observe the beam path adjustments
through the accessory cover opening.
To check white light alignment:
1. Alternatively block the beam at the reference and transmission entrance ports and
view the alignment through the opposite port.
2. Click the Windows Start button, then Programs, then Cary WinUV, and then Align.
For centre mount use, load the translucent paper into one of the centre mount sample
holders and load the entire assembly into the sphere. Block the reference beam with a
plate and remove the reference port plug. View the centre mount holder through the
reference port. Turn the adjustment screws of mirror M3 until the beam is centred on the
sample area but does not clip the edges of the transmission port. When finished remove
the blocking plate.
Variable Angle sample holders
A variable angle centre-mount sample holder enables the sample reflectance and
absorbance to be studied at various incidence angles of the sample beam. The variable
angle centre-mount sample holder uses a rotating dial to allow the user to quickly set the
desired incidence angle to the nearest 1°. Depending on the sample size and the
instrument beam characteristics, the user can perform measurements at beam incidence
angles ranging from 0 - 60°.
Clip and Jaw style centre mount sample holders
The clip and jaw type centre-mount sample holders fix the sample at the centre of the
integrating sphere at selectable incidence angles.
The clip style sample holder, shown in the figure below, uses a spring-loaded clip to hold
the sample. This is useful for measuring transflectance. The sample must be in a sheet
configuration and large enough to accommodate the entire sample beam.
The jaw style sample holder (shown in figure 31) is better for holding large, bulky
samples. The sample must be opaque or an absorbent backing must be applied. The
sample holder is designed for reflectance measurements of samples that do not transmit
light.This centre mount sample holder is not designed for transflectance measurements.
The jaws accommodate sample sizes up to 1.5" in length and width. A clean disc of
SRM-99O optical grade Spectralon material approximately 30 mm in diameter can be
used as a reflectance standard.
Figure 31: The clip style variable angle sample
holder.
Figure 32: The jaw style centre
mount.
The width limitation of the jaw style sample holder depends on the thickness of the
sample and the maximum angle of incidence the application requires. The jaws protrude
12 mm from the frame of the sample holder. If possible, the reflectance standard and
sample should be loaded so the reflecting surface is even with the front edge of the jaws.
This will place the front surface at the rotational axis of the sample holder.
Centre-Mount Cuvette Sample Holder
The transmission port cuvette holder is used for measuring the transmission of a liquid
sample. The centre-mount cuvette sample holder provides a liquid sample measurement
capability to the DRA accessory that includes the scattered component of transmitted
radiation. A centre-mounted cuvette allows the simultaneous measurement of a turbid
sample diffuse transmission and reflectance, so that absorbance can be derived in one
easy measurement. The device is ideal for measuring turbid samples such as sea water,
proteins, and other biological solutions. Measurements performed with this device are in
the 0°/d geometry. Since the cuvette is fixed at 0° angle of incidence, the specular
component of reflection is directed out of the sphere through the transmission port.
Alignment
Upon first time use, the sample holder should be loaded into the centre-mount port and
checked for proper angle alignment to the sample beam, the beam should strike at normal
incidence when the dial is set at 0°. If it does not, rotate the knob until the angle is normal
to the sample beam, loosen the four screws along the perimeter of the dial and rotate the
dial so it reads 0°.
The reflecting surface of the standard should be the same angle of incidence as the
intended sample. When properly aligned, the 0° dial reading on both clip style and jaw
style sample holders holds the sample for normal incidence where the reflecting surface
is perpendicular to the path of the sample beam.
Ideally, the beam geometry for a reflectance accessory should be optimized for the
application concerned. For centre-mount applications, the ideal configuration has the
sample beam focused on the front surface of the sample at the centre of the sphere. In
general, the maximum dimensions of a centre-mounted sample is proportional to the size
of the integrating sphere. It should be obvious that the smaller the sample, the more
accurate the reflectance measurements - as long as the sample beam does not overfill the
surface area of the sample. For measurements with an Edwards sphere, ASTM E 903
recommends limiting specimen size to one percent of the surface area of the sphere.
Thus, for a 150 mm diameter integrating sphere, the maximum specimen size is a total
surface area of approximately 700 mm2. Sample sizes exceeding the recommended
specimen dimensions may interfere with the radiance uniformity at the wall surface or
clip the reference beam inside the integrating sphere.
Centre-mount sample holders inflict further restrictions on reflectance samples. The DRA
accessories utilize a three position mirror to focus the sample beam at the transmission
port, sample reflectance port, or centre-mount positions, depending on the sphere
configuration. Mirror M3, however, is a concave mirror such that the spot produced by
the sample beam depends on the position of the mirror and the angle of incidence to the
sample. The spot size grows larger as the angle of incidence increases, to a point where
the spot may no longer fit on the sample surface. At near-normal angles, the specular
component of the reflected beam is rejected completely out the transmission port and is
not collected during the scan. Finally, the horizontal dimension of the sample or
reflectance standard may clip the reference beam at steep angles of incidence, thereby
placing premature limitations on reflectance measurements.
Loading a sample into the jaw style centre sample holder
Tighten the jaws using the thumbscrew. Do not overtighten the jaw mechanism as this
could damage the sample.
When loading a sample into the clip sample holder, the sample should be held perfectly
vertical by the clip with the plane of the reflecting surface along the centre of rotation of
the dial. The sample beam path will strike the sample at a point midway between the
bottom tip of the clip and the baffle. There is no need to use a diffuse reference standard
with the clip style sample holder, the sphere wall serves as the reference.
After loading the sample holder into the accessory, view the sample from the reference
port, making sure the reference beam is not clipped by any part of the assembly at the
incidence angles required.
Centre-Mount Cuvette Sample Holder
The cuvette holder (figure 33) is designed to hold a standard 10 mm path length cuvette
at the centre of the integrating sphere. A pocket in the bottom platform to the sample
holder orients the cuvette at normal incidence to the sample beam. The upper platform is
spring loaded to hold the sample in place. The baffle located under the sample prevents
the detectors from directly viewing first strike reflections.
Figure 33: The cuvette variable sample holder.
Using the centre mount cuvette holder
1. Position M3 at the centre-mount location "C"
2. Check the alignment of the accessory.
3. Carefully place the filled cuvette into the holder and carefully lower the sample holder
into position.
Caution
Exercise great care when loading the centre-mount cuvette holder into the integrating
sphere, the sample holder is bulky and spilled sample solutions may damage the interior
surfaces of the sphere.
Small Spot Kit
A sample loaded at the DRA reflectance port or other sample site should be the same
size as the focused sample beam. If the sample is smaller than the beam spot, the
accuracy of the results will be reduced. If the sample surface fills the entire port, the
spectra obtained may be accurate but the signal-to-noise ratio is reduced by the
absorption characteristics of the sample. The small spot kit allows the user to focus a
small beam spot at the transmission port, reflectance port or sphere centre of the diffuse
reflectance accessory. The kit adds versatility to the DRA in three ways. The kit can be
used to reduce the sample beam size to measure small samples. It can be used to focus the
sample beam to measure a small portion of a larger sample. Or, it can be used with a
centre-mount sample holder to prevent the sample beam from overfilling the sample at
high measurement angles. The small spot kit consists of the following standard and
optional components:
Description
Part number
Iris Assembly
XXXX
Collimating Mirror
Assembly
XXXX
Lens Holder w/ (2)
Mounting Screws
XXXX
Transmission Lens
XXXX
Centre-mount Lens
XXXX
Reflectance Lens
XXXX
Wire Attenuator Screen
XXXX
Tool Kit, 3/16² hex key
XXXX
Reflectance Port Aperture
XXXX
Kit
XXXX These part numbers were not available at the time of publishing, please refer to
the Varian website, for the most up to date information. See www.varianinc.com
The lens holder and rail are illustrated in the figure below. Each lens is marked by a letter
identifying the corresponding to the sample location and an arrow indicating the correct
orientation for installation.
Figure 34: The small spot kit lens holder, rail and lens.
Note
The small spot kit replacement for mirror M3 must be used instead of the standard
accessory mirror. The two mirrors look similar, but the small spot kit mirror is
visibly less concave than the standard accessory M3 and is marked "M-3 SSK".
Installation and Alignment
The small spot kit requires an initial installation. Once installed, the user can refer to the
Operation section for details regarding reflectance measurements. To install the small
spot kit, follow these instructions:
1. Remove the accessory from the instrument sample compartment and install the
replacement mirror to M3 (M-3 SSK) at the "T" position. The replacement mirror
assembly must always stay at the "T" position when using the small spot kit
Figure 35: Installing the small spot kit.
2. Install the iris assembly in the position shown above. The mounting plate for the iris is
magnetized to hold the iris firmly in place. Two adjustment controls are provided on the
iris, one for adjusting the iris position laterally and one for controlling the aperture size.
Open the iris fully.
3. Remove the lens holder from the dovetail base and mount the rail onto the accessory
base plate as shown. Load reflectance standards at the reference and reflectance ports.
Figure 36. The small spot kit in the DRA.
4. Turn on the instrument on and allow it to warm up (approximately 2 hours).
5. Set the instrument to Zero order using the Align application. See Installation step 14.
6. Once the instrument is warmed up, remove the reflectance standards from the ports (if
they are currently loaded). Load the reflectance lens into the small spot kit lens mount.
The reflectance lens is marked "R", the transmission lens is marked "T", and the centremount lens is marked "C". The lens should be oriented so the arrow points toward the
integrating sphere. Gently rotate the lens until it clips into place. The grooves in the
outside of the lens sit on the clips on the mount.
7. Remove the transmission holder. (The transmission holder may clip the beam,
reducing the energy entering the sphere.)
7. Install the DRA into the instrument. Turn the instrument ON and allow it to initialize.
8. Install a beam blocker over the reference beam entrance port.
9. Find the sample beam at mirror M2 and centre if necessary.
10. Fully close the iris. Look at the top left hand corner of M3 and observe the beam on
the back of the iris. When the iris is closed to its smallest opening size, the beam should
be taller than the hole but centreed in the iris opening. To realign the iris assembly in the
beam path, first loosen the thumb screw that secures the two sections of the iris assembly
together. Move the top portion of the iris assembly, sliding it laterally, until the beam is
centreed on the iris opening. Retighten the thumb screw.
11. Fully open the iris. Dim the light in the room.
12. Adjust mirror M2 to centre the beam on the M3 SSK mirror. See Alignment for
instruction on aligning the mirrors.
13. Hold the translucent paper just outside the open reflectance port. Adjust the M3 SSK
to centre the sample beam within the reflectance port opening. It may be necessary to
adjust the aperture size of the iris or relocate the lens mount along the dovetail rail to
achieve the desired spot size and make a note of the position of the iris.
Figure 37. The beam from the small spot kit with the iris partially open.
14. Remove the beam blocker from the reference beam path.
15. Replace the reflectance plug. The small spot kit is now aligned.
16. Turn off the instrument.
17. Plug in the DRA using the connector at the back of the sample compartment.
18. Fully open the iris and replace the accessory cover.
19. Turn on the instrument and allow it to initialize.
20. Return the iris to the position noted in step 13.
Powder cell
In some cases, a reflectance measurement may deliver better diffuse reflectance spectra
when the sample is ground to powder form. As shown in Figure 38 and 39, the powder
cell is designed to fit inside the reflectance sample holder in the same manner as the
reflectance standard. Each sample holder comes as a set: one cell with a Spectralon insert
for use as a reflectance standard, and an empty cell for loading the powdered sample. The
quartz window for each cell is compatible with each DRA accessory across the entire
250-2500 nm wavelength range.
Figure 38. The powder cell fits into the sample holder at
the reflectance port.
Figure 39. The powder cell
in position at the reflectance
port.
The design of the PCH-150 sample holder does not facilitate an accurate means of
loading a powdered sample to an accurate packing density. An approximate packing
density and reflectance measurement can be obtained using the following procedures.
Prior to loading, the sample should be ground to the desired particle size.
Sample Preparation Using the PCH-150 Powder Cell Holder
Figure 40. An exploded view of the powder cell.
1. Disassemble the powder cell holder. DO NOT disassemble the reference cell holder.
Place the front cover onto the flat surface of a balance scale, face down, and load the
quartz window into the cover.
2. Record the weight of the two sample holder components.
3. Load a portion of the sample into the powder cell cavity over the quartz window.
Gently tap the side of the holder against the work table, or use a spatula to smooth the
surface of the sample. Repeat this loading process until the desired sample depth or
sample weight is achieved.
4. Record the weight on the balance scale and calculate the total weight of the powdered
sample.
5. Estimate the average height of the sample by measuring the distance from the sample
to the top surface of the container.
6. Load the plunger and spring over the sample and screw the body over the entire
assembly. Screw the pieces together snugly, but do not apply excessive force.
7. Examine the surface around the sample holder for any loose sample material that may
have spilled out of the sample holder cavity. Weigh the spilled powder and make
corrections to your calculation in Step 4.
Figure 41. Calculating the packing density.
8. Calculate the packing density using the sample weight recorded in the previous steps.
Reflectance Measurements Using the Powder Cell Holder
To perform reflectance measurements using the Powder cell holder, proceed as follows.
1. Load the powder cell containing the Spectralon insert against the reflectance sample
port of the sphere. There should be a Spectralon reflectance standard mounted at the
reference port.
2. Record one of the baseline scans as directed previously. DRA configuration during the
baseline scan should conform exactly to the configuration anticipated during the sample
scan.
3. Replace the powder cell sample holder at the sample reflectance port with the powder
cell containing the sample. Do not change the configuration of the integrating sphere in
any other way.
4. Open the Setup Dialog and check the instrument parameter Setup. Normally, the Setup
parameters for the application should match those used for the baseline scan. If using a
previously defined baseline correction, retrieve the correct baseline.
5. Record the sample scan by selecting the Start button in Cary WinUV software.
6. If the standard reference option was used for the baseline scan, the reflectance spectra
is generated automatically. If the simple or zero baseline correction was selected without
the standard option, multiply the sample scan data by the spectral reflectance factors for
the calibrated reflectance standard.
To obtain the best results follow these guidelines when using the Powder cell holder.
•
•
The sample reflectance depends upon sample handling factors, such as the
packing density, surface uniformity, and characteristics of the sample. Finely
ground powder samples will give different reflectance results than the same
sample when measured in its coarse, granular, or pressed powder form. The
spectrum shape of the sample reflectance does not change with packing density,
that is, the peak location does not change. Only the relative reflectance value
changes with changes in the sample packing density.
If you wish to compare subsequent sample measurements, take care to ensure that
sample presentation to the beam and packing density are identical between scans.
Double aperture accessory
The double aperture accessory is used to determine the absolute photometric accuracy of
the DRA in the UV-VIS and NIR spectral range. The accessory mounts directly in the
sample beam path on the base plate.
Components accompanying the double aperture apparatus include the following:
•
•
•
•
Base mount
Aperture plate
Masking Wheel
Assorted fasteners
A detailed explanation of the double aperture method is provided in the Validate section
of the Help.
Figure 42: The optics of the double aperture accessory.
Figure 43. The double aperture attachment on the polarizer mount.
The accessory optics should be aligned according to the Installation instructions before
installing the double aperture. The base mount for the double aperture apparatus is the
same base used for the polarizer. Install the double aperture accessory as follows:
1. Remove the DRA from the instrument sample compartment. Locate mirror M3 at the
"R" position.
2. Insert the base mount into the locator holes in the DRA base plate as shown in the
figure above. The orientation of the mount is not important. Fasten the device to the
accessory using the M5 socket head screw provided and a 4 mm hex wrench.
3. Re-install the DRA into the sample compartment.
4. Click the Windows Start button, then Programs, then Cary WinUV, and then Align.
5. Turn on the instrument and allow the instrument time (about 2 hours) to warm up.
6. Remove the reflectance standards at each port.
7. Open the sample compartment lid and slide the aperture plate into the base mount slot
as shown in the figure. The protruding alignment pins should point into the accessory.
8. Block the reference and sample beam entrance ports to the integrating sphere and
configure the sample beam for white light operation.
9. Observe the beam profile as it strikes the aperture plate, adjust the height of the plate
so the rectangular apertures are centreed on the sample beam.
10. Remove the beam blocker from the sample beam path. Observe the reflectance port
from the open centre-mount port, mount a piece of translucent paper in the sample holder
against the reflectance port. Check that the images of the double apertures lie within the
perimeter of the sample reflectance port. Make slight adjustments to mirror M3 as
necessary. The double aperture device is aligned.
There are four aperture positions on the masking wheel each spaced at 90° intervals along
the perimeter. A dimple is drilled at the centre of the wheel to match the tiny centre pin
on the aperture plate. Both the aperture plate and masking wheel should be removed from
the accessory during reflectance and transmission measurements.
Note
If reflectance or transmission applications require use of the optional polarizer, the
base mount must be relocated to the polarizer position.
Polarizer/Depolarizer
A polarizer optic can be provided as an optional assembly to either of the DRA
accessories for conditioning the polarization of the sample beam. The polarizer is a GlanTaylor constructed device. Specifications of the optic is provided on the Help and Videos
CDROM in the Cary WinUV software package. The light reflecting off the Spectralon
walls is completely diffuse, so a depolarizing optic is never required for reflectance
measurements. It may be useful for transmission measurements on polarizing samples.
The following components accompany the polarizer attachment:
Base mount with attachment screws Lens holder Polarizer lens
Figure 44. The polarizer attachment
Figure 45. The polarizer attachment in the DRA.
The polarizer assembly uses the same base mount as the double aperture apparatus.
Install the polarizer assembly into the accessory as follows:
1. Insert the base mount for the polarizer into the locator holes in the accessory base
plate as shown in the figure below. Fasten the device to the accessory base plate using the
M5 socket head screw provided and a 4 mm hex wrench.
2. Click the Windows Start button, then Programs, then Cary WinUV, and then Align.
Turn power to the spectrophotometer on. Install a beam blocker at the reference beam
and sample beam entrance ports to the sphere and configure the sample beam for white
light operation.
3. Remove reflectance standards from the reference and reflectance ports. Remove the
centre-mount port plug.
4. Slide the polarizer optic into the base mount slot. The optic should be oriented in the
direction shown in the figure above.
5. Observing the sample beam profile as it strikes the entrance aperture to the polarizer,
adjust the height of the device so the sample beam penetrates the optic unclipped.
6. Remove the blocking device from the sample beam. Check the sample beam
alignment at the reflectance port using a piece of translucent paper. Make any
adjustments to mirror M3 as necessary.
7. Suspend white light operations and remove the blocking device from the reference
beam. The accessory is aligned for polarizer operations.
The base mount can remain installed in the accessory when the polarizer is not being
used. If adjustment to the sample beam alignment is required, an alignment check should
be performed whenever the polarizer is removed.
Note
The polarizer is an attenuation device and may reduce significantly the signal-tonoise ratio of the accessory during use.
Operation
Samples can be mounted at the transmission or reflectance ports. At the reference port,
attenuators may be mounted.
Routine DRA installation
The accessory must be installed in the sample compartment and the DRA cable
connected before turning the instrument power switch on. During initialization, the
spectrophotometer will adjust instrument radiation levels appropriate to the high
attenuation characteristics of the DRA, making the necessary gain adjustments to the
detector circuitry. Follow these instruction to install and configure for routine DRA
operation:
1. Turn the instrument off. Remove any cell holders or other accessories from the
instrument sample compartment.
Caution
The spectrophotometer must be turned OFF before plugging in the DRA, or serious
damage may result.
2.
Slide back the sample compartment lid and remove the compartment front panel.
3. Remove the accessory from the wooden container by lifting the accessory by the "T"
handle and the corner marked "Lift Here".
4. Slide the DRA into the sample compartment at a 20° angle. Take care to align the
metal edges of the DRA with the guide tabs on the edge of the instrument sample
compartment. This will correctly align and engage the rear lockdown pins into the the
sample compartment floor.
5. Place the front lockdown pin into the hole in the DRA floor next to the "T" handle.
6. Gently maneuver the DRA until the pin falls into place.
7. Flick the lockdown lever on the front instrument panel to the left.
8. Install the guillotine/light seal.
9. Load a reflectance standard at the reference and sample reflectance ports. Remove any
centre-mount sample holders installed in the sphere and install the centre port plug.
10. Connect the accessory detector cable to the connector at the rear of the sample
compartment. Make sure the detector cable does not obstruct the beam path inside the
optical chamber of the accessory. Install the accessory cover.
11. Click the Windows Start button, then Programs, then Cary WinUV, and then Scan.
12. Close the sample compartment lid and turn power to the instrument ON.
13. Allow the instrument and accessory to warm up for at least 30 minutes before
proceeding with measurements.
Removing the DRA from the instrument
Use the following procedure to disconnect and remove the DRA from the instrument:
1. Turn the spectrophotometer off.
2. Open the sample compartment lid and disconnect the accessory cable.
3. Remove the accessory cover.
Figure 46. Removing the accessory cover.
4. Remove the guillotine/light seal.
Figure 47. Removing the light seal.
Note
The lockdown lever is accessible just underneath the DRA base plate.
5. Slide the lever on the instrument front panel to the right.
6. Remove the front lockdown pin.
7. Tilt the front end of the accessory. Using the accessory handle, lift the DRA up and
out of the sample compartment and store it in the accompanying wooden box.
8. Replace the sample compartment front panel.
Collecting baseline scans
When taking reflectance measurements using a reflectance accessory, three types of
baseline corrections can be applied to the scan data. A simple correction is used in the
diagnostic scans that is quick and does not require zeroline or reflectance standard data.
A second and third method uses a zero baseline correction that can be applied by one of
two methods: either the sample beam can be blocked off from the integrating sphere
during the 0%R baseline scan or a light trap can be installed over the sample reflectance
port.
Note
The blocked beam method is discouraged by ASTM E 903 for reflectance
measurements because the effect of scattered light incident on the sphere wall is
not included in the data collection.
During transmission measurements, either the standard baseline or the blocked beam
method should be used. The spectrophotometer and accessory must be warmed up for 30
minutes prior to recording any of these baseline scans.
An integrating sphere is sensitive to small-angle scatter from the sample beam coupling
optics. Sometimes, the scattered radiation strikes the wall of the integrating sphere near
the reflectance sample port, creating a "halo" surrounding the port. This halo-effect
causes a small error in the measurement of the reflectance factor that is most significant
when measuring samples of very low reflectance. This error is easily corrected by using
the light trap zero baseline correction method discussed above.
Simple Baseline Scan for Reflectance or Transmission Measurements
Baseline scan data is recorded from the Cary WinUV Scan application. Prior to recording
the scan, make sure that mirror M3 is located in the correct position. To collect a baseline
scan:
1. Click the Setup button and set up instrument parameters as required by the intended
application. Select the %R or %T ordinate scale, depending on the type measurements
anticipated. The Beam mode should be double.
2. Select the Baseline radio button on the Baseline tab.
3. Load a Spectralon standard at the reference port and a calibrated reflectance standard,
if available, at the sample reflectance port. If a calibrated standard is unavailable for
reflectance measurements, an uncalibrated Spectralon standard can be substituted. Install
the magnetic port covers over their respective ports.
4. Click the Baseline button.
The recorded baseline correction will be effective until replaced by a follow-up baseline
scan.
Zero Baseline Scan for Reflectance or Transmission Measurements
Prior to recording the scan, make sure that mirror M3 is located in the correct position.
To record a zero baseline scan:
1. Click the Setup button and set up instrument parameters as required by the application.
Select the %R or %T ordinate scale, depending on the type measurements anticipated.
The Beam mode should be double.
2. For reflectance measurements, select the Zero/baseline correction or Zero x std ref
correction radio button on the Baseline tab. For transmission measurements, Zero/
baseline correction should be selected.
3. Load a Spectralon standard at the reference port and a calibrated reflectance standard,
if available, at the sample reflectance port. If a calibrated standard is unavailable for
reflectance measurements, an uncalibrated Spectralon reflectance standard can be
substituted. Install the magnetic port covers over their respective ports.
4. Click the Baseline button.
5. At the 100%T scan prompt, select OK. The standard at the reflectance port serves as
the 100%R reference.
6. At the 0%T scan prompt when running reflectance scans, either block the sample
beam at the transmission port or replace the reflectance standard at the sample port with a
light trap. When running transmission scans, the sample beam should be blocked for the
0%T scan.
The recorded baseline correction will be effective until replaced by a follow-up baseline
scan.
Note
If a light trap is unavailable, the baseline scan can be run with the sample
reflectance port open and the outside magnetic cover to the reflectance port
installed.
8°/h Reflectance Factor Measurements (Comparison Method)
For reflectance measurements, make sure that mirror M3 is placed in the reflectance
position, closest to the sphere. Repeat the alignment procedure if the mirror has been
moved. This mirror configuration provides a focused spot size of approximately 6.5 mm
wide x 15 mm high. If a large reflectance spot is desired, such as for measurement of
fabrics or other non-homogenous samples, place mirror M3 in the transmission mirror
position. This mirror configuration provides an unfocused spot size of approximately 20
mm wide x 25 mm high. Place the mirror in the centre-mount position if an intermediate
beam size is desired.
The reflectance port is constructed at an 8° angle from the incident sample beam to
facilitate 8°/h measurements. Additionally, the DRA has a specular exclusion port - the
diffuse and specular reflectance components can be separated by removing the specular
port plug. During 8°/h reflectance measurements, the specular port plug should be
installed. The following procedure should be used to measure the hemispherical
reflectance factor of a sample:
1. Collect a Baseline scan.
2. Replace the reflectance standard at the sample reflectance port with the sample. Do
not change the configuration of the integrating sphere in any other way.
3. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
4. Click the Start button.
5. If the standard reference option was used for the baseline scan, the reflectance spectra
is generated automatically. If the simple or zero baseline correction was selected,
multiply the sample scan data by the spectral reflectance factors for the calibrated
reflectance standard.
8°/d Reflectance Factor Measurements (Comparison Method)
The DRA integrating sphere is fitted with a specular exclusion port. When the exclusion
port plug is removed, the specular component of reflection from the sample is directed
out of the sphere and is not sampled by the detector. The diffuse component of the main
beam reflection remains inside the sphere and is sensed by the sphere detector. The
procedure for diffuse reflectance factor measurement is as follows:
1. Collect a Baseline scan.
2. Replace the reflectance standard at the sample reflectance port with the sample.
3. Replace the specular port plug with the specular port light trap. Do not change the
configuration of the integrating sphere in any other way.
4. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline..
5. Click the Start button.
6. If the standard reference option was used for the baseline scan, the reflectance spectra
is generated automatically. If the simple or zero baseline correction was selected,
multiply the sample scan data by the spectral reflectance factors for the calibrated
reflectance standard.
8°/h Reflectance Factor Measurements (Single Beam Mode)
Although the DRA is a double beam accessory, single beam operation is still possible.
When operating the DRA in this mode, a substitution error will be present in the
reflectance measurement data. The reference beam entrance port can be blocked off using
a Spectralon surface during the baseline and sample scans. The following procedure can
be used to measure the hemispherical reflectance of a sample.
1. Collect a Baseline scan, making sure the instrument is configured for single rear beam
mode.
2. Replace the reflectance standard at the sample reflectance port with the sample. Do
not change the configuration of the integrating sphere in any other way.
3. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
4. Click the Start button.
5. If the standard reference option was used for the baseline scan, the reflectance spectra
is generated automatically. If the simple or zero baseline correction was selected,
multiply the sample scan data by the spectral reflectance factors for the calibrated
reflectance standard.
0°/h Transmission Measurements (Comparison Method)
For transmission measurements, make sure that mirror M3 is placed in the transmission
position, marked "T" on the base plate, located farthest from the sphere. If this mirror is
moved or if the cuvette holder is installed over the transmission port, the transfer optics
must be realigned. Repeat the alignment procedure if M3 has been moved. The "T"
position mirror configuration provides a condensed spot size of approximately 5 mm
wide x 9.5 mm high. If a large transmission spot size is desired, such as for the
measurement of fabrics or other homogeneous samples, place mirror M3 in the
reflectance "R" position. This mirror configuration provides a spot size of approximately
11 mm wide x 28 mm high. If an intermediate spot size is required, place the mirror in
the centre-mount "C" position.
1. Collect a Baseline scan, following the procedures specific to transmission
measurements. If the sample resides on a substrate, load an untreated substrate blank at
the transmission port for the baseline scan recordings. If the transmission sample is
suspended in solution, load a blank cuvette at the transmission port for the baseline.
2. Load the sample at the transmission port. Do not change the configuration of the
integrating sphere in any other way.
3. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
4. Click the Start button.
5. The value displayed by the instrument is the sample transmission. No data correction
is required.
0°/d Transmission Measurements (Comparison Method)
The approximate diffuse transmission of a given test sample can be measured using the
DRA as follows:
1. Collect a Baseline scan, following the procedures specific to transmission
measurements. If the sample resides on a substrate, load an untreated substrate blank at
the transmission port for the baseline scan. If the transmission sample is suspended in
solution, load a blank cuvette at the transmission port for the baseline.
2. Load the sample at the transmission port and replace the reflectance standard at the
reflectance port with a light trap. Do not change the configuration of the integrating
sphere in any other way.
3. Click the Setup button and check the parameters. Normally, the Setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
4. Click the Start button.
5. The value displayed by the instrument is the sample transmission. No data correction
is required.
Loading samples at the reference or reflectance ports
When taking a sample at either the sample or reflectance port requires the use of the
sample holder as shown below.
Figure 48. The sample is mounted at the reflectance or reference port using the sample
holder.
Variable Angle Reflectance Measurements (Centre-Mount Sample Holder)
The DRA can collect variable angle of incidence reflectance data when a centre-mount
sample holder is installed inside the integrating sphere. Shift mirror M3 to the centremount position and align the transfer optics before proceeding with either of the
following procedures. The centre-mount sample holder should be employed only when
operating the instrument in double beam mode. Photometric accuracy of the variable
angle data may be reduced due to absorption characteristics of the sample holder
surfaces.
When using centre-mount devices, correct beam alignment is essential. Occasionally, the
requirement exists to conduct fine tune alignment of the beam inside the integrating
sphere. Rather than subject the sphere detectors to white light radiative flux, the operator
can drive the instrument to 500 nm and observe the beam path adjustments through the
accessory cover opening.
Note
Not all transfer optics are accessible through the sample compartment trap door,
and white light operation may be necessary.
To drive the instrument to 500 nm, select Goto from the Commands menu, enter 500 nm
and click OK. The sample compartment lid must remain shut in this mode of operation.
To establish white light operation temporarily, load beam blocks at the transmission and
reference beam entrance ports and select Align from the Commands menu.
Clip Style Sample Holder Measurements
1. Darken the room and drive the instrument to 500 nm.
2. Mount the sample into the sample holder, making sure it is properly centreed and
secured to the holding clip. Load the assembly into the integrating sphere and set the
anticipated angle of incidence using the attached dial.
3. While viewing the sample surface through the reference port, check that the sample
beam strikes the centre and does not overfill the sample at the angle selected. This step
may require use of a piece of translucent paper and will be more difficult at greater angles
of incidence. If the beam is off centre or will not fit on the sample, either adjust the
sample mounting in the sample holder or readjust the sample beam optics to achieve the
correct alignment. If any adjustments are made to the optics, make sure the sample beam
does not clip the transmission port.
4. Examine the path of the reference beam inside the integrating sphere. The beam
should strike the reference port without clipping any part of the sample or sample holder.
5. Remove the sample from the sample holder clip and load the empty sample holder
into the centre-mount port.
6. Load Spectralon reflectance standards at the reference and sample reflectance ports.
Install the magnetic covers over each respective port.
7. Collect a Baseline scan.
8. Mount the sample into the centre-mount sample holder and load the assembly into the
integrating sphere.
9. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
10. Click the Start button.
The value displayed by the instrument is the absolute sample reflectance. No data
correction is required.
Jaw Style Sample Holder Measurements
1. Darken the room and drive the instrument to 500 nm.
2. Mount the sample onto the sample holder, making sure it is properly centreed and
secured to the holding jaws. Load the assembly into the integrating sphere and set the
anticipated angle of incidence using the attached dial.
3. While viewing the sample surface through the reference port, check that the sample
beam strikes the centre and does not overfill the sample at the angle selected. This step
may require use of a piece of translucent paper and will be more difficult at greater angles
of incidence. If the beam is off centre or will not fit on the sample, either adjust the
sample mounting in the sample holder or readjust the sample beam optics to achieve the
correct alignment. If any adjustments are made to the optics, make sure the sample beam
does not clip the transmission port.
Figure 49. The beam falling on the reference mounted in the jaw style centre mount.
4. Examine the path of the reference beam inside the integrating sphere. The beam
should strike the reference port without clipping any part of the sample or sample holder.
5. Remove the sample holder from the sphere and replace the sample with a calibrated
diffuse reflectance standard. If a calibrated standard is not available, use an uncalibrated
Spectralon standard. Load the sample holder assembly into the integrating sphere and
install the accessory cover.
6. Collect a Baseline scan.
7. Mount the sample into the centre-mount sample holder. For the jaw style device, the
transmitted component from the sample beam must be eliminated so it is not collected by
the sphere. This can be accomplished by backing the sample with a piece of black felt
cloth. Load the sample holder assembly back into the sphere.
8. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
9. Click the Start button.
10. If the standard reference option was used for the baseline scan, the reflectance
spectra is generated automatically. If the simple or zero baseline correction was selected,
multiply the sample scan data by the spectral reflectance factors for the calibrated
reflectance standard or the typical data in Appendix B. Reflectance standards at
Labsphere are calibrated using 8°/h geometry
Absorbance Measurements (Cuvette Centre-Mount Sample Holder)
The following procedure can be used for obtaining absorbance measurements with a
centre-mounted cuvette. In the centre-mount configuration, normally reflected light exits
the sphere through the transmission port and is not counted.
1. Darken the room and drive the instrument to 500 nm.
2. Fill a clean cuvette with the pure solvent used as the sample preparation.
Note
If the intended sample is turbid, use an empty cuvette for the baseline scan. Load
the blank cuvette into the holder and load the sample holder assembly into the
centre-mount port. Position the alignment pins on the centre-mount device to match
the holes in the sphere.
3. While viewing the front cuvette surface through the reference port, check that the
sample beam strikes the centre of the cuvette. This step may require use of a piece of
translucent paper. If the beam is off centre or will not fit on the sample, re-adjust the
sample beam optics using M3 to achieve the correct alignment. If any adjustments are
made to the optics, make sure the sample beam does not clip the transmission port.
Figure 50. The beam falling on the cuvette centre mount.
4. Examine the path of the reference beam inside the integrating sphere. The beam
should strike the reference port without clipping any part of the cuvette or sample holder.
5. Collect a Baseline scan, or use a zeroline baseline, using the blocked beam method.
6. Remove the sample holder and replace the blank cuvette with the sample cuvette.
Load the sample holder assembly back into the sphere.
7. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
8. Click the Start button.
The value displayed by the instrument is the combined transmission. No data correction
is required.
Using the Small Spot Kit
The DRA small spot kit is composed of three lens options that focus the beam to a small
diameter spot at the selected sphere location. The top of each lens is marked as either:
"R" for reflectance port, "T" for transmission port, or "C" for centre-mount location. An
arrow appears next to each lens marking. The direction of the arrow indicates the side of
the lens which should face the sphere. After the desired lens is installed into the lens
holder assembly, it can be moved along its rail to focus the sample beam. When the
transmission lens is installed, the overall beam spot size will change as the lens holder is
adjusted along the dovetail rail. The spot size can be reduced down to 2.5 - 3 mm
diameter at the transmission port. For controlling beam size at the centre-mount or
sample reflectance port locations, the iris should be used in conjunction with the
corresponding lens. For the reflectance beam spot, the iris assembly can be closed to
reduce the spot size from approximately 8 mm tall by 2 mm wide to approximately 3.5
mm tall by 1.5 mm wide. Similar results are achieved with the centre-mount lens and iris
combination. A mask should be fitted over the transmission or reflectance ports when
collecting small sample measurements.
When operating in small spot mode, the sample beam undergoes considerable attenuation
before it reaches the integrating sphere. Increased energy and an expanded slit width may
be required for collecting accurate spectra. When measuring highly absorbing samples, it
may be necessary to attenuate the reference beam. A wire attenuation screen is provided
for this purpose. The screen is designed to fit at the entrance port for the reference beam.
The reference beam energy should be attenuated so that it matches the sample beam
energy in its most reduced state. Consult the Cary instruction manual for more
information on instrument requirements regarding sample and reference beam energy
balance.
Note
A reflectance port aperture kit, Labsphere Part No. AS-02021-000, is available
through your Varian representative to reduce the DRA reflectance port diameter to
better suit small samples. The kit consists of five different aperture plates which
mount on the reflectance port dovetail rail. These plates effectively change the
reflectance port diameter to 1”, 0.5”, 0.375”, 0.25”, or 0.15” (25 mm to 4 mm
diameter). A special sample restraining clamp is provided, and it can be fitted with
one of five suitably sized spacers to adapt to any sample size.
Transmission Measurements (Small Spot Kit)
At the transmission port location, the DRA small spot kit can be used to measure a small
test sample, or to measure a small portion of a larger sample. Prior to entering this
procedure, the small spot kit should be installed and aligned. Mirror M3 must always be
installed at the "T" position for small spot kit measurements.
1. Install the transmission lens, marked “T”, into the small spot kit lens holder. The
arrow marked on the lens should be pointing towards the sphere.
2. Darken the room and drive the instrument to 500 nm.
3. If the intended sample size is smaller than the transmission port opening, secure a
mask over the transmission port. The mask should be attached to the transmission port or
holder, and it must remain in place for both the baseline and sample scans. If the sample
is larger than the port size, place a piece of translucent paper into the clips of the
transmission sample holder and install the holder at the transmission port.
4. Adjust the position of the small spot kit lens assembly on its dovetail rail until the
desired spot size is obtained at the transmission port. The spot should be adjusted to fit
just within the sample surface. In general, the transmission spot size will be smallest
when the lens is moved away from the sphere. To optimize the signal reaching the sphere
detectors, the iris should remain fully open for small spot kit transmission scans.
Figure 51. The beam at the transmission port
5. Collect a Baseline scan, following the procedures specific to transmission
measurements. If the sample resides on a substrate, load an untreated substrate blank at
the transmission port for the baseline scan. If the transmission sample is suspended in
solution, load a blank cuvette at the transmission port for the baseline.
6. Load the sample at the transmission port. Do not change the configuration of the
integrating sphere in any other way.
7.
Click the Setup button and check the parameters. Normally, the setup parameters
for the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
8. Click the Start button.
9. The value displayed by the instrument is the sample transmission. No data correction
is required.
Reflectance Measurements at the Centre-Mount Location (Small Spot Kit
)
For samples loaded at the centre-mount location, the DRA small spot kit can be used to
measure a particularly small test sample, a portion of a larger sample, or to increase the
variable angle measurement capabilities of the accessory. Prior to entering this procedure,
the small spot kit should be installed and aligned. Mirror M3 must always be installed at
the "T" position for small spot kit measurements.
1. Install the centre-mount lens, marked “C”, into the small spot kit lens holder. The
arrow marked on the lens should be pointing towards the sphere.
2. Darken the room and drive the instrument to 500 nm.
3. Remove the transmission sample holder from the dovetail at the integrating sphere
transmission port.
4. Mount the sample onto the centre-mount sample holder, making sure it is properly
centreed and secured. Load the assembly into the integrating sphere and set the anticipated angle of incidence using the attached dial.
5. Adjust the iris aperture to full open.
6. Adjust the position of the small spot kit lens assembly on its dovetail rail, changing
the distance between the “C” lens assembly and the sphere until the beam spot obtained
on the centre-mount sample is crisp and well-focused. Make sure that the beam does not
overfill the edges of the sample. In general, the centre-mount spot size and focus will be
optimized when the lens is moved away from the sphere. If it is necessary to reduce the
beam size to eliminate sample overfilling, adjust the iris diaphragm until the spot on the
sample fills approximately 75% of the entire sample surface.
7. While viewing the sample surface through the reference port, check that the sample
beam strikes the centre and does not overfill the sample at the angle selected. This step
may require use of a piece of translucent paper and will be more difficult at greater angles
of incidence. If the beam is off centre or will not fit on the sample, either adjust the
sample mounting in the sample holder or re-adjust the sample beam optics using M3 to
achieve the correct alignment. If any adjustments are made to the optics, make sure the
sample beam still fits within the small spot lens aperture.
Figure 52. The small spot kit beam falling on a sample using one of the centre mount
options.
8. Examine the path of the reference beam inside the integrating sphere. The beam
should strike the reference port without clipping any part of the sample or sample holder.
9. Once the sample beam spot is set, remove the sample from the centre-mount holder,
noting the correct orientation and position. In the case of the jaw style sample holder,
mount a reflectance standard or, in the case of the clip style sample holder, leave the
sample holder empty. Load the sample holder assembly back into the sphere.
10. Collect a Baseline scan. If using a jaw style centre-mount sample holder, the zeroline
standard reference correction may be used.
11. Mount the sample into the centre-mount sample holder. For the jaw style device, the
transmitted component from the sample beam must be eliminated so it is not collected by
the sphere. This can be accomplished by backing the sample with a piece of black felt
cloth. Load the sample holder assembly into the sphere.
12. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
13. Click the Start button.
14. If the standard reference option was used for the baseline scan, the reflectance
spectra is generated automatically. If the simple or zero baseline correction was selected
and the jaw style sample holder was employed, multiply the sample scan data by the
spectral reflectance factors for the calibrated reflectance standard or the data in Appendix
B. If using the clip style centre-mount sample holder, no correction is required.
Reflectance Measurements at the Reflectance Port (Small Spot Kit )
For samples loaded at the sample reflectance port, the DRA small spot kit can be used to
measure a particularly small test sample or a portion of a larger sample. Prior to entering
this procedure, the small spot kit should be installed and aligned. Mirror M3 must always
be installed at the "T" position for small spot kit measurements.
1. Install the centre-mount lens, marked "R", into the small spot kit lens holder. The
arrow marked on the lens should be pointing towards the sphere.
2. Darken the room and drive the instrument to 500 nm.
3. Remove the transmission sample holder from the dovetail at the integrating sphere
transmission port.
4. If the intended sample size is smaller than the reflectance port opening, secure a mask
over the port. The mask should be attached to the reflectance port, and it must remain in
place for both the baseline and sample scans. If available, the optional reflectance port
aperture kit, Labsphere Part No. AS-02021-000 can be used. If the sample is larger than
the port size, place a piece of translucent paper over the reflectance port sample holder
and install the holder at the port.
5. Adjust the iris aperture to full open.
6. Adjust the position of the small spot kit lens assembly on its dovetail rail, changing
the distance between the "R" lens assembly and the sphere until the beam spot obtained at
the reflectance port is crisp and well-focused. Make sure that the beam does not overfill
the edges of the sample. In general, the spot size and focus will be optimized when the
lens is moved closer to the sphere. If it is necessary to reduce the beam size to eliminate
sample overfilling, adjust the iris diaphragm until the spot on the sample fills
approximately 75% of the entire sample surface. Once the beam size is set, remove any
paper at the reflectance port of the sphere, so that the port or mask is open.
7. Load a calibrated diffuse reflectance standard against the reflectance port of the
sphere. The standard should be placed behind the sample port mask or aperture plate, if
one is used. Record one of the baseline scans as directed previously in this chapter.
8. Replace the reflectance standard at the sample reflectance port with the sample. Do
not change the configuration of the integrating sphere in any other way.
9. Click the Setup button and check the parameters. Normally, the setup parameters for
the application should match those used for the baseline scan. If using a previously
defined baseline correction, retrieve the correct baseline.
10. Click the Start button.
11. If the standard reference option was used for the baseline scan, the reflectance
spectra is generated automatically. If the simple or zero baseline correction was selected,
multiply the sample scan data by the spectral reflectance factors for the calibrated
reflectance standard.
Small Sample Masking Techniques
Small samples that do not completely fill the sample reflectance or transmission port
should be measured using masking techniques. Masking in this case may be necessary if
only to mount the sample at the appropriate port. When using the small spot kit to
measure the reflectance or transmission of samples smaller than the port diameter, both
the reference and the sample can be masked such that the port is filled completely.
Generally a black mask is used to prevent reflectance from the mask adding to the
reflectance of the sample. Another reason for a black mask is consistency - a black mask
is always the same and easy to make. The reflection off the black mask is very small and
does not contribute to the reflectance properties of the sample. Simple and effective
masks can be prepared from a piece of cardboard. A manila file is excellent because it is
thin and easily manipulated. The mask must be constructed large enough to fill the port.
The internal surface of the mask should be painted black with flat black Krylon™ paint
or its equivalent. The illustrations in the figures above and below demonstrate the use of a
mask at the transmission and reflectance ports, respectively. The following guidelines
will help when constructing masks:
•
•
•
•
The mask surface area should cover the entire transmission or reflectance port.
The mask aperture should be in the same profile of the sample surface, but
slightly smaller in size.
The sample beam should overfill the mask aperture.
The baseline scan should be collected during reflectance measurements with the
reflectance standard in the same mask geometry. For transmission measurements,
the masked port constitutes the 100% transmission standard.
Note
There are two negatives of using a mask in your analyses. Firstly, using a mask at
either the transmission port or the sample reflectance port reduces the throughput
of the accessory and energy seen by the detector. Secondly, using a mask at the
sample reflectance port upsets the balance between the sample and reference beams
because the reference beam strikes the high reflectance inner surface of the sphere.
If the spectrophotometer is operating in single beam mode, of course, this is not a
problem. Impact of these factors can be minimized if you can localize the beam to
the target area of the sample using the small spot kit so the beam just barely fits
over the edges of the mask.
Large sample reflectance measurements
When measuring large samples that cannot be accommodated within the sample
reflectance port cover, you will need to follow the steps below:
Prior to recording the scan, make sure that mirror M3 is located in the correct position.
To measure a sample::
1. Click the Setup button and set up instrument parameters as required by the application.
Select the %R ordinate scale. The Beam mode should be double.
2. Select the Zero/baseline correction or Zero x std ref correction radio button on the
Baseline tab.
3. Load a Spectralon standard at the reference port and a calibrated reflectance standard,
if available, at the sample reflectance port. If a calibrated standard is unavailable for
reflectance measurements, an uncalibrated Spectralon reflectance standard can be
substituted. Install the port covers over their respective ports.
4. Click the Baseline button.
5. At the 100%T scan prompt, select OK. The standard at the reflectance port serves as
the 100%R reference.
6. At the 0%T scan prompt block the sample beam at the transmission port or remove the
reflectance standard and use the reflectance port cover as a light trap.
7. Remove the reflectance port cover, the spring loaded sample holder, the sample shelf
and unscrew the dovetail using a 3mm hex driver.
8. Position and secure your sample up against the reflectance port and start you
reflectance measurement.
The recorded baseline correction will be effective until replaced by a follow-up baseline
scan.
Note
If you have adequate control over the room lighting, it is recommended that you
run your 0%T scan without the reflectance port cover in place. In this configuration
the room itself becomes the light trap.
Applying a Nitrogen Purge
The Cary 4000/5000/6000i instruments are fitted with connection points for purging the
optical system with nitrogen to enhance the performance of each instrument at extremes
of its range. More details are provided in the Cary Hardware operation manual (part
number 8510197200), supplied with the instrument.
Nitrogen supplies are not available from Varian but may be obtained from commercial
suppliers. Liquid nitrogen (in conjunction with a heat exchanger) is recommended
because it is generally less costly than compressed nitrogen and is of better quality.
Where compressed nitrogen must be used, the gas must be dry, oil–free and
uncontaminated. Do not use compressed nitrogen from a supplier who uses oil or water in
the compression process (these methods leave fine particles of oil or water suspended in
the nitrogen that may be deposited on the instrument optics). Only use nitrogen from a
supplier who fills containers from immersion pumps lubricated with liquid nitrogen.
Note
The instrument warranty will be void if damage is caused by the use of contaminated nitrogen.
Operating pressure at the pressure regulator (# 7 in figure 53) for the nitrogen purging
system is 83 to 172 kPa (12 to 25 psi). Use a suitable regulator and gauge assembly to
ensure that the nitrogen supply is maintained at the correct pressure.
Nitrogen supply tubing should be clean, flexible plastic tubing 6 mm (1/4“) inside
diameter (Tygon PVC or equivalent). Do not use rubber tubing as this is usually treated
internally with talc which will be carried into and contaminate the instrument optics.
The nitrogen system should include a manifold assembly with inlet from the supply and
two outlets for connection to the instrument. Manifold outlets should each be fitted with a
stop valve and flowmeter for control of gas flow to the instrument. Flow meters should be
adjustable for flow rates of 0 to 30 litres per minute (0 to 64 cubic feet per hour). Refer to
the figure below for more details.
Figure 53.
The position of flowmeters when purging with nitrogen:
1.
2. External
Instrument * DRA
3. Tubing
4. Flow meters
5. Shut-off
6. Manifold
valves
7. Pressure
8. Nitrogen
regulator
control valve
*Refers to the purge inlet labelled "Instrument".
The DRA accessories each have an inert gas purge capability for reducing water vapour
absorption inside the integrating sphere. The gas nozzle is located underneath on the lefthand side of the overhanging accessory. A nitrogen purge can be applied as follows:
1. Install the accessory into the instrument sample compartment.
2. Attach a suitable gas regulator to the gas outlet of a nitrogen dewar or N2 cylinder.
3. Connect a suitable hose between the regulator outlet and the nitrogen connector on the
accessory.
Figure 54. Attach the connector on the hose Figure 55. The connectors snap together.
to the connector on the under side of the
integrating sphere.
4. Crack open the shut off valve until the flow meter indicates the flow of nitrogen. Wait
approximately five minutes before proceeding with reflectance or transmission
measurements.
NIR reflectance measurements (not for Cary 4000)
Note
Parameters activated by a radio button that are not specifically mentioned in the
following procedure should be set to ’Off’ (e.g. the Signal-to-noise mode radio
button). These parameters will not affect the procedure.
1.
Click the Windows Start button, then Programs, then Cary WinUV, and then Align.
2.
Click the Setup button.
3.
Set the following parameters:
Cary tab
X mode: Mode
Nanometers
X mode: Start
2000
X mode: Stop
300
Y mode: Mode
%R
Y mode: Y min
0.00
Y mode: Y max
100.00
Show status display
ON
Options tab
SBW/Energy: Beam
mode
Double
SBW/Energy: Slit
height
Reduced
Source/Detector:
Lamps
UV-Vis
Source: Source
changeover (nm)
350.0
Source: Detector
changeover (nm)
800.0
Independent tab
Independent control
ON
Measurement mode
Auto
UV-Vis controls
Ave time (s)
0.1
Data interval (nm)
1.000
Scan rate (nm/min)
600.00
SBW (nm)
2.00
NIR controls
Ave time (s)
1.000
Data interval (nm)
2.000
Scan rate (nm/min)
120.00
Energy level
3.00
Baseline tab
Correction
Zero correction
Autostore tab
File Storage: Storage
Storage on
(prompt at start)
Note
The NIR detector is noisier than the UV-Vis detector, so a higher Signal Averaging
Time (Ave time) may need to be set in the NIR. To obtain a constant signal-to-noise
ratio over the entire wavelength range, set a value in the Signal-to-noise field. If
you require a faster scan rate, increase the Data interval or lower the Ave Time.
4.
Place the appropriate PTFE reference plate over the sample port.
4.
Place the appropriate PTFE reference plate over the sample port.
5. Press the ’Goto’ button to open the ’Goto wavelength’ dialog. Enter ’801’ in the
wavelength field and click OK. The instrument will then drive to 801 nm.
Note
Note the SBW reading in the Status Display dialog.
6. The SBW reading needs to be at approximately 18. This can be adjusted by changing
the NIR Energy level in the Setup page, under the Independent tab. If the reading is
greater than 18, raise the value of the Energy level field. If the SBW is under 18, lower
the energy level. Once the Energy level has been adjusted, you will need select OK in
order to note the change to the SBW reading. Then press the Goto button and again drive
the instrument to 801 nm by entering ’801’ in the wavelength field and pressing OK. This
procedure may need to be repeated in order to reach the required setting. Please note that
each time you adjust the Energy level reading, you must also drive the instrument to
801 nm.
7. Select the Baseline button from the Scan dialog. Follow the on-screen prompts to
perform a 100%T baseline scan and a 0%T baseline scan.
Hot Tip
When performing reflectance measurements, remove the PTFE reference disk from
the sample port and allow the light to be trapped by the magnetic port covers.
8. Once the baseline correction is complete, the Ordinate status display in the top left
corner of the dialog will show ’Zero baseline’ in red text.
9. Clamp the sample over the sample port. The sample should be homogeneous,
substantially flat, and large enough to completely cover the image.
10. Press the Start button. The Save As dialog will appear, allowing the method to be
saved as either a data file or a batch file. If the file is saved as a batch file, all of the
method parameters will be stored with the scan.
Specular-only reflectance measurements
Note
Parameters activated by a radio button that are not specifically mentioned in the
following procedure should be set to ’Off’ (e.g., the Signal-to-noise mode radio
button). These parameters will not affect the procedure.
1.
From the Setup menu, set the following parameters:
Cary tab
X mode: Mode
Nanometers
X mode: Start
800
X mode: Stop
300
Y mode: Mode
%R
Y mode: Y min
0.00
Y mode: Y max
100.00
Scan controls:
Ave time (s)
0.100
Scan controls: Data
interval (nm)
1.000
Scan controls: Scan
rate (nm/min)
600.00
Options tab
SBW/Energy: Fixed
SBW
ON
SBW/Energy: SBW
(nm)
2.00
SBW/Energy: Beam
mode
Double
SBW/Energy: Slit
height
Reduced
Source: Lamps
UV-Vis
Source: Source
changeover (nm)
350.0
Baseline tab
Correction
Zero
baseline/correction
Autostore tab
File Storage: Storage
Storage on
(prompt at start)
2.
Place the specular port plug into position.
3.
Place the appropriate PTFE reference plate over the sample port.
4. Select the Baseline button from the Scan dialog. Follow the on-screen prompts to
perform a 100%T baseline scan and a 0%T baseline scan.
Hot Tip
When performing specular measurements, block the sample beam in the
transmission position with a black masking.
5. Once the baseline correction is complete, the Ordinate status display in the top left
corner of the dialog will show ’Zero baseline’ in red text.
6. Clamp the sample over the sample port. The sample should be homogeneous,
substantially flat, and large enough to completely cover the image.
7. Press the Start button to perform the scan of the total (specular and diffuse)
reflectance of the sample.
8. Remove the specular port plug and install the light trap in its place and click the Start
button to collect the diffuse-only data.
9. From the main Scan window, click on the Calculator icon
Maths dialog.
to open the open the
10. On the graph displayed, highlight the first scan (of the total reflectance), by clicking
on it. When the scan is selected, it will be highlighted in red.
11. From the Maths dialog choose Selected Trace and then the ’-’ (minus) sign.
12. On the graph displayed, highlight the second scan (of the diffuse-only reflectance),
by clicking on it. When the scan is selected, it will be highlighted in red.
13. From the Maths dialog choose Selected Trace and then the ’=’ (equal) sign.
14. The results of this specular data equation will be displayed in a new graph.
Measurement calibration and corrections
Calibration
The detector calibration functions store separate sets of correction factors for the
instrument detectors and for the DRA detectors, so both require calibrations. The
instrument will recognize when an external DRA has been connected to the instrument
and will restore any previous calibrations stored in the external DRA.
Calibrations are performed using the Validate application, under the Calibration menu.
Caution
Both instrument and DRA are calibrated at the factory and should be recalibrated only
when tests indicate the need for it.
When should I perform a calibration?
Below are some common reasons that may indicate the necessity for calibration.
Calibrate PGA (Programmable Gain Amplifier)
PGA calibration should be executed each time a DRA is installed in a Cary instrument
for the first time, and after each time it is removed. At other times, the need for it may be
seen on an uncorrected baseline as steps or plateaus or on a corrected baseline as small
spikes-either positive or negative.
UV/VIS 0%T Correction
This calibrates the photomultipliers for 0%T (electronic zero) effects. This is executed
every time the instrument is switched on except if a DRA is installed (where the DRA
correction factors stored in the DRA EEPROM are used).
Instrument check: If high precision is needed at high absorbance, measure the 0%T error
at 500 nm in the UV-VIS (blocked sample beam). The error should be less than 0.01 %T.
Calibrate with the instrument fully warmed up. It may be desirable to calibrate Calibrate
PGA prior to this. Click here for the instrument parameters.
NIR 0%T Correction
This is the NIR equivalent for 0%T error.
Instrument check: After instrument has fully warmed up, go to wavelength 1200 nm with
grating change at 800 nm and block the sample beam with a black metal mask. If the
error exceeds 0.1 %T calibration may be required.
Calibration using Cary Win UV Software
The recommended method for performing calibration is by using the Auto Calibrate
function in the Validate application.
Caution
Both instrument and DRA are calibrated at the factory and should be recalibrated only
when tests indicate the need for it. Failure to complete or the use of incorrect filters may
render the instrument unusable.
Signal processing
This causes the Cary system to calibrate the programmable gain amplifiers on the
photomultiplier tube. This test is performed during initialization of the Cary
4000/5000/6000i instruments.
UV/Vis 0 %T correction
This causes the Cary system to close the shutter and calibrate the UV/Vis detector for 0
%T errors. If a DRA is connected a mask must be placed in front of the transmission port
(rear instrument beam) during the calibration process. The software will prompt you for
this.
Note
This calibration is part of the normal initialization procedure, however calibration
is advised when working at high absorbance where a repeat calibration after the
instrument is fully warmed up would be beneficial.
NIR 0%T correction
This closes the shutter and calibrates the NIR detector for 0 %T errors. If a DRA is
connected a mask must be placed in front of the transmission port (rear instrument beam)
during the calibration process. The software will prompt you for this.
Auto calibrate
Will perform all the calibrations relevant to the instrument and DRA combination being
used. User interaction is required if a DRA is in place.
Wavelength status
This allows the user to view the Wavelength offsets stored in the EEPROM.
Performing a correction to ASTM E903-C-OS/2
If you are using a NIST Standard Reference material (SRM) (e.g. White ceramic tile) as
the reference disk then you should enter the calibrated reflectance values as a continuum
in the Cary system. To do this, create an ASCII file and enter the list of X and Y data
pairs (separated by commas). Save this ASCII file in the ’.CSV’ format.
If you are using the PTFE reference disk supplied with the DRA, then the following
values may be used. These values are approximate only. The PTFE reference plate has
not been calibrated. The reflectance values are representative of the PTFE reference
plates supplied with the DRA(3).
1.
Click the Windows Start button, then Programs, then Cary WinUV, and then Scan.
2.
Click the Setup button.
3.
Set the following parameters:
Cary tab
X mode: Mode
Nanometers
X mode: Start
300
X mode: Stop
2000
Y mode: Mode
%R
Y mode: Y min
-5.00
Y mode: Y max
110.00
Show status display
ON
Options tab
SBW/Energy: Beam
mode
Double
SBW/Energy: Slit
height
Reduced
Source/Detector:
Lamps
UV-Vis
Source: Source
changeover (nm)
350.0
Source: Detector
changeover (nm)
800.0
Independent tab
Independent control
ON
Measurement mode
Auto
UV-Vis controls
Ave time (s)
0.1
Data interval (nm)
1.000
Scan rate (nm/min)
600.00
SBW (nm)
2.00
NIR controls
Ave time (s)
1.000
Data interval (nm)
2.000
Scan rate (nm/min)
120.00
Energy level
3.00
Baseline tab
Correction
Zero x std
ref correction
Autostore tab
File Storage: Storage
Storage on
(prompt at start)
Place the reference disk or SRM in the DRA.
Run a baseline as follows:
1. Select the Baseline button in the Scan dialog box. Follow the on-screen prompts to
perform a 100%T baseline scan and a 0%T baseline scan.
Hot Tip
When collecting the 0%T baseline scan do not block the beam instead, remove the
PTFE reference disk from the reflectance port and allow the light to be trapped by
the magnetic port covers.
2. Once the baseline correction is complete, the Ordinate status display in the top left
corner of the dialog box will show ’Zero baseline’ in red text.
3. Clamp the sample over the reflectance port. The sample should be homogeneous,
substantially flat, and large enough to completely cover the image.
4. Click the Start button. The Save As dialog box will appear, allowing the method to
be saved as either a data file or a batch file. If the file is saved as a batch file, all of the
method parameters will be stored with the scan. The sample will be auto-corrected for
100%T, 0%T and Standard Reference.
5.
Place your sample in the DRA and click Start.
The Cary will scan your sample and automatically perform the ASTM correction.
Maintenance
The performance of the integrating sphere is dependent on the efficiency of the coating
on the sphere and the reference plates, and the cleanliness of the optical components of
the accessory.
Keep the reference plates clean; if they become dirty, new plates are available from
Varian. The part number for the flat PTFE reference plate is 04 1014439 00, and for the
protruding PTFE reference plate 04 101988 00.
For technical support please contact Varian on:
Varian Analytical Instruments, Melbourne
679 Springvale Road
MULGRAVE, VIC 3170
Cleaning and Inspection
You may gently flush the accessory with pure nitrogen to remove water.
Perform this maintenance procedure weekly when the accessory is in use. Record the
results in the accessory or instrument maintenance log.
1. Remove the accessory from the wood container and set it on a flat surface.
2. Check that each mirror mount in the optics chamber is fastened securely to the base
plate.
3. Blow clean air or nitrogen over the transfer optics to remove any dust lying on the
mirror surfaces.
4. Examine the surface of each mirror using a flashlight. Look for dust particles or film
damage that might scatter the incident radiation.
5. Remove the reflectance standards and centre mount plug from the integrating sphere
or box. Inspect the reflective surfaces of the standards for damage or dirt. Use a
magnifying glass, if necessary.
6. Inspect the reflecting surface of the centre mount plug.
7. Illuminate the sphere interior with a flashlight and inspect the surfaces for soiling.
Blow out any debris using clean dry air or nitrogen.
8. Re-install the centre mount plug and reflectance standards to their respective sphere
ports or store the entire accessory in the wooden container.
Mirror Cleaning Procedure
Hot Tip
Holding the mirror under a bright light will show up any marks on the surface of
the mirror.
The transfer optics mirrors should not be touched or handled with bare fingers. Never
clean the mirrors with abrasive cleaners or tissue paper. The mirrors have a protective
magnesium fluoride coating to allow cleaning if necessary. The following cleaning
procedure is recommended:
1. Remove the mirror fixture.
2. Spray the mirror with Fantastic Spray Cleaner.
3. Rinse the mirror with distilled water.
4. Repeat until the water sheets off the mirror.
5. Blow dry the mirror surface with a stream of clean nitrogen.
6. Reinstall the mirror fixture and check the alignment of the optics.
Standards
Reference surfaces for reflectance and transmission in the solar wavelengths are available
from (among others) Labsphere in the USA, the National Institute of Standards and
Testing (NIST) in the USA, and from the National Physics Laboratory (NPL) in the UK.
Labsphere provide reference surfaces with reflectances varying from 2%R to 99%R.
Labsphere may be contacted at:
P.O. Box 70
Shaker St,
North Sutton, N.H. 03260
Tel: 603 927 4266
Fax: 603 927 4694
NIST provide a range of transmission filters and solutions, and also provide the following
materials for reflectance:
•
•
•
•
First surface, Aluminium on glass
First surface, Gold on glass
Second surface, Aluminium on fused quartz
Second surface, Aluminium on fused quartz, with wedge.
For more information:
Office of Standard Reference Materials
Room 205, Building 202
National Institute of Standards and Technology
Gaithersburg, MD 20899
Reference Materials available from NPL for reflectance include:
•
•
•
•
•
•
Russian opal
White ceramic tile
Black ceramic tile
Colored tiles
Aluminium mirrors
Absorbing glass.
NPL also have transmission standards of neutral glass filters with transmission values of
0.92 to 0.001.
Contact:
Division of Electrical Science
National Physical Laboratory
Teddington, Middlesex
TW11 OLW
UK.
Troubleshooting
Warning This instrument contains electrical circuits, devices, and components
operating at dangerous voltages. Contact with these circuits, devices and
components can cause death, serious injury, or painful electrical shock.
To avoid electrical shock operators and other unauthorized personnel must
never remove the main cover. This must be opened only by Varian-trained,
Varian-qualified, or Varian-approved service engineers.
Problem
Solution
Measurements on
standard materials are
not producing certified
values.
Ensure that you are referring to the hemispherical reflectance
values of the SRM, not the directional and hemispherical values.
Ensure that your PTFE disks are clean and in good condition.
If you are calibrating the PTFE disk, you need only apply the
necessary correction to your measured values.
The signal-to-noise
ratio is low.
This can be caused by degraded sphere coating, poor detector
performance, the lamps requiring replacement, unclean mirrors
or lens, or bad alignment.
Check the sample port image, and re-align the accessory if
necessary.
Check that the lens and mirrors are clean, and carry out a Zero
%R error check.
A Failure to initialize
instrument error
message occurs.
Error number:
9:9303SEQ:E9303
Check that the:
The DRA is plugged in.
The beams are not blocked.
The DRA is not out of alignment.
A Cary Exception error An ADL command is necessary to clear this error. Click here to
occurs.
view/print a PDF instructing you how to use this ADL.
References
1. Weidner V.R., Hsia J.J: J.Opt.Soc.Am. 71/7 (1981)
2. Zwinkels J., Dodd C.X.: Workshop on Optical Property Measurement
Techniques, Commission of the European Communities. (1988).
3. Weidner V.R., Hsia J.J., Adams B.:Applied Optics 24/14 (1985)
Alignment targets
l
(nm)
250
260
270
275
280
290
300
310
320
325
330
340
350
360
370
375
380
390
400
450
500
550
600
650
R
0.973
0.976
0.978
0.979
0.980
0.982
0.984
0.985
0.987
0.988
0.988
0.989
0.990
0.990
0.991
0.991
0.991
0.992
0.993
0.993
0.994
0.994
0.994
0.994
l
(nm)
700
750
800
850
900
950
1000
1050
1100
1150
1200
1250
1300
1350
1400
1450
1500
1550
1600
1650
1700
1750
1800
1850
R
0.994
0.994
0.994
0.994
0.994
0.994
0.994
0.994
0.994
0.994
0.993
0.993
0.992
0.991
0.991
0.992
0.992
0.992
0.992
0.991
0.990
0.990
0.990
0.986
l
(nm)
1900
1950
2000
2010
2020
2030
2040
2050
2060
2070
2080
2090
2100
2110
2120
2130
2140
2150
2160
2170
2180
2190
2200
2210
R
0.985
0.984
0.981
0.979
0.978
0.976
0.975
0.973
0.972
0.971
0.970
0.969
0.968
0.967
0.966
0.964
0.964
0.965
0.967
0.970
0.973
0.975
0.977
0.977
l
(nm)
2220
2230
2240
2250
2260
2270
2280
2290
2300
2310
2320
2330
2340
2350
2360
2370
2380
2390
2400
2450
2500
R
0.978
0.978
0.977
0.977
0.976
0.976
0.975
0.974
0.972
0.971
0.970
0.968
0.966
0.965
0.964
0.963
0.963
0.962
0.962
0.961
0.960
Sample Mounting Kits
The following mounting options are available:
Item
Description
Part number
Double aperture
Mount and mask for checking the photometric
accuracy of the instrument and accessory.
79 100473 00
Centre mount
sample holder
(jaw)
Jaw style, variable angle, centre mount sample holder.
Fits into the top of the sphere and can be located at
79 100475 00
difference angles. Samples are clamped into place.
Centre mount
sample holder
Clip style, variable angle, centre mount sample holder.
79 100476 00
Fits into the top of the sphere and can be located at
(clip)
difference angles. Samples are clipped into place.
Centre mount
cuvette holder
Centre mount holder for cuvettes. Fits into the top of
the sphere.
79 100387 00
Transmission
cuvette holder
Holds standard 10 mm quartz cuvettes in %T port of
DRA. Mounts to the transmission port holder.
79 100383 00
Solid sample
holder
Aperture kit
79 100478 00
Kit containing 3 x apertures (1 mm, 2 mm and 5 mm),
4 small spacers and 1 large spacer. Select an aperture
plate slightly smaller in diameter than the sample
79 100381 00
surface and a spacer small enough to clamp the sample
against the outer aperture plate surface.
Small spot kit (with apertures)
Samples must be greater than 3mm in width and length. The kit includes the following:
Item
Description
Part number
Small spot kit
Kit containing, iris and lens for focusing the sample
beam for taking measurements of small samples at the 79 100472 00
reflectance port.
Powder cell kit
Item
Description
Part number
1 x Powder cell
kit
Fits inside the reflectance sample holder in the same
manner as the reflectance standard. Each sample
holder comes as a set: one cell with a Spectralon insert 79 100477 00
for use as a reflectance standard, and an empty cell for
loading the powdered sample
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