www.harricksci.

com

THE PRAYING MANTIS

USER'S MANUAL

HARRICK SCIENTIFIC PRODUCTS, INC.

141 Tompkins Ave, 2"d fioor Pleasantville, NY 10570 (800) 248-3847 FAX (914) 747-7209

f:f,l~~~G-<:>~,

TABLE OF CONTENTS

"'--~~~~~~~~~~~~~~~~~~~

General Information
Unpacking ................................... ...................................... .. ............................... .. ........................
Technical Support... ... .......... ............................. .. .. ....... ......... ............... ... .. .......... ... .. ... .................
Feedback .. ..... .... ... .. ... .. ....... .. ....... .. ... .. .. ..... . ... . .... ..... .. .. .... . ... . ..... ... ...... ..... ...... . ...... ..... ... .............. .

1
1
1

About the Praying Mantis

Installation and Alignment

Open Beam Spectrum ................. ................................................................................................
Getting Ready ........ ................................................................................... ........................ ...........
Purge Installation .................... .......................................................... ...........................................
Installing the Praying Mantis ................... ................................................ .................................
Aligning the Praying Mantis TM ........................ . .................... . .... . ......... . .... . ....... .. ............... ...........
Verifying the Throughput ........................................................................................... ........... .......
Specular Reflectance ........................................................... ..... ..................................................

3
3
4
5
6
8
8

Operation
Background Spectrum ........................................ .... ........ ......... ....................................................
Sample Spectrum ........................................................... ........ ...... .... ......... ..................................

9
9

Ambient Chamber .... ...... .. ..... ......... ..... ..... ................................... ............. ..... .. 10
HVC
About the High Temperature Reaction Chamber ........................................................... .. ...........
Getting Ready ......... .... ..................................................................... .............. .... .... ......................
Window Installation .................... ..................................................................................................
Dome Installation ....................... ..................................................................................................
Installing the HVC ... ............................................................ .. .......................................................
Fluid/Electrical Connections ............................ ............................................................. ......... ......
Collecting the Background Spectrum ........................................................................ .. .... ............
Sample Spectrum ........ ......... ..... .. ....... .. .......................................................................................

12
13
14
15
16
17
18
19

CHC
About the Low Temperature Reaction Chamber . . . .. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. .. . .. . .. . . . .. .
Getting Ready .... .......... ...................................................... ............ ..... .. .... ...... ................ ..... ... .....
Window Installation ................... ...... ......... .. ... ......................................... ... ............... ... .... ... ..........
Dome Installation ........................... ..... ...... ................ ..... .... ... ......... .......... ..... ..................... .... ..... .
Installing the CHC ... ............... ........................ ............ ............................ .... .................. .... ........ ....
Fluid/Electrical Connections ................................................. ..................................... .... ..... .........
Collecting the Background Spectrum . ..... .. ... .. .. ... .... .... ..... .... .. ... .... ..... .. ... ... .......... ... ... .. ... .. .... .... ..
Sample Spectrum ....... .................. ........................................................................... :...................

DRP-M-04

20
21
22
23
24
27
28
29

TABLE OF CONTENTS

Reaction Chamber Maintenance

Leak Checking ............ ... .. ................. ...... ..... .. ....... ..... ......... ............. ........... ......... ... ..... ................
Cleaning the Reaction Chambers ............... ..... ....... ....................... ....................... .................. ....
Replacing the 0-rings .... ......... .. ... .......... ..... .............. ..... .......................... ......... ......... .... ..............
Replacing the Heater ................ ... ................. ...... ................ .. ......................... ... ... ..... ...................
Replacing the Thermocouple . .. ..... ...... .... ...... ............. ..... ..... ..... .. ...... ..... ..... ... . ... .. ......... ...... ........

30
30
31
31
32

Appendix A
Mounting the Harrick Rail Plate ................ ....... ..................... .. ... ...... ....... ..... ................. .......... ..... 33

Appendix B
Optional and Replacement Parts .................................................................. .. ... ... .. ..... .... ...... ..... 35

f~f,i~lH~IG-<>~(

GENERAL INFORMATION

UNPACKING

Before Installing the Praying Mantis Diffuse Reflection

Accessory make sure all the parts on the included check-off
list are present. If any parts are missing or damaged,
contact Harrick Scientific immediately.

TECHNICAL SUPPORT

For additional information please contact our

Technical Support Center at 800-248-3847 between 9 a.m.
and 5 p.m. EST; or e-mail your questions to:
[email protected]

FEEDBACK

Your comments and suggestions are welcome.

send them to:
Harrick Scientific Products, Inc.
PO Box 277
141 Tompkins Ave, 2"d floor
Pleasantville, NY 10570
Phone: 800-248-3847; Fax: 914-747-7209
E-mail: [email protected]
Web: www.harricksci.com

1of 36

Please

~:f,t~~~QI(:~'

ABOUT THE PRAYING MANTIS

---~~~~~~~~~~~~~~~~~--~--

The Praying Mantis (DRP) accessory is specifically designed for examining powders by diffuse
reflection spectroscopy. The optical design of the Praying Mantis incorporates two 6X, 90 off.
axis ellipsoid mirrors. The ellipsoids are optically arranged so that their near focal points coincide
and they are arranged to discriminate against the collection of specularly reflected radiation. This
is achieved by placing the collecting ellipsoid 60 away from the direction of the specularly
reflected radiation. The sample Is placed In the common focal point of the two ellipsoid mirrors.
The beam Is condensed to a spot less than 2mm in diameter. This allows analysis of very small
quantities of sample. A purge fitting and two purge seals are provided if purging is desired.
The sample is loaded in to a sample cup. Two cups are included, regular and micro-sampling
cups. The sample is typically diluted in a non-absorbing powder. The same non-absorbing
powder is used to collect the background spectrum. An optional ambient chamber allows the
sample to be loaded in a controlled atmosphere (glove box) and then analyzed without being
exposed to room atmosphere.
Two reaction chambers are available for use with Praying Mantis, the high temperature
chamber HVC and the low temperature chamber CHC. The reaction chambers enable a reaction
gas to be introduced and reacted with the sample so that the reaction can be studied in situ,
reaction rates determined and intermediates and reaction products identified. The reaction
chambers are enclosed with a dome with three windows, two for the spectrometer radiation to
enter and exit the chamber and the third for viewing, illuminating, or irradiating the sample. This
enables the use of the reaction chambers for photochemical studies. The standard material for
the viewing window is UV quartz and the other two windows are KBr.

2 of 36

INSTALLATION AND ALIGNMENT

OPEN BEAM SPECTRUM

Prior to installation:
Make sure all sample holders are removed from
the sample compartment.
Prior to installation collect an open beam
background spectrum (no accessory in the
sample compartment). This spectrum should be
used later to verify the throughput of the Praying
Mantis.

GETTING READY

Before installing the Praying Mantis, familiarize yourself

with the accessory and its various components by
referring to the drawing of the Praying Mantis rM found
below (Figure 1).

M5 Cap

Purge Line Fitting

Window

Thumbscrew
Purge Sleeve
Thumbscrew (2)
Foam Purge Seal
Purge Door

Locking
Mechanism
Knob
Rail Plate
Height Adjustment Knob
Sample Stage Mounting Screw

Figure 1 Front View of the Praying Mantis

3 of 36

INSTALLA T/ON AND ALIGNMENT

PURGE INSTALLATION

PURGE SLEEVES

Loosen the thumbscrews and push the purge sleeves in

to retract them (Figure 2).

Thumbscrew
Purge Collar

Foam Purge Seal

Figure 2 Purge Sleeves

PURGE LINE

For quicker purging or If the spectrometer has windows

on the beam ports, connect an additional purge line to the
fitting on the Praying Mantis as illustrated in Figure 3.

Purge Fitting

Figure 3 Purge Line

4 of 36

INSTALLATION AND ALIGNMENT

INSTALLING THE PRAYING

MANTIS

If your spectrometer is equipped with rails:

Install the Praying Mantis 1 M onto the rails.

RAIL MOUNTING

NOTE:

If you received the Harrick rail plate with your Praying

Mantis, first mount the supplied rails directly onto the floor
of the sample compartment (see Appendix A).

FIXED FLOOR MOUNTING

Move the Praying Mantis along the rails until the

spectrometer focal point is in the center of the
attachment.
Lock the Praying Mantis in place by tightening
the locking mechanism knob.
Extend the purge sleeves until they firmly contact
the sides of the sample compartment.
Lock the purge sleeves in place with the
thumbscrews.

Install the Praying Manti srM onto the floor of the

sample compartment using the base plate
provided.
Extend the purge sleeves to the walls of the
spectrometer and tighten the thumbscrews on the
purge collars.

5 of 36

INSTALLATION AND ALIGNMENT

ALIGNING THE
PRAYING MANTIS

The Praying Mantis has been pre-aligned prior to

shipment. Hence It requires only minor adjustments to
optimize its performance.
Open the door on the front of the attachment
(Figure 1).
Slide the alignment fixture (Figure 4) into the
Praying Mantis rM, with the horizontal mirror
going in first. In this orientation, the tilted mirror
is in the sampling position.
Gently push the alignment fixture in against the
stop.

Tilted Mirror

Figure 4 Alignment Fixture

Remove the plastic caps over mirrors M2 and

MS. This allows access to the turn and tilt
adjustments for these mirrors (Figure 5).
Set the spectrometer to measure the "energy"
on the detector.
Adjust the turn and tilt controls for MS with the
supplied 3/32" hex driver until the signal on the
detector is maximized.
Adjust the height of the alignment fixture with
the height adjustment knob to maximize the
signal.
Adjust the turn and tilt controls for M2. Repeat
this sequence until there is no further increase
in the signal on the detector.

6 of 36

INSTALLATION AND ALIGNMENT

Figure 5 Interior View of the Praying Mantis

If using rail mounting:

Loosen the thumbscrews on the purge sleeves.

Unlock the locking mechanism.

Slide the Praying Mantis r M along the rails until

the signal is maximized.

Lock the locking mechanism, extend the purge

sleeves to the walls of the spectrometer and
tighten the thumbscrews on the purge collars.

7 of 36

INS TALLATION AND ALIGNMENT

VERIFYING THE
THROUGHPUT

Make sure that the specified background

spectrum is the previously collected open beam
background spectrum.
Collect a transmittance spectrum with the Praying
Mantis TM in the sample compartment.

NOTE:

To maximize the performance of your accessory, it

should be tested before first use and at regular intervals
thereafter.

90 ..,...-~~~~~~~~~~~~~~

80
70

60

~ w

.i

J :~
20
10
O ;--~-.-~----..~~.--~..,....~-.-~.......,.~

4000

3500

3000

2500
2000
Wavenumber cm- 1

1500

1000

Figure 6 Praying Mantis Throughput

SPECULAR REFLECTANCE

Read the maximum value at 2500 cm-1

The Praying Mantis throughput at that
wavenumber should be at least 40% and the
spectrum should resemble the Praying Mantis
throughput spectrum shown above.

Slide the alignment fixture (Figure 4) into the

Praying Mantis, with the tilted mirror going in
first. In this orientation, the horizontal mirror is
in the sampling position.
Gently push the alignment fixture In against the .
stop.

The detector now measures the specular

reflectance from the mirror. The energy should
be near-zero. If it is not less than 10% of the
throughput measured earlier, realign with the
tilted mirror or contact Harrick Scientific.

8 of 36

f:f,t~~~Gt<>X'

OPERATION

"-~~~~~~~~~~~~~~~~~~~~

BACKGROUND SPECTRUM

Overfill one of the sampling cups (Figure 7) with

the reference material (i.e. KBr). Use the
provided sample funnel to fill the microsampling
cup.
Level off the surface using a flat blade.
Open the purge door and slide the sample holder
(with the sampling cup going in first) Into the
Praying Mantis, pushing it in against the stop.
Close the purge door.
Make small adjustments to the height of th e
sample using the micrometer to maximize the
signal on the detector.
Record the background spectrum.

Standard Sampling Cup

Microsampling Cup

Figure 7 Sampling Cups

SAMPLE SPECTRUM

NOTE:

Replace the reference material with th e sample.

Record the sample spectrum.

If the sample Is a strong absorber it may need to be

diluted (approximately 5%) In a nonabsorbent matrix.

9 of 36

f:f,t~~~Gt<:>*'

AMBIENT CHAMBER

----------------------~

USING THE OPTIONAL

AMBIENT SAMPLE
CHAMBER

Before using the ambient chamber, verify that the

windows, o-ring and groove on the bottom of the
dome are clean and free of dust (see page 17).
Put the ambient chamber in a glove box or similar
enclosed environment.
Unscrew the two thumbscrews to remove the
dome.
Carefully fill the sample cup with the reference.
Clean up any spills.
Install the dome making sure that the larger
orientation slot on the dome engages the
orientation pin on the ambient chamber.

Dome

Orientation Slot

Orientation Pin

Ambient Chamber

Figure 8 The Ambient Chamber

Remove the sealed ambient chamber from the

glove box.
Open the purge door and slide the ambient
chamber into the Praying Mantis TM, orienting it so
that the two notches on the bottom of the ambient
chamber go in first.
Close the purge door.

10 of 36

AMBIENT CHAMBER

Make small adjustments to the height of the

sample using the micrometer to maximize the
signal on the detector.
Record the background spectrum.
Replace the reference material with the sample.
Record the sample spectrum.

11 of 36

HVC

ABOUT THE HIGH TEMPERATURE REACTION CHAMBER (HVC)

The HVC is designed for operation up to 910C under vacuum (the lifetime of the heater is
significantly reduced at temperatures above 450C). The pressure range is from high vacuum to
pressures up to 3.44MPa or 25.8 ktorr (the high pressure dome is required for pressures above
133 Pa or 1 ktorr). At higher pressures, the maximum operating temperature may be lower
HVC is made of chemically resistant 316 stainless steel. Within the chamber Is a temperaturecontrolled sample stage with integral sample cup. This stage incorporates a cartridge heater and
a thermocouple. It Is thermally isolated from the outer chamber wall. A water-cooling jacket
controls the temperature of the outer surface of the chamber and windows during high or low
temperature operation. The reaction chamber has three gas ports for evacuating, pressurizing or
flowing gas through the sample. These ports are equipped with 1/4" VCO fittings. The vacuum
port leads directly under the sample cup; the two gas por1s lead into the sides of the chamber.
The chamber is enclosed with a dome with three windows. two for the spectrometer radiation to
enter and exit the chamber and the third for viewing, illuminating, or irradiating the sample. This
enables the use of the reaction chambers for photochemical studies. The standard material for
the observation window is UV quartz and KBr for the other two windows.

CAUTION:
Parts for the high pressure and low pressure domes should not be exchanged. The high
pressure domes undergo high pressure testing and are guaranteed to worl< under the rated
pressure.

12 of 36

HVC

GETTING READY

Before installing the High Temperature Reaction Chamber

(HVC) familiarize yourself with it by referring to the
drawing of the HVC found below (Figure 9).

HVC Dome

Gas Inlet/Outlet
Gas Outlet

Mounting pins (2)

Inlet/Outlet

Heater
Connector
Heater Access Hole

Figure 9 The High Temperature Reaction Chamber HVC

13 of 36

HVC

WINDOW INSTALLATION

If the windows are not already installed or need to be

cleaned or changed follow the steps below (Figure 10).

NOTE:

The observation window is the window that is located

between the two semicircular indentations on the rim of
the dome.
Insert an o-ring in one of the window ports.
Hold the retaining ring upside-down and
place a PTFE washer inside.
Then carefully place a window on top of the
PTFE washer.

Hold the retaining ring so that it continues to

retain the window and thread it into the
window port.
Tighten to secure the window in place using
the tool provided for tightening and loosening
the retaining rings.
Repeat these steps until all three windows
are installed.

NOTE:

Be careful not to touch the windows during Installation.

Retaining Ring

I
(J'

Window
Dome

PTFE Washer

Semicircular Indentation (2)

Figure 10 Installing the HVC Dome Windows

14 of 36

HVC

DOME INSTALLATION

Although it is not necessary to install the dome until later,

it is recommended to become familiar with the procedure
before proceeding to the next step.
Prior to installation of the dome make sure that
the o-ring and groove on the bottom of the dome
are clean and free of dust.
Retract the retaining plates on the HVC as far as
possible .
Install the dome making sure that the orientation
slot on the dome engages the orientation pin on
the HVC (Figure 11 ).
Slide the retaining plates all the way over the rim
of the dome.
Tighten tn1:: ;etaining plate screws to secure the
dome.

Orientation slot

Relaining Plate

S"e~

Olentalion pin

~
I

Figure 11 Installing the HVC Dome

15 of 36

HVC

INSTALLING THE HVC

Before installing the HVC in the Praying Mantis, make

sure that the Praying Mantis is aligned in the
spectrometer.
Unscrew the thumbscrew on the top plate of the
Praying Mantis (Figure 1).
Carefully swing the top plate of the Praying
Mantis out of the way.
Grasp the sample stage (Figure 12) and unscrew
its mounting screw.
Slide the sample stage slightly to the left to
dislocate Its mounting pins.
Remove the sample stage.
Locate the mounting pins on the side of the HVC
(Figure 9) in the pin holes where the sample
stage was located.
Reinstall and tighten the sample stage mounting
screw.

Mounting Screw

Sample stage

Mounting Pins (2)

Figure 12 Installing the HVC

16 of 36

HVC

Thermocouple

Figure 13 The HVC Installed

FLUID I ELECTRICAL
CONNECTIONS

If temperature control is desired, connect the

thermocouple and the heater (Figure 13) to a
suitable temperature controller.
If the HVC is to be operated at temperatures
above 100C, use 1/4" tubing to connect the two
cooling ports (see Figure 13) to a water
inlet/outlet or a coolant circulator.
If vacuum is desired, connect the gas outlet (1/4"
VCO fitting, see Figure 13) to a vacuum pump or
other source of vacuum using 3/8" l.D. vacuum
tubing. Seal off the two gas inleUoutlet ports.
If reaction or process gas/es are to be passed
through the sample, connect the gas inleUout
ports (1 /4" VCO fitting, see Figure 13) as needed
to the gas source/s. Connect the gas outlet and
seal off any unused gas ports.
If reaction or process gas/es are to be passed
over the sample, seal off the gas outlet. Connect
one of the gas inlet/outlet ports to the gas source
and the other as the outlet.

17 of 36

HVC

COLLECTING THE
BACKGROUND SPECTRUM

Place a sample screen into the sample cup and

locate the plastic overflow tray over the sample
cup (Figure 14).
Fill the sample cup with the reference material
using the provided packing tool.
Draw the
straightedge across the top of the cup to level off
the surface.
Carefully remove the overflow tray.
Install the dome on the HVC (see page 15).
Swing the Praying Mantis rM cover back into place
and tighten the thumbscrew.
Set the temperature and pressure to desired
operating conditions.
Set the spectrometer to measure the "energy" on
the detector.
Adjust the micrometer (Figure 1) to maximize the
signal on the detector.
Collect the background spectrum.

Overflow Tray

Sample Cup

Figure 14 Fiiiing the Cup

18 of 36

HVC

SAMPLE SPECTRUM

Restore the reference material to ambient

conditions.
Remove the dome.
Empty the sample cup. This can be done by
vacuuming out the reference sample or by
removing the HVC from the Praying Mantis and
dumping out the material.
If needed, clean the sample cup.
Fill the sample cup with the sample (follow
procedure in the alignment section).
Install the dome.
Install the HVC into the Praying Mantis if it was
removed to empty the sample cup.
Swing the top plate back into place and tighten
the thumbscrew (Figure 1).
Restore the desired sampling conditions.
Collect the sample spectrum.
Empty the sample cup and clean it before
running the next sample.

19 of 36

f:f,t~~F-!G-<>X'

CHC

'-~~~~~~~~~~~~~~~~~~~~

ABOUT THE LOW TEMPERATURE REACTION CHAMBER (CHC)

The CHC is designed for operation from -150C up to 600C under vacuum. The pressure range
is from high vacuum (133 ~lPa or 105 torr) to pressures up to 304kPa or 2.3 ktorr (for pressures
above 133 kPa or 1 ktorr use either the high pressure dome or use Si0 2 or ZnSe windows). At
higher pressures, the maximum operating temperature may be lower.
The CHC is made of chemically resistant 316 stainless steel. Within the chamber Is a
temperature-controlled sample stage with an Integral sample cup. This stage incorporates a
cartridge heater and two thermocouples, one in the sampling stage and one in the sample cup.
The sample stage is thermally isolated from the outer chamber wall. A water-cooling jacket
controls the temperature of the outer surface of the chamber and windows during high or low
temperature operation. The chamber has three gas ports for evacuating, pressurizing or flowing
gas through the sample. These ports are equipped with 1/4" VCO fittings. One of the ports leads
directly under the sample cup, the other two lead into the sides of the chamber.
The chamber is enclosed with a dome with three windows, two for the spectrometer radiation to
enter and exit the chamber and the third for viewing, illuminating, or irradiating the sample. This
enables the use of the reaction chambers for photochemical studies. The standard material for
the observation window is UV quartz and KBr for the other two windows.

~ CAUTION:
Parts for the high pressure and low pressure domes should not be exchanged.
The high pressure domes undergo high pressure testing and are guaranteed
to work under the rated pressure.

20 of 36

CHC

Before installing the Low Temperature Reaction Chamber

(CHC) familiarize yourself with it by referring to the
drawing of the CHC found below (Figure 15).

GETTING READY

-Dewar

Elevation Adjustment Micrometer

CHC Dome

Gas Outlet

Heater
Connector

Thumbscrew Hole

Cooling Port (2)

Figure 15 The Low Temperature Reaction Chamber CHC

21 of 36

CHC

WINDOW INSTALLATION

If the windows are not already installed or need to be

cleaned or changed follow the steps below (Figure 16).

NOTE:

The observation window is the window that Is located

between the two semicircular indentations on the rim of
the dome.
Insert an o-ring in one of the window ports.
Hold the retaining ring upside-down and
place a PTFE washer Inside.
Then carefully place a window on top of the
PTFE washer.
Hold the retaining ring so that it continues to
retain the window and thread it into the
window port.
Tighten to secure the window in place using
the tool provided for tightening and loosening
the retaining rings.
Repeat these steps until all three windows
are installed.

NOTE:

Be careful not to touch the windows during installation.

Retaining Ring
Window

Dome

PTFE Washer
0-Ring

Semicircular Indentation (2)

Figure 16 Installing the CHC Dome Windows

22 of 36

CHC

DOME INSTALLATION

Although it is not necessary to install the dome until later,

It is recommended to become familiar with the procedure
before proceeding to the next step.
Prior to installation of the dome make sure that
the o-rlng and groove on the bottom of the dome
are clean and free of dust.
Retract the retaining plates on the CHC as far as
possible.

Install the dome making sure that the orientation

slot on the dome engages the orientation pin on
the CHC (Figure 17).
Slide the retaining plates all the way over the rim
of the dome.
Tighten the retaining plate screws to secure the
dome.

Orientation slot
Retaining
Plate (2)

Figure 17 Installing the CHC Dome

23 of 36

CHC

INSTALLING THE CHC

Before installing the CHC in the Praying Mantis TM, the

Praying Mantis TM should have been aligned In the
spectrometer.
Unscrew the thumbscrew on the top plate of the
Praying Mantis TM .
Carefully swing the top plate of the Praying
Mantis TM out of the way.
Grasp the sample stage and unscrew its
mounting screw.
Slide the sample stage slightly to the left to
disengage its mounting pins.
Remove the sample stage.
For spectrometers with a low working height (2" or less),
some additional assembly is required to mount the CHC
on the Praying Mantis. This includes the Varian FTIR
spectrometers with serial numbers starting with DRPDl4,
DRPDIS, DRPDl6, DRPDl7 and DRPDl8.
Lift the accessory out of the sample compartment
and rest it on its back.
Loosen the two setscrews that secure the knob
and slide the knob off its rod (see Figure 18).

Knob

Setscrews (2)

//

Figure 18 The Camlock Plate

24 of 36

CHC

Slide the locking adapter over the rod, as shown

in Figure 19.
Tighten th e two setscrews to secure the locking
adapter.
Mount the CHC mounting plate on the Praying
Mantis body, as described on the next page.
Be sure to carefully slide the mounting plate
between the bottom plate of the Praying Mantis
and the camlock plate.

CHC Mounting
Plate

Locki ng Adapter
Setscrews (2)

Figure 19 Installing the Locking Adapter

25 of 36

CHC

Slide the CHC mounting plate (Figure 20) under

the Praying Mantis TM body locating the CHC
mounting plate pin in the hole In the bottom of the
Praying Mantis TM .
Use the two pan head screws provided to secure
the mounting plate in place.

Thumbscrew
Hole

CHC Locating Pin Hole

Praying Mantis
Figure 20 Installing the CHC Mounting Plate (Top View)

Mount the CHC by guiding the locating pin which

is directly under the CHC body into the locating
hole In the DRP base.
Fasten the thumbscrew (Figure 21) to secure the
CHC to the CHC mounting plate.
Dewar

Heater Thermocouple

CHC Mounting Plate

Gas lnlel/Outlet (2)
Thumbscrew
Figure 21 The CHC installed

26 of 36

CHC

FLUID I ELECTRICAL
CONNECTIONS

If temperature control is desired, connect the

thermocouple and the heater (Figure 21) to a
suitable temperature controller.
If the CHC is to be operated at temperatures
above 1ooc or below oc, use 1/4" tubing to
connect the two cooling ports (see Figure 22) to a
water inleUoutlet or a coolant circu lator.
If vacuum is desired, connect the gas outlet (1/4"
VCO fitting , see Figure 22) to a vacuum pump or
other source of vacuum using 3/8" l.D. vacuum
tubing. Seal off the two gas inleUoutlet ports.
If reaction or process gas/es are to be passed
through the sample, connect the gas inleUout
ports (1/4" VCO fitting, see Figure 22) as needed
to the gas source/s. Connect the gas outlet and
seal off any unused gas ports.
If reaction or process gas/es are to be passed
over the sample, seal off the gas outlet. Connect
one of the gas inleUoutlet ports to the gas source
and the other as the outlet.

Gas lnleVOutlet
Cooling Ports /

Gas lnleVOutlet
Gas Outlet

Figure 22 The CHC Installed

27 of 36

CHC

COLLECTING THE
BACKGROUND SPECTRUM

Place a sample screen into the sample cup and

locate the plastic overflow tray over the sample
cup (Figure 21).
Fill the sample cup with the reference material
using the provided packing tool.
Draw the
straightedge across the top of the cup to level off
the surface.
Carefully remove the overflow tray.
Install the dome.
Swing the Praying Mantis TM cover back into place
and tighten the thumbscrew (Figure 1).
Fiii the Dewar with liquid nitrogen or other
coolant.
Set the temperature and pressure to desired
operating conditions.
Set the spectrometer to measure the "energy" on
the detector.
Adjust the elevation adjustment microm eter on
the CHC (Figure 15) to maximize the signal on
the detector.
Collect the background spectrum .

28 of 36

CHC

Overflow Tray

Sample Cup

Figure 23 Filling the Cup

SAMPLE SPECTRUM

Restore the reference material to ambient

conditions.
Remove the dome.
Empty the sample cup. This can be done by
vacuuming out the reference sample or by
removing the CHC from the Praying Mantis rt.1
and dumping out the material.
If needed clean the sample cup.
Fill the sample cup with the sample (follow
procedure in the alignment section).
Install the dome (see page 23).
Install the CHC into the Praying Mantis if it was
removed to empty the sample cup.
Swing the top plate back into place and tighten
the thumbscrew (Figure 1).
Restore the desired sampling conditions.
Collect the sample spectrum.
Empty the sample cup and clean it before
running the next sample.

29 of 36

f:f,t~~~ltjt(>x

REACTION CHAMBER MAINTENANCE

LEAK CHECKING

The Reaction Chambers have been carefully checked for

leaks before shipment. However, each time the Reaction
Chambers are disassembled and reassembled, leaks
may develop due to improper setting of the o-rings. If
leaks occur, carefully inspect all o-rings and sealing
surfaces for damage and contamination. Small leaks can
be pinpointed using a Helium Leak Detector. Contact
Harrick Scientific Products, Inc. for advice and/or repair
information.

CLEANING THE REACTION

CHAMBERS

To thoroughly clean the reaction chambers follow the

procedure below.
To clean the HVC:
Vacuum out the sample or remove the HVC from
the Praying Mantis, remove the dome, turn the
HVC upside-down and dump out the sample.
Use solvent to clean off the remaining sample.
Unscrew the eight screws that secure the bottom
cover of the HVC.
Remove the bottom cover to reveal three access
holes.
Gingerly wipe or blow clean air through these
holes to clean the interior of the HVC.
When the interior is clean, make sure the a-rings
on the bottom plate are clean and free of dirt.
Re-install the bottom cover.
To clean the CHC:
Vacuum out the sample or remove the CHC from
the Praying Mantis TM, remove the dome, turn the
CHC upside-down and dump ou t the sample.
Use solvent to clean off the remaining sample.
Unscrew the four screws that secure the bottom
cover of the CHC.
Remove the bottom cover to reveal the access
hole.
Gingerly wipe or blow clean air through the hole
to clean the interior of the CHC.
When the interior is clean, make sure the o-ring
on the bottom plate is clean and free of dirt.
Re-install the bottom cover.

30 of 36

REACTION CHAMBER MAINTENANCE

REPLACING THE 0 -RINGS

The a-rings used by the Reaction Chambers should be

replaced periodically. The Reaction Chambers have
o-rings for sealing the windows, o-rings for sealing the
access holes, a-rings on the fittings, and an o-ring to seal
the dome to the Reaction Chamber.

REPLACING THE HEATER

To replace the HVC heater:

Remove the HVC from the Praying Mantis .
Loosen the screw on the side of the HVC that
anchors the heater wire to the HVC.
Remove the two screws at the back of the HVC
that clamp down the heater and thermocouple
wires.
Push a small, blunt object through the heater
access hole (Figure 9) at the front of the HVC.
Slide the heater out the back of the unit.
To install a new heater, coat the heater with MgO
powder (Maalox or the equivalent).
Slide it into the HVC until it hits the stop.
Make sure that the heater is inserted completely
into the body before re-securing the wire.
To replace the CHC heater:
Remove the CHC from the Praying Mantis TM .
Push a small, blunt object through the heater
access hole (Figure 15) at the opposite side of
the heating wires.
Slide the heater out the other side of the unit.
To install a new heater, coat the heater with MgO
powder (Maalox or equivalent antacid).
Slide It Into the CHC until it hits the stop.
Make sure that the heater is inserted completely
into the body before re-securing the wire.

31 of 36

REACTION CHAMBER MAINTENANCE

REPLACING THE
THERMOCOUPLE

To replace the HVC thermocouple:

Remove the HVC from the Praying Mantis TM.
Loosen the screw on the side of the HVC that
anchors the thermocouple wire to the HVC.
Remove the two screws at the back of the HVC
that clamp down the heater and thermocouple
wires.
Gently pull out the thermocouple.
Slide the new thermocouple into the HVC until it
hits the stop.
Make sure that the thermocouple is inserted
completely into the body before re-securing the
wire.
To replace the CHC thermocouple:
Remove the CHC from the Praying Mantis.
Gently pull out the thermocouple.
Slide the new thermocouple into the CHC until it
hits the stop.
Make sure that the thermocouple is inserted
completely into the body before re-securing the
wire.

32 of 36

APPENDIX A

To install the supplied rail plate onto the floor of the

sample compartment of your spectrometer:
Remove any existing sample holders from the
floor of the spectrometer.
Install the rail plate in the orientation indicated in
Figure 24. See Table 1 on the next page for the
appropriate screws/holes for your spectrometer.

MOUNTING THE
HARRICK RAIL PLATE

Mating Plate

Harrick Rail Plate

BACK

@
8
D

@
A

D
8

@
FRONT

Figure 24 Screw and Pin Positions for Rail Plate

33 of 36

APPENDIX A

FTIR SPECTROMETERS

HOLES

VARIAN or D IGILAB (All Models)

MATTSON (Polaris, Galaxy, RS Infinity, Genesis, Satellite)

PERKIN ELMER (Spectrum 1)

THERMO-NICOLET (Nexus, Avatar, Magna, Impact)

Table 1 Screw and Pin Positions for Rall Plate

34 of 36

f~bt~~Flj1tjl(:S{

APPEND/XS

'--~~~~~~~~~~~~~~~~~~~

OPTIONAL AND REPLACEMENT PARTS

OPTIONAL PARTS (Praying Mantis)

Ambient Sample Chamber ...................................................................................
High Temperature Reaction Chamber, 24V (FTIR) ...............................................
Low Temperature Reaction Chamber, 24V (FTIR) ..............................................
High Temperature Reaction Chamber, 24V (UV-Vis) ...................... .. .. .. ...............
Low Temperature Reaction Chamber, 24V (UV-Vis) ............................................
Spectroscopic Grade KBR Powder ......................................................................

DRP-ASC
HVC-DRP-4
CHC-CHA-3
HVC-VUV-4
CHC-VUV-3
KBR-100

OPTIONAL PARTS (Reaction Chambers)

Temperature Controller, 110V ................................................................................ ATC-024-1
Temperature Controller, 220V ................................................................................ ATC-024-2
Vacuum Pump, 110V .... ........ ............................................................... ................... VPE-001
Vacuum Pump, 220V .. .. .. ..................................................................... ..... .. ............ VPE-002
UV Quartz Window for the Vacuum/Low Pressure Domes .......... ..... .. .. .. ............... WAD-U23
Si Window for the Vacuum/Low Pressure Domes ........... .. ..................................... WED-U23
CaF2 Window for the Vacuum/Low Pressure Domes ............................................ WFD-U23
ZnS Window for the Vacuum/Low Pressure Domes .............................................. WID-U23
ZnSe Window for the Vacuum/Low Pressure Domes ............................................ WMD-U23
KBr Window for the Vacuum/Low Pressure Domes ............................................... WPD-U23
0 -Ring (#23) for the Dome, Kalrez ....................................... ................................... ORK-023
0 -Ring (#13) for Windows of the Dome, Kalrez ............ .. ....................................... ORK-01 3
0 -Ring (#10) for the VCO Fittings, Kalrez .............................................................. ORK-010

HVC Reaction Chambers Only

High Pressure Dome, ZnS Windows ...................................................................
High Pressure Dome, ZnSe Windows .................................................................
High Pressure Dome. UV Quartz Windows ........................................................
ZnS Window for the High Pressure Dome .................... .......................................
ZnSe Window for the High Pressure Dome ........................................................
UV Quartz Window for the High Pressure Dome ........ ........................................
0 -Ring (#16) for the Bottom Cover, Kalrez .... ............. ............ .. ........ ..................

HVC-DWl-3
HVC-DWM-3
HVC-DWA-3
WID-U43
WMD-U43
WAD-U43
ORK-016

CHG-CHA Reaction Chambers Only

0 -Ring (#001) for Thermocouple Fitting, Kalrez ................................................. ORK-001
0 -Ring (#26) for the Bottom Cover, Kalrez ....................................... .................. ORK-026
0 -Ring (#19) for the Dewar, Kalrez ..................................................................... ORK-019

35 of 36

APPENDIXB

REPLACEMENT PARTS (Praying Mantis)

Alignment Fixture ..... ...... .. .... .. ....... .. ... .... ..... ......... .... ......... ... ..... ..... . .... .. ... ... .. ... .. .... ..
Sampling Accessory Kit .. ......... ................................................................................
Micro-sampling Cup .. .................... .............. .......... .... ......... .. .......... .. .... ..... ..... ..........
Sampling Cup ............................................. ................................................ .............

DRP-ALN
ORA-SAP
DRP-SAP
DRP-S10

REPLACEMENT PARTS (Reaction Chambers)

Packing Tool ...... ........................................................................... ........ ..................
Screen Set, two each of three mesh size ...............................................................
K-Type Thermocouple .................................................................... ........................
Flex Mounting Plug - Male ............................................. .. .............. ........................
UV Quartz Window for the Vacuum/Low Pressure Domes .......... ..........................
KBr Window for the Vacuum/Low Pressure Domes ... .. .... ............................... .......
0 -Ring (#23) for the Dome, Vlton .................... .......................................................
0 -Ring (#13) for Windows of the Dome, Viton .......................................................
0 -Ring (#10) for the VCO Fittings, Viton ...................... .... ................... ...................

116-836
116-439
008-144
008-266
WAD-U23
WPD-U23
ORV-023
ORV-013
ORV-010

HVC Reaction Chambers Only

UV Quartz Window for the High Pressure Dome ................................................
1.00"x0.25" Cartridge Heater, 100W, 24V ................. .......................... ................
24V Heater Assembly ......... ............ ......... ...................... ......................................
0 -Ring (#16) for the Bottom Cover, Viton ...........................................................
Overflow tray ............... .. .. .. ................................................................. .. ..... ..........

WAD-U43
HTRS-26
HVC-HT4
ORV-016
116-835

CHG-CHA Reaction Chambers Only

24V Heater Assembly .................... ......................................................................
1.00"x0.25" Cartridge Heater. 75W, 24V ........................................... ..................
0 -Ring (#001) for Thermocouple Fitting, Viton ............................... ....................
0 -Ring (#26) for the Bottom Cover, Viton .... ..... ..................................................
0-Ring (#19) for the Dewar, Viton ........ ............. ..................................................
Overflow tray ........................................ ...............................................................

HVC-HTR
HTRS-16
ORV-001
ORV-026
ORV-019
116-854

36 of 36

f:f,t~~~tjl(>~'

Manual Part No. DRP-M-04

"-~~~~~~~~~~~~~~~~~-

2009 Harrick Scientific Products, Inc.

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