SP VirTis BenchTop 2K User manual

SP INDUSTRIES, INC.
Freeze Dryer Operator's Manual
VirTis BenchTop 2K, 4K and 6K
Freeze Dryers

Committed to Product Excellence
…and Continuous Support
Copyright © 2009 SP Industries, Inc. All marks herein are used under license.
All brand or product names mentioned may be trademarks or registered trademarks of their respective companies.
Part Number 414258
Revision 004, 12/09
SP Industries Inc. Corporate Headquarters
935 Mearns Road 815 State Route 208 3538 Main Street
Warminster, PA 18974 USA Gardiner, NY 12525 USA Stone Ridge, NY 12484 USA
[phone] [phone] [phone]
[phone] [phone] [phone]
[phone]
SP Service [phone]
SP Service Fax [phone]
Website www.spindustries.com
This Freeze Dryer Operator's Manual contains confidential and proprietary information of SP Industries, Inc. and may be
used only by a recipient designated by and for purposes specified by SP Industries, Inc.
Reproduction of, dissemination of, modifications to, or the creation of derivative works from this Freeze Dryer Operator's
Manual, by any means and in any form or manner, is expressly prohibited, except with the prior written permission of SP
Industries, Inc. Permitted copies of this document must retain all proprietary notices contained in the original.
The information in this document is subject to change without prior notice. Always confirm with SP Industries, Inc. that you are
using the most current version of this document. SP Industries, Inc. is free to modify any of its products and services, in any
manner and at any time, notwithstanding the information contained in this document.
THE CONTENTS OF THIS DOCUMENT SHALL NOT CONSTITUTE ANY WARRANTY OF ANY KIND, EITHER
EXPRESSED OR IMPLIED, INCLUDING BUT NOT LIMITED TO THE IMPLIED WARRANTIES OF MERCHANTABILITY
AND/OR FITNESS FOR A PARTICULAR PURPOSE OR GIVE RISE TO ANY LIABILITY OF SP INDUSTRIES, INC., ITS
AFFILIATES OR ITS SUPPLIERS.
The terms and conditions governing the use of this Freeze Dryer Operator's Manual shall consist of those set forth in written
agreements with SP Industries, Inc.
Revision 004, 12/09 i
© SP Industries, Inc. 2009

Important Symbols
Warning! Injury or even death
may result if a recommendation
marked with this symbol is not
heeded.
Crush Hazard. Keep hands clear when
operating door.
Electric Shock Danger! Use
appropriate caution to avoid injury or
death.
Corrosive Chemical. Wear suitable
gloves, safety glasses, and protective
clothing.
Burn Danger! Potentially hot surface.
Use appropriate caution.
Property Caution! To prevent damage to
chamber equipment and/or load, adhere
to procedures marked by this symbol.
Do not store flammable materials in
chamber.
Practical Operating Tip. These
recommendations streamline unit
operation and prevent common operator
errors.
Wear Safety Glasses.
Explosive Materials Hazard! Keep
objects away from heat.
Freeze Dryer Safety Warnings
9Always assume that shelf, condenser and internal parts may be very cold or very hot. Wear protective equipment to
avoid burns.
9Always ensure that only an authorized technician services the refrigeration, heat transfer, vacuum and electrical
systems.
9Always ensure that refrigeration air intake is clear and clean.
9Always ensure vacuum pump exhaust is properly ventilated and/or contained.
9Always practice team lifting when moving heavy equipment.
9Always use a maximum one pound regulator if backfilling from an inert gas source.
9Always wear safety glasses when using glass flasks.
9Do carefully read the entire instruction manual before attempting to operate the freeze dryer.
9Do verify that the electric service and other utilities match the unit’s requirements before connecting to power.
9Never allow hand or body contact with open vacuum ports.
9Never clean with solvents. Use mild detergent and water only.
9Never operate the unit without all covers in place.
9Never pressurize chambers. Laboratory freeze-drying systems are designed for vacuum only.
9Never stopper vials unless the chamber door is tightly closed.
9Never use acrylic closures if they are cracked or crazed.
9Never use with toxic, corrosive, flammable or organic materials unless special precautions are in place to prevent injury
to personnel or damage to equipment.
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© SP Industries, Inc. 2009

Revision 004, 12/09 iii
© SP Industries, Inc. 2009
Warranty Information
VirTis BenchTop 2K, 4K and 6K are warranted by SP Industries to be free of defects in material and workmanship when
operated under normal conditions as specified in the instructions provided in this manual. Please take this opportunity to locate
the serial tag on your new VirTis BenchTop 2K, 4K and 6K and record the information below for future reference. SP Industries
also recommends that you complete and return your unit’s warranty registration card.
Model Number
Serial Number
Part Number
Limited Warranty
SP Industries (the “Company”) warrants each of its products against any defects in material or workmanship, provided that the
product is used in a reasonable manner under appropriate conditions and consistent with the applicable operating instructions,
for a period of 12 months from the date of installation or 15 months from the date of shipment (whichever comes first).
The obligation of the Company shall be, at its option, to repair or replace, without charge any parts that prove to be defective
within the warranty period, if the purchaser notifies the Company promptly in writing of such defect. The Company shall not be
responsible for labor charges payable with respect to persons other than Company employees. Replacement or repair of parts
pursuant to this warranty shall not in any way extend the original warranty period. The Company will not be responsible for any
unauthorized repairs, replacements or product modifications, nor will it be responsible for any product failures resulting from
such unauthorized repairs, replacements or product modifications negligently or otherwise made by persons other than
Company employees or authorized representatives of the Company.
THE COMPANY DOES NOT MAKE AND EXPRESSLY DISCLAIMS ANY WARRANTY OF MERCHANTABILITY OR FITNESS
FOR A PARTICULAR PURPOSE OR ANY OTHER WARRANTY, EXPRESSED OR IMPLIED, WITH RESPECT TO THE
SALE, INSTALLATION, DESIGN OR USE OF ITS PRODUCTS. ADDITIONALLY, THE COMPANY SHALL NOT BE LIABLE
FOR ANY CONSEQUENTIAL DAMAGES RESULTING FROM THE USE OF OR ANY DEFECTS IN ITS PRODUCTS.
The Company’s employees are available to provide general advice to customers concerning the use of the Company’s
products; however, oral representations are not warranties with respect to particular products or their uses and may not be
relied upon if they are inconsistent with the relevant product specifications for the items set forth herein.
Notwithstanding the above, the terms and conditions set forth in the Company’s formal sales contracts shall be controlling and
supersede any inconsistent terms contained herein, and any changes to such contracts must be made in writing and signed by
an authorized executive of the Company.

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© SP Industries, Inc. 2009

Revision 004, 12/09 v
© SP Industries, Inc. 2009
Contents
Important Symbols ............................................................................................................................................... ii
Freeze Dryer Safety Warnings............................................................................................................................. ii
Warranty Information .......................................................................................................................................... iii
Introduction............................................................................................................................................ 1
Key Features........................................................................................................................................................1
BenchTop Usage .................................................................................................................................................1
Available Configurations ......................................................................................................................................2
From Freeze Dryer to Condenser Module............................................................................................................2
Cold Trap Condenser Module ..............................................................................................................................2
Installation and Setup ........................................................................................................................... 3
Initial Inspection ...................................................................................................................................................3
Service Connections ............................................................................................................................................3
Vacuum Pump Installation ...................................................................................................................................4
Installing the Vacuum Pump............................................................................................................................4
Oil Mist Eliminators..........................................................................................................................................5
Freeze Dryer Setup..............................................................................................................................................6
Vacuum Baffle Plate ............................................................................................................................................7
Freeze-Drying Concepts ....................................................................................................................... 9
Elements of Freeze-Drying ..................................................................................................................................9
Freeze .............................................................................................................................................................9
Vacuum ...........................................................................................................................................................9
Heat...............................................................................................................................................................10
Condenser.....................................................................................................................................................10
Product Dependencies.......................................................................................................................................10
Sentry 2.0 Controls.............................................................................................................................. 11
LED Wave Display (Qualitative Reference) .......................................................................................................11
Button Functions ................................................................................................................................................12
Up/Down (+/-) Buttons...................................................................................................................................12
MENU Button ................................................................................................................................................12
COND Button ................................................................................................................................................12
VAC Button....................................................................................................................................................12
AUTO Button .................................................................................................................................................12
DEFR Button .................................................................................................................................................12
LCD Display Functions ......................................................................................................................................13
Main Menu .........................................................................................................................................................13
Vacuum Control.............................................................................................................................................14
Purge (Optional) ............................................................................................................................................14
Heat (Optional) ..............................................................................................................................................14
User Options Menu ............................................................................................................................................14
Vacuum Control.............................................................................................................................................14
Temperature Units.........................................................................................................................................15
Vacuum Units ................................................................................................................................................15

Contents VirTis BenchTop 2K, 4K and 6K
Relay Test .....................................................................................................................................................15
Vacuum Pump Maintenance .........................................................................................................................15
Alarms Menu......................................................................................................................................................16
Setpoints Menu ..................................................................................................................................................16
Condenser Temperature ...............................................................................................................................16
Vacuum OK ...................................................................................................................................................16
Power Save Deadband .................................................................................................................................16
Maintenance Menu and Factory Options ...........................................................................................................17
Factory Options .............................................................................................................................................17
Interstage Control..........................................................................................................................................18
Calibration .....................................................................................................................................................18
Basic Operation ................................................................................................................................... 21
Getting Started...................................................................................................................................................21
Product Preparation: Flask / Manifold Drying.....................................................................................................21
Product Preparation: Drum Manifold Shelf Drying .............................................................................................21
Product Preparation: Chamber Drying ...............................................................................................................22
Quickseal Valves ...............................................................................................................................................22
Operation Instructions........................................................................................................................................23
Meltback.............................................................................................................................................................24
Preventing Glassware Breakage........................................................................................................................25
Product Dryness End Point ................................................................................................................................25
Stoppering (Optional).........................................................................................................................................25
Cold Trap Condenser .......................................................................................................................... 27
Product Requirements .......................................................................................................................................27
Cold Trap Setup.................................................................................................................................................28
Optional Components ......................................................................................................................... 29
Manifolds............................................................................................................................................................29
Shelf Racks........................................................................................................................................................30
Liquid Nitrogen Trap ..........................................................................................................................................31
Filter Trap...........................................................................................................................................................32
BenchTop Cold Plate .........................................................................................................................................33
Initial Setup of the BenchTop Cold Plate .......................................................................................................33
Cold Plate Operation .....................................................................................................................................33
General Maintenance .......................................................................................................................... 35
Vacuum System.................................................................................................................................................35
Vacuum Pump...............................................................................................................................................35
Changing Vacuum Pump Oil .........................................................................................................................35
Vacuum Tubing and Gaskets ........................................................................................................................36
Door Gasket ..................................................................................................................................................36
Vacuum Pump Gas Ballast Valve..................................................................................................................36
Quickseal Valves...........................................................................................................................................37
Refrigeration System .........................................................................................................................................37
The Air-Cooled Condenser............................................................................................................................37
Condenser Chamber .....................................................................................................................................38
Acrylic Parts .......................................................................................................................................................38
Appendix A: Troubleshooting............................................................................................................ 39
Vacuum Problems..............................................................................................................................................39
Product Melting ..................................................................................................................................................40
Appendix B: Serum Vial Capacities................................................................................................... 41
Appendix C: Stainless Steel Cleaners............................................................................................... 43
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VirTis BenchTop 2K, 4K and 6K Contents
Revision 004, 12/09 vii
© SP Industries, Inc. 2009
Appendix D: Spare Parts List............................................................................................................. 45

Chapter
1
Revision 004, 12/09 1
© SP Industries, Inc. 2009
Introduction
VirTis BenchTop 2K, 4K and 6K freeze dryers offer a low-cost solution for laboratories
with space constraints. Featuring condenser temperatures of -55 °C to -105 °C,
BenchTop freeze dryers can handle a wide range of processing requirements.
Key Features
•Extremely compact design.
•Direct chamber, flask and/or shelf drying capabilities.
•Versatile Sentry 2.0 control panel.
•Three- to nine-liter condenser capacity.
•Variety of refrigeration system options.
•Digital display of temperatures and setpoints.
•Quickseal valves for processing flasks.1
•Manual shelf stoppering (optional).
BenchTop Usage
BenchTop units are mechanically refrigerated condenser modules that can be utilized
as freeze dryers or cold traps. These versatile units can also be used for initial product
freezing.
When used in freeze-drying mode, the BenchTop unit can effectively remove up to
99% of product moisture. The cold trap condenser module is capable of trapping
vapors off of a vacuum concentrator or gel dryer.
1Requires optional manifold.

Introduction VirTis BenchTop 2K, 4K and 6K
2 Revision 004, 12/09
Available Configurations
Freeze-drying in
the condenser
Shelf unit in
drum manifold
Vertical manifold
Flask drying on
drum manifold
Flask drying on drum
manifold with stoppered
Fitted for cold
trap application
shelves
From Freeze Dryer to Condenser Module
When using your BenchTop as a condenser module, the vacuum cover plate is
replaced with either a ¾-inch stainless steel port for the manifold plate or a plain cover
plate, which must be purchased separately if no manifold is ordered. The manifold
adapter plate is required when any manifold is purchased.
Cold Trap Condenser Module
When using a vacuum concentrator or gel dryer with your BenchTop unit, the
condenser module can be used as a cold trap, which traps vapors driven off of the
product before they reach the vacuum pump. For more information, refer to Chapter 6:
Cold Trap Condenser.
Note: A low temperature condenser is required when trying to trap organic solvents.
© SP Industries, Inc. 2009

Chapter
2
Revision 004, 12/09 3
Installation and Setup
Initial Inspection
Upon receiving your BenchTop series freeze dryer, inspect all contents of your
shipment for damage. Check packing material for small accessory items. Remove all
packing material carefully and inspect the unit for shipping damage. In the event that
shipping damage has occurred, retain all packing material and contact your freight
carrier immediately.
Note: In the event of shipping damage, SP Industries will cooperate in the matter of collecting
your claim, but is not responsible for the collection or free replacement of material. When
possible, replacement parts will be shipped and invoiced to you, making them a part of your
claim.
Service Connections
Make sure that the outlet you intend to use meets the voltage and amperage
requirements listed on the serial tag of your unit.
CAUTION! ONLY A QUALIFIED ELECTRICIAN SHOULD CONNECT THE UNIT TO THE
AVAILABLE ELECTRICAL SUPPLY.
The line cord has three individual conductors inside the outer jacket.2To make the
appropriate plug connection:
1. Trim back enough of the jacket to facilitate installation of the plug.
2. The three individual conductors are BROWN, BLUE, and GREEN with a
YELLOW tracer.
3. Connect the BROWN wire to the line (hot) terminal on the plug.
4. Connect the BLUE wire to the neutral terminal.
5. Connect the GREEN/YELLOW wire to the ground terminal.
2Consult SP Industries and a qualified electrician if electrical configurations vary from standard, specified service requirements.
© SP Industries, Inc. 2009

Installation and Setup VirTis BenchTop 2K, 4K and 6K
4 Revision 004, 12/09
Vacuum Pump Installation
A remotely mounted vacuum pump is required for operation of your BenchTop freeze
dryer. The vacuum pump must be a two-stage, high-vacuum pump that does not
exceed the maximum allowable amperage listed on the unit’s serial tag and back
panel label.
The following parts are included with your BenchTop unit for connection to the
vacuum pump:
•Four (4) feet of ¾-inch ID (Inside Diameter) rubber vacuum tubing
•One (1) 90° rubber elbow
•One (1) plastic connector
Installing the Vacuum Pump
Notes: If you are installing a previously used vacuum pump, refer to the
vacuum pump manual and the General Maintenance section of this manual.
Ensure that the pump was properly maintained prior to installation.
A vacuum pump inlet port adapter and sufficient tubing are required for
connection to the vacuum pump. If you need assistance, please contact SP
Industries.
1. Position the vacuum pump in a convenient location near the
freeze dryer. Ensure that the pump will be easily accessible
during routine maintenance.
2. Cut the supplied vacuum tubing as short as possible. Allow
enough length between the vacuum pump and the
BenchTop unit.
Note: Clamp and cut the ¾-inch ID vacuum hose. If you do not
wish to cut the hose, it may be used at its full length, but may take
up more space than necessary.
3. Locate the inlet port on your vacuum pump. Refer to the
vacuum pump manual.
4. Remove any material with the exception of the inlet filter
screen and gasket.
5. Place the adapter on the inlet port and secure with a fitting.
If an adapter is not present, contact SP Industries.
6. Remove all objects from the vacuum pump outlet port, but
retain for future use.
7. Connect the BenchTop unit to the vacuum pump using the
¾-inch vacuum tubing. If connecting to a vacuum pump
purchased from SP Industries, attach the ¾-inch tubing from
the BenchTop to the vacuum pump intake nipple, add a tubing clamp and
tighten securely.
Vacuum pump
8. Check the vacuum pump oil level. The oil level should read half way up the
sight glass. Add oil only if necessary. DO NOT OVERFILL!
9. Verify that the power switch on the vacuum is off. The LED next to the VAC
button on the unit’s front panel must be off.
© SP Industries, Inc. 2009

VirTis BenchTop 2K, 4K and 6K Installation and Setup
Revision 004, 12/09 5
© SP Industries, Inc. 2009
10. Plug the vacuum pump into the receptacle marked VACUUM PUMP on the
back of the unit. The receptacle is an IEC universal outlet. This allows you to
control the pump using the Sentry 2.0. The voltage, phase and frequency of
the vacuum pump must match the voltage, phase and frequency specified on
the rear panel of the freeze dryer.
Note: You can power your vacuum pump from a wall socket if it does not have an IEC
connector, but you will not be able to control the pump from the Sentry 2.0 Controller.
Only a qualified electrician should perform installation of an IEC connector. The pump
used should not exceed the amperage listed on the BenchTop serial tag.
11. Enable power to the vacuum pump by switching the pump’s circuit breaker to
the on position.
Oil Mist Eliminators
To reduce fumes from the vacuum pump and/or vent the vacuum exhaust externally,
SP Industries recommends the installation an Oil Mist Eliminator (OME).
Related Parts
•Oil Mist Eliminator, Plastic for Oerlikon Leybold TRIVAC E D2.5E Vacuum
Pump (P/N 414203).

Installation and Setup VirTis BenchTop 2K, 4K and 6K
6 Revision 004, 12/09
Freeze Dryer Setup
To set up your BenchTop unit:
Note: Refer to Basic Operation for complete equipment operation instructions.
1. Install a condenser gasket (black rubber ring with a slit in it) on the top of the
unit. It should have a light film of vacuum grease on the outer surface.
2. Prepare the unit for your intended use.
a. If the unit is to be used as a standalone freezer, cover the condenser
with a plain cover plate to prevent air circulation from warming the
samples. Skip to step 5.
b. If the unit is to be used as a manifold dryer, place a manifold adapter
plate (clear acrylic or stainless steel circular disk with a hole) over the
gasket.
c. If you are using an acrylic drum manifold, place a second condenser
gasket around the bottom lip of the manifold.
BenchTop with acrylic manifold.
d. If you are using a stainless steel manifold, place the supplied O-ring in
the groove of the manifold adapter plate.
3. If using a manifold, attach Quickseal valves to each port on the manifold and
ensure that each is in the closed position. For more information, refer to the
Quickseal valve section in Chapter 5.
Note: Quickseal valves are siliconized at the factory. Vacuum grease is not required.
4. If using an acrylic drum manifold, apply a thin coating of vacuum grease to the
tapered surface and place the tapered plug in the top center of the manifold.
Slowly turn the plug 360° clockwise and then 360° counterclockwise. This will
ensure a good seal between the surface of the plug and the manifold.
5. Plug the unit into an appropriate outlet and switch on the circuit breaker
located on the rear of the unit. The control panel display will illuminate.
© SP Industries, Inc. 2009

VirTis BenchTop 2K, 4K and 6K Installation and Setup
Revision 004, 12/09 7
Vacuum Baffle Plate
The BenchTop 2K and 4K models include a two-position vacuum baffle plate.
•Baffle Plate on Chamber Bottom (Position 1).
By raising the baffle plate handle, the plate can
be dropped to the bottom of the chamber. This
allows you to pre-freeze items on the baffle plate.
In some cases, it may be more convenient to
remove the baffle plate completely and freeze
items directly on the bottom of the chamber.
Note: Freeze-drying cannot be performed with the baffle on the chamber bottom
(position 1) since the vacuum port will be blocked and the product will remain too
cold for water vapor transfer.
•Baffle Plate in Raised Position (Position 2).
Lower the baffle plate handle to raise the baffle
plate when freeze-drying products directly on the
baffle. This allows ice to build up on the
condenser below and provides more room for the
materials to be dried.
© SP Industries, Inc. 2009

Installation and Setup VirTis BenchTop 2K, 4K and 6K
8 Revision 004, 12/09
© SP Industries, Inc. 2009

Chapter
3
Revision 004, 12/09 9
© SP Industries, Inc. 2009
Freeze-Drying Concepts
The first step of lyophilization (freeze-drying) is typically to freeze the product to a
minimum of -40 °C. After the product is frozen, moisture can be extracted through
sublimation. The sublimation process takes a solid (i.e., ice) and converts it to a gas
(i.e., vapor), bypassing the liquid stage. The moisture is converted to a gas, while
maintaining the material’s crystalline structure.
The second step involves the migration of moisture from the product. BenchTop
series freeze dryers facilitate the migration of moisture by using a vacuum to extract
non-condensable vapors in the product chamber or container. The freeze dryer
creates a low-pressure zone to allow moisture to flow easily from the product. Since
vapor naturally travels toward cooler surfaces, the condenser chamber is cooled to at
least 15 °C below that of the product to attract product moisture.
Many products require a secondary drying process to remove moisture that did not
convert to vapor during the first process. During secondary drying, BenchTop units
remove the remaining bound moisture by slightly warming the product.
Note: To prevent meltback, the product should not be warmed above its eutectic point until all
free ice has sublimated.
Elements of Freeze-Drying
Freeze
The product must be completely frozen before freeze-drying can begin. Product
freezing can be accomplished directly in the condenser chamber, or through pre-
freezing methods such as dry-ice baths or a laboratory freezer. The product’s frozen
temperature should be at least -40 °C. To minimize freeze-drying time and protect the
product against meltback, the product should be frozen in the thinnest cross section
possible.
Vacuum
Adding vacuum assists in removing air and other non-condensable vapors from the
chamber to facilitate vapor migration. The vacuum system creates a nearly pressure-
free environment to allow the vapor from the frozen product to flow toward the cold
condenser surface easily.

Freeze-Drying Concepts VirTis BenchTop 2K, 4K and 6K
10 Revision 004, 12/09
© SP Industries, Inc. 2009
Heat
Carefully controlled heat input to the frozen product speeds the drying process. The
BenchTop unit is designed to be used as either a manifold freeze dryer or a tray dryer.
Exposing glassware containing frozen product to ambient room temperature helps
drive the drying process by adding heat. This causes the frozen solvents in the
product to sublimate and then migrate to the colder surface of the condenser wall.
Several heated and unheated racks and stoppering accessories are available for
freeze-drying in drum manifolds.
In its simplest configuration, a BenchTop unit will freeze-dry products on the partially
raised vacuum baffle in the center of the condenser. Heat will be added by radiation
through the acrylic cover.
Condenser
Trapping water vapor molecules in the form of ice on the condenser surface
effectively removes moisture from the product. The refrigeration system cools the
internal condenser at the bottom of the chamber to attract and trap vapors migrating
off the product.
The condenser is located under the manifold to provide the shortest vapor path to
achieve the maximum drying rate. The condenser capacity ranges from 3 to 9 liters,
which indicates the maximum volume that can be condensed from the product before
defrosting is necessary.
Product Dependencies
The freeze-drying process is completely dependent upon (and will change with) each
specific product. In all cases, the condenser temperature must be cold enough to trap
the vapors migrating from the product effectively. If the condenser is not cold enough,
excess vapors may be pulled into the vacuum pump inadvertently. To compensate for
this issue, SP Industries offers optional filter and liquid nitrogen (N2(liq)) traps.