The Lab Manager

FREEZE DRYERS
RESOURCE
GUIDE

How to Pick the Best Freeze Dryer / Lyophilizer

for Your Lab Application
BY RYAN ACKERMAN

Freeze Dryers: It's All About Temperature, Pressure,

and Time

2017
BY TREVOR HENDERSON

Top 4 Signs That You Should Service or

Replace Your Freeze Dryer
BY LAB MANAGER

Freeze Dryers: From Storage to Sample Preparation

BY MIKE MAY

Freeze Dryers Product Finder

BY LAB MANAGER
Freeze Dryers Resource Guide 2017

How to Pick the Best Freeze Dryer /

Lyophilizer for Your Lab Application
Two main configurations exist for lab freeze dryers
By Ryan Ackerman

MAINTENANCE TIP:
FREEZE DRYERS /
LYOPHILIZERS
To get the longest life out of your freeze dryer, experts
recommend keeping up with basic oil changes on the
vacuum pumps, neutralizing the stainless steel from acids,
and cleaning the collectors as you would on a refrigerator.
Most freeze dryers will last a long time with the proper care,
however, if a major component such as a condenser breaks, it
may be time to replace the unit.

Will the size or volume of samples to be

lyophilized affect which style of freeze dryer
should be used? How does the volume of liquid to be removed
affect the type of freeze dryer needed?
Yes. Two main configurations exist. Benchtop, which come in a
variety of configurations and styles, are ideal for small volumes Different sample types hold differing amounts of water. A
of samples which need to be accessed easily. Floor standing tissue sample may hold a small amount of liquid, whereas a
models, on the other hand, are beneficial for large scale freeze food product may hold a much higher level of liquid. Using a
drying capabilities, such as large amounts of samples or bigger lyophilizer that does not have sufficient capacity (for example
samples. freeze drying 6L of liquid in a 5L freeze dryer) can have
detrimental effects on the system. This can result in damage
How does sample type affect which type of to the system (increased collector temperature) and poor
freeze dryer is ideal? vacuum. Knowing the typical amount of liquid to be removed
beforehand is therefore critical in purchasing the right system.
In order to properly freeze dry samples, a differential of 15-
20C between the eutectic temperature (freezing point) of the
sample and the lyophilizer is needed. Most biological samples
are sufficiently frozen by a standard system reaching -50C.
For samples such as HPLC preparations in acetonitrile, which
has a eutectic point of approximately -42C, a much lower
temperature will need to be achieved. A cascade-type collector
which can reach down to -84C will be able to accommodate
this. It should be noted that with many lab professionals
switching to methanol for these processes due to its availability
and affordability, an ultra-low temperature lyophilizer, able to
hit as low as -105C may be required due to methanol having a
eutectic point of -97.6C.

Lab Manager 2017 2 LabManager.com

Freeze Dryers Resource Guide 2017
Freeze Dryers: It's All About
Temperature, Pressure, and Time
Freeze-drying, or lyophilization, is a long established process in the food, biotechnology, pharmaceutical,
and diagnostic industries that involves the removal of water or another solvent from a frozen product
by means of sublimation. This process is commonly used for improving product stability, for long-term
preservation, for product purification, and for sample preparation.
By Trevor Henderson
While the immediate benefit of freeze drying is obviousthe
ability to store samples at ambient temperaturesfreeze-
drying also may afford long-term savings by eliminating the
need for costly cold storage.
The process of freeze-drying relies on the balance of only
three controllable variables: temperature, pressure, and time.
Although the process may seem straightforward, freeze-drying
can often be problematic. Having an intimate understanding
of the physical and chemical properties of the samples
you are working with is essential to selecting a process and
equipment best suited to your needs.
Knowing your sample
Controlling the freeze-drying process is dependent on two
factors: the presence of a deep vacuum and a temperature
differential of 15 to 20 degrees between the samples eutectic
temperature (freezing point) and the temperature of the
collector. Choosing a freeze dryer that meets the demands
of your application can be a daunting task and requires
careful consideration of the samples to be prepared. Choose a
system that is too small and you will overload your collector;
if your system doesnt reach the correct temperature or has
insufficient vacuum, you will risk sample melt back.
For many biological samples, including urea, blood plasma,
Lab Manager 2017
serum, and vaccinia, a standard freeze-drying system with
a refrigeration system that reaches -50C will be sufficient.
In the case of HPLC samples where the freezing point of
acetonitrile is much lower (approximately -42C), however,
you will require a cascade-type collector. Cascade systems
have dual condensers that can reach -84C and would be a
suitable choice for these samples.
Switching to methanol
Many labs are looking at methanol as an alternative to
acetonitrile, due to its general availability and affordability.
However, methanol has a much lower freezing point of
-97.6C, making lyophilization difficult even when it is
diluted. In response to this demand, some manufacturers are
offering ultra-low temperature freeze-dry systems. Labconcos
FreeZone systems, for example, are able to achieve collector
temperatures as low as -105C, making lyophilization of dilute
methanol, ethanol, and acetonitrile possible.
A matter of timing
The most common question concerning freeze-drying is
likely, How long will it take? The answer, however, is not so
direct. The time required to freeze-dry a sample is dependent
on a number of factors, including sample volume, thickness,
and surface area; the eutectic point and solute concentration
of the sample; and the temperature of the collector and the
maximum vacuum obtained. In general, samples with a large
surface area will freeze-dry faster than those that are thick or
dense. Additionally, thick samples require moisture to pass
through the layer of dried material, increasing the chance
that the sample will thaw and collapse. Depending on your
sample, freeze-drying can be a lengthy process lasting from
hours to weeks. While freeze-drying provides superior drying
capacity, if time is of the essence, you may consider a vacuum
concentrator or evaporator for your application.
Finally, if you are shopping for a freeze-drying system,
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Freeze Dryers Resource Guide 2017

remember to budget for a rotary vane vacuum pump with

vacuum deep enough to pull down to 2 x 103 mBar, as well as
any glassware or adapters that may be required.

Top 4 Signs That You Should Service or

Replace Your Freeze Dryer
By Lab Manager

1. Your application has changed.

The freeze dryer was intended for aqueous samples,
now solvents or acids are used. A temperature differential is
3. Sharing a community freeze dryer.
Personal freeze dryers used by a single researcher are
more popular than ever. No more guessing if an oil change was
required for proper freeze drying; an upgrade to a cascade done, or if a harmful sample is being processed..
model is recommended.

2. The freeze dryer was inherited from

another lab.
4. The unit no longer pulls a good vacuum.
Gaskets, hoses and all rubber components break down
over time causing poor vacuum and refrigeration leaks.
A used freeze dryer can cause problems. Rubber parts dry out
and crack, decontamination may not have been done properly.
A used pump can have corrosion that cant be seen until its
too late.

Lab Manager 2017 4 LabManager.com

The wrong
way to check
samples.

The right way to

check samples.
Dont get stuck waiting for your samples to freeze dry.
With a FreeZone Freeze Dryer, you are free to roam.
The FreeZone emails you alert messages and status
updates whenever and wherever you choose. Add the
End-Zone accessory and know precisely when freeze NEW Labconco
drying is complete.
FreeZone
Freeze drying is now as effortless as childs play: Freeze Dryers
Large, full color display with touch screen with End-ZoneTM

navigation gives you parameter status at-a-glance.

Lyo-Works OS software provides numerous
programming options and stores data for proof of
sample integrity.
USB port and Ethernet connection make it easy to
output data.
Find out more at 800.821.5525 or www.labconco.com
We double dog dare you!
Kansas City, MO | 800.821.5525
www.labconco.com Made in U.S.A.
Freeze Dryers Resource Guide 2017
Freeze Dryers: From Storage to Sample
Preparation
By Mike May
Freeze drying faces new challenges in storage and sample
preparation. In the past, researchers typically freezedried
aqueous mixtures, but todays samples might include solvents
or alcohols.
As an example of sample preparation, Jenny Sprung, product
manager at Labconco (Kansas City, MO), says, For analysis
using HPLC [high-performance liquid chromatography],
samples are freeze-dried to a powder and reconstituted with
another solvent that is compatible with the analyzer. The
freeze-drying might, for example, remove acetonitrile, and
then the sample could be reconstituted with, say, methanol for
analysis.
To improve efficiency, many users want to know when the
endpoint, or dryness, is reached. Determining 100 percent
dryness can be difficult, says Sprung, but using tools on the
freeze dryer allows you to monitor the conditions during a run.
This includes product temperature probes, vacuum-pressure
monitoring, or weighing the sample periodically during the
process. After freeze-drying, researchers can store the sample.
Refrigerating hundreds of vials can be expensive, and room-
temperature storage is more efficient. To simplify that process,
Labconco developed a mini-stoppering chamber. It allows
you to stopper samples under vacuum for longterm storage
without being exposed to moisture in the atmosphere, Sprung
explains. This lets you easily stopper a few samples instead of
Lab Manager 2017
using a large tray dryer, which can be very expensive.
Systems for sharing
At Marquette Universitys environmental laboratories
(Milwaukee, WI), manager Michael Dollhopf and his
colleagues freeze-dry small batches of microbial cultures,
often from waste-treating and methane-producing biomass.
The main feature for our lab, Dollhopf says, is ease of use:
push a few buttons and load the sample and go. He adds, We
have multiple users, and it has to be a solid-state and easy-
toreproduce, consistent function.
Many users share a freeze dryer at Stanford Universitys
department of environmental earth system sciences, and they
work with a wide variety of materials, from insects and plant
tissues to soils and saliva, says lab manager Douglas Turner. In
thinking about shopping for a freeze dryer, Turner says, For
us, its important that multiple users can have access to it at the
same time, so we prefer the style with removable flasks versus
the cabinet type.
When sharing is not enough, freeze-drying can be outsourced
to American Lyophilizer (Yardley, PA). This company works
with customers to create a custom freeze-drying program.
If a product does not require current good manufacturing
processes (cGMP), American Lyophilizer even provides low-
cost experimental runs that can be turned around in 24 to 48
hours. For lab directors interested in getting into freeze drying
with less of an investment, American Lyophilizer also offers
used instruments.
Pushing ahead
Users have their own replacement guidelines. For instance,
Dollhopf says, For our use, the only time to replace would
be if some major non-swappable componentprobably the
condenserdid not function.
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Freeze Dryers Resource Guide 2017

Turner notes, Our freeze dryer is about 12 years old. Usually stainless steel from acids, and cleaning the collectors as you
its the pump that needs attention. The seals of the unit can all would on a refrigerator. In the end, a freeze dryers longevity
be replaced, so I dont think we would replace the unit until it depends on maintenance and care.
no longer chills.

To get the longest life, Sprung recommends keeping up with

basic oil changes on the vacuum pumps, neutralizing the

Freeze Dryers
Product Finder
Freeze dryers find use in a variety of research and manufacturing
environments and are commonly used for material storage, food and
pharmaceutical processing, as well as for less common applications
such as taxidermy and document recovery. With a wide variety of
options available, there is much to consider when purchasing a new
freeze dryer.

Product Finder: Freeze Dryers

Featured Manufacturers
Labconco has been manufacturing laboratory equipment since 1925. Their
laboratory equipment is marketed to industrial, environmental, life science,
pharmaceutical, clinical and crime laboratories. Products include fume hoods,
biological safety cabinets, glove boxes, glassware washers, freeze dry systems,
carbon-filtered enclosures, balance enclosures, bulk powder enclosures,
lab animal research enclosures, evaporation systems and centrifugal
concentrators. Several of Labconcos product lines contribute toward LEED
credits. Labconco is ISO 9001 certified and is a member of the USGBC.

www.labconco.com

American Lyophilizer  www.freezedrying.com

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