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Q: How does one purify solvents to HPLC grade ? ( Answered 3 out of 5 stars,   3 Comments )
Subject: How does one purify solvents to HPLC grade ?
Category: Science
Asked by: tiger17-ga
List Price: $25.00
Posted: 29 Oct 2002 00:37 PST
Expires: 28 Nov 2002 00:37 PST
Question ID: 91806
We need to save money in our lab . How can we buy high-grade  solvents
and turn them into HPLC and Pesticide etc purity ? Is it just water
removal ? Can we filter the water out ? Can it be done econimically ?
Say 50-100 gallons a week ?
Subject: Re: How does one purify solvents to HPLC grade ?
Answered By: till-ga on 29 Oct 2002 01:44 PST
Rated:3 out of 5 stars
As HPLC grade solvents can be very expensive and as you need larger
amounts of them it can for sure be econocmic to purify the solvents
There are several products available that can help you to reach the
necessary purity of the solvents. These methods seem to be well
developped and economically interesting.
You will certainly have to contact the companies offering these
products to get the necessary details and prices.

Here is what I´ve found out for you:


"Solvent Filteration and Degassing Products

Pure and Simple Solutions to Liquid Chromatography Problems.
HPLC, as an analytical tool for detection and separation of chemical
has become the most important laboratory technique over the last
decade. As
with all analytical techniques, minor processing problems sometimes
which in the long run can have major impact on the accuracy of the
system as
well as its durability.
Although the evolution of liquid chromatographs has brought the
via the microprocessor into the computer age there are still problems
the computer cannot solve.
This is why we at LAZAR have spent the majority of our R & D time in
those seemingly simple but persistent problems so that we can proudly
you that we have the pure and simple chromatography solutions.

The LAZAR Filter-Degasser can be used to accommodate almost all HPLC
applications. For most ISOCRATIC applications, the Filter-Degasser can
directly screwed onto the popular 1 liter HPLC solvent/reservoir
bottle (38mm
cap). In this fashion, it is not necessary to further transfer the
degassed solvent where reabsorption of gasses as well as particle
can further occur. 28mm and 33mm caps for 250 and 500 ml bottles are
The Filter-Degasser with 38mm cap also fits on the standard one gallon
(4 liter)
solvent bottle for filtration and degassing of solvent without
requiring an
operator's attention. A gallon of solvent can usually be filtered in
less than
10 minutes. Further, the Filter-Degasser is also available with 24/40
and 19/22
standard taper for use with various Erlenmeyer and volumetric flasks.
addition it can be used with a 40/35 standard taper for use with the
MilliporeŽ type filtration flasks.
For most GRADIENT separations, binary or ternary, LAZAR offers a
manifold system where simultaneous vacuum filtration and degassing of
2 or 3
solvents can be run from one vacuum source.
The manifold system features individual shutoff valves for each vacuum
operation, quick disconnect couplings for the individual filtration
a master control valve for adjusting vacuum flow, and a disposable
line filter as a safety feature against pump contaminants.  The
can be attached to any vacuum source."
from: HPLC Solvent Purification
( )

"Solvent Purification Process
Solvent Purification is designed to remove moisture and oxygen from
reagent grade solvents.
By applying a head pressure of a inert gas of your choice the solvent
is driven through a dual designed pressure vessel system. The pressure
vessels are packed with either activated alumina to remove moisture,
or copper catalyst to remove oxygen. Alternatively the solvent must be
run through a bubble degassing process when not suited for copper
catalyst oxygen removal. (please see chart # 1.1)
Dispensing the solvent can be completed either by using inert gas head
pressure, or more preferably by using a stainless steel schlenk vacuum
Maintenance of the system is limited. The SPS-400 columns are designed
to purify 400 liters of solvent. Regeneration can be completed by
Innovative Technology supplied heating blanket and temperature
controllers, or we provide fresh columns for a nominal fee. It is also
recommended that all filters are replaced every year to assure good
flow of solvent through columns.
Solvent Purification Systems are the safe alternative
It is widely accepted that Solvent Purification Systems are the safe
alternative to the distillation of solvents typically performed in
labs. This is largely due to the fact that Innovative Technologies
SPS-400 requires absolutely no heating elements to remove impurities.
It is also important to know that the entire system is pressure rated
well beyond standard operating pressures. This can only be done by
using the highest quality fittings, valves, and components available.
Innovative Technology has also placed a great of emphasis on the
structural design of the SPS-400. Our Modular extruded aluminum style
frame allows us to offer the stability, and chemical resistant
surface, while allowing us the flexibility to meet your particular
space requirements. The System has also been designed with the
operator in mind. All directional, evacuation, and refill valves are
clearly labeled, allowing for easy operation of all solvent dispensing
All systems are designed with an emergency stop device allowing for
immediate stoppage of solvent flow to and from pressure vessels.
Where can I get a SP system?
As a supplier of Solvent Purification Systems, we have knowledgeable
technicians, and an engineering department to help design you the
perfect system. Our SPS-400 was designed to purify HPLC grade
solvents, removing Moisture, Oxygen to the low PPM levels required by
Solvent & Innovative Technology, Inc. 
2 New Pasture Road Newburyport, MA. 01950 
(978)462-4415 (voice) -- (978)462-3338 (fax) -- 
( )

There is a closer description with some details and photos of the
SPS-400 system here:
( )

The SPS-400 seems to be a good choice as it´s purification capacity
should be high enought for your needs.

Another example of a solvent purification system in a lab:
"solvent purification system

We have set up a solid state solvent purification system in our
laboratory. This system (J.C.Meyer) has proven to be much safer over
conventional distillation apparatuses. It will complement our efforts
to handle highly reactive species under very careful conditions. The
solvent dispensing system provides common solvents such as
acetonitrile, THF, ether, toluene, pentane, and methylenechloride air-
and water free. The solvents are stored in fire-proof cabinets in
stainless-steel reservoirs, pressurized with ultra-pure argon, and
passed through two sequential columns to remove any water and trace
impurities as well as oxygen. The system is equipped with a
cross-diffusion prevention between the solvents and a vacuum transfer
device for refilling the solvent kegs without pouring. The solvent
lines are plumbed directly into the glove-box, which allows to collect
solvents at a "filling station" inside the boxes as well as at the
solid state solvent purification
( )


Although I could not find details on ther page, you still might have a
look at this system:
"MBRAUN provides a safer option to distilling solvents either into a
glove box or into collection flasks outside of the glove box. The
MBRAUN SPS system removes O2 and H2O from a wide range of organic and
deuterated solvents quickly and safely. The completely mobile system
can purify up to 400 liters of solvent before a regeneration of the
filter material is necessary."
from: MBRAUN Science & Research
( )

"B/R Instrument offers a variety of equipment for purifying or
upgrading solvents and chemicals. High purity solvents can be very
expensive. It is often economical to purchase industrial grade
solvents and upgrade them to laboratory grade or higher. This not only
reduces costs but also ensures that there is always an adequate supply
of solvent with the required purity.
Our customers are currently purifying solvents for use in the
laboratory and in the electronics industry.
Distillation systems can be fully automatic, semi-automatic, or
manually operated depending on your needs. Flask sizes range from 1 to
50 liters.
Click the product navigation bar below to view specific information
about our different types of distillation equipment. If you need
additional information, please contact us."
from: B/R Instrument Solvent Purification
( )

Remark: when I tried to access their webpages they were extremely
slow. Maybe there was a techniccal problem then.

I hope these hints help you to reduce costs in your lab.


Search strategy:
( ://
( ://
tiger17-ga rated this answer:3 out of 5 stars
pretty good answer . Would have liked advice from some 'hands-on'
experience at this as all companies will only tell one how easy it is
. would use again .

Subject: Re: How does one purify solvents to HPLC grade ?
From: rupert_sg-ga on 29 Oct 2002 20:25 PST
Hmm.. . I'm not sure about the usefulness of that answer - the only
simple answer to that question is solvent distillation. Add a drying
agent to the AR solvent (the drying agent will depend on the solvent -
and then distill. The main problem is that this can be hazardous esp.
with volumes > 1 litre. Many accidents in labs are caused primarily by
solvent distillation. My honest recommendation: spend the extra cash -
it is simply not worth the hassle and risk.
Subject: Re: How does one purify solvents to HPLC grade ?
From: silverius-ga on 31 Oct 2002 18:57 PST
Altough the answer offered a quantity of information, I do not think
it provided information pertinent to your question.  Spinning band
distillation and drying agents are what you need.  Keep in mind
solvent distillation can be very dangerous!!!!
Subject: Re: How does one purify solvents to HPLC grade ?
From: kimgart-ga on 02 Nov 2002 08:01 PST
The main reason for using "HPLC grade" solvents is that they have been
treated to remove UV absorbing impurities that interfere with peak
detection by UV. For example, "regular" reagent-grade hexane contains
traces of benzene that absorb enough at 254nm to cause problems with
some HPLC detectors. Normal distillation often will not remove these
impurities (after all, they have already been distilled ). Most non
HPLC grade solvents are plenty dry enough and work just fine straight
from the bottle without further purification, although I usually run
them through a millipore filter to make sure there is no sediment that
would gunk up the  HPLC plumbing. PS: I have been doing HPLC since
1971, so my comments are from hands-on experience, not a web search.

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