www.chromatographyonline.

com OCTOBER 2010 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 1

Considerations on Switching from

Helium to Hydrogen

The operational considerations for switching from helium to hydrogen

are explained and options discussed. Analysts need to make decisions
about their approach to switching the carrier gas to hydrogen. Are they
looking for analysis time reductions or would they like to quickly switch
their analysis without having to optimize or change their run conditions?
The source of the hydrogen and purity levels needed for its use as a
carrier gas are discussed along with the advantages or disadvantages of
using hydrogen generators versus gas cylinders.

G as chromatography (GC) uses

a wide range of gases including
helium, hydrogen, and nitrogen
as the carrier gas. In the U.S., the most
common carrier gas is helium, as it pro-
Kansas. Sites outside the U.S. with high
concentrations of helium are in Algeria
and Qatar.
Helium has many uses and applica-
tions. These include (by order of size)
vides good separations, is inert, is readily cryogenic cooling (28%), tank purging
available, and it is safe to use. In many (26%), welding cover gas (20%), as a
other countries, helium is less available controlled atmosphere (13%), leak detec-
or is very expensive, and hydrogen is tion (4%), and for breathing mixtures
commonly employed. In recent years, (2%) (2). The use of the gas as a carrier
the availability of helium has decreased gas for GC falls under a miscellaneous
and its cost has increased significantly, category and is a relatively small fraction
so many chromatographers have consid- of the available supply. Many larger users
ered switching to the use of hydrogen of helium are seeing considerable growth
(1). In this article, we compare the use of in their use of the gas and will need even
helium and hydrogen in GC and discuss larger quantities in the future.
the advantages of hydrogen. In addition, Helium is a critical and national
we will discuss how a chromatographer resource for the U.S. During World War
can obtain hydrogen in a convenient, II, huge caverns were sealed and used
safe, and economical manner to meet to store the helium, creating the USA
Reginald J. Bartram* and the needs of the laboratory. Helium National Reserves. In 1995, the
Peter Froehlich† government decided to allow the sale of
The Availability of Helium 600 million ft3 of helium between Janu-
*GC Consultant, State College, Helium is a minor component of natu- ary 1, 2005 and January 1, 2015 (The
Pennsylvania
ral gas formed by the natural breakdown Helium Privatization Act of 1996- Pub-
of uranium. Fractional distillation of lic Law 104-273) (3). Sales are ongoing
†Peak Media, Franklin, Massachusetts natural gas allows for the purification and continue in the U.S. and to foreign
of helium from the natural gas. The countries, leading to reduced supplies
Direct correspondence to: largest helium concentrations found in and much higher prices for helium. In
[email protected]
natural gas are in Texas, Oklahoma, and addition, breakdowns in manufacturing
2 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 OCTOBER 2010 www.chromatographyonline.com

facilities have also reduced available sup-

plies (4). The end result of the increase
in demand and the decrease in supply
has required the withdrawal of the gas
from the national reserves and there are
significant concerns about the ability to
obtain helium on a reliable basis. Many
users worry more about the ability to
obtain helium when they need it than
the increased price.

Why Use Hydrogen for Gas

Chromatography
Hydrogen and helium are both very effi-
cient gases to use for GC and chroma-
tographers can switch from one to the
other with little to no difficulty. While
Figure 1: Plot of HETP versus linear velocity (5). the nature of the separation is the same
with the two gases, the differences in
the properties of the two gases will lead
to differences in the efficiency of the
separation. A plot of the efficiency of
a column is a van Deemter (4) (packed
column) or Golay (5) (capillary column)
plot that depicts the efficiency of a col-
umn versus different operating veloci-
ties of various carrier gases. The van
Deemter equation (equation 1) is used
to calculate the height equivalent to a
theoretical plate (HETP). It describes
the column efficiency or a measure of
its ability to separate peaks. The desired
HETP value would be the smallest value
obtainable.

Figure 2: Typical plot for various carrier gases with capillary columns (6). HETP = A + B/μ + Cμ [1]

where
μ = linear velocity of carrier gas
(mobile phase)
A = A constant that accounts for the
effects of “eddy” diffusion in the col-
umn. (The A term is not used with cap-
illary columns because there is only one
flow path and no packing material in a
capillary column)
B = A constant that accounts for the
effect of molecular diffusion of the vapor
in the direction of the column axis
C = A constant proportional to the
resistance of the column to mass transfer
of solute through it.
Figure 1 shows a plot of HETP versus
linear velocity and depicts the areas of
the plot that represent the A, B, and C
terms
μ = L/tM [2]
Figure 3: Separation of bacterial acid methyl esters (7).
www.chromatographyonline.com OCTOBER 2010 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 3

terial acid methyl esters on an Equity-1

column with a linear velocity of 25 cm/s
for both helium and hydrogen. Notice
that at the same LGRs that even with
this complex sample the retention times
for these components are about the same.
Comparing Chromatograms at
Optimum LGR: The chromatograms
shown in Figure 3 shows the bacte-
rial acid methyl esters for helium and
hydrogen with the helium being at the
optimum LGR for helium and the run
for hydrogen also being at 25 cm/s but
not at its optimum (hydrogen is the top
chromatogram and helium is the bot-
tom chromatogram.) The run shown for
hydrogen shows a total run time of 19.5
Figure 4: Separation of bacterial acid methyl esters using hydrogen (50 cm/s) (8). min. What would this run look like at
the optimum of 50 cm/s with hydrogen?
where ditions that provide the smallest value for The chromatogram in Figure 4 is
L = Length of the column in centi- HETP, as this would provide the accu- the same column run at 50 cm/s using
meters mulation of the most plates or separation hydrogen at the same program rate as
t M = Retention time in seconds of a power within a column). When looking used in Figure 3. The total run time is at
nonretained compound (typically meth- at the typical plot of HETP versus the 16 min. Though there is an improvement
ane). linear gas rate (LGR), there is not much in the reduction of the run time, you do
The B term in the van Deemter difference between the minimum value not see a great reduction. This is because
expression defines the slope of the curve for the HETP for helium and hydrogen, this separation is very temperature sen-
after the minimum (or bottom) or low- but there is a large difference for the sitive and needs a higher temperature
est HETP value. It is this slope and the average linear velocity or linear gas rate program rate to speed it up. To obtain
minimum that displays the difference values obtained for the HETP minimum a faster separation you would increase
between the use of hydrogen and helium. for each gas. When using helium with your temperature program rate by close
From an operational perspective, the typical capillary columns, the usable to twice that used for the run in Figure 3.
HETP values are determined experimen- range of LGR is 20–30 cm/s, while for (See later in this article for temperature
tally at various carrier gas velocities. A hydrogen, we see a much wider range of program concerns.)
plot of HETP versus the linear velocity LGR of 25–65 cm/s. The slope of the Major Benefits of Hydrogen: The
is generated using equation 3 and equa- HETP versus LGR curve for hydrogen use of hydrogen provides the chromatog-
tion 4. (C term) is smaller than that for helium rapher with a number of benefits:
HETP = L/Neff [3] and shows only a 25% reduction in the • Increased speed: Increasing the lin-
optimum HETP value over the 25–65 ear flow rate allows for shorter run times,
where cm/s range. thereby increasing the throughput of a
L = Length of the column in centi- laboratory.
meters Switching from Helium to Hydro- • Achieve lower temperature separa-
Neff = Theoretical plate number gen: tions: At the faster elution times, it might
When you switch from helium to hydro- not be necessary to increase the column
and gen, there are two options: temperature run rate. You might be able
• Choose to duplicate your analysis to lower the maximum temperature
Neff = 16 (tR /w)2 [4] using hydrogen with little to no loss of needed for the analysis or remain at those
efficiency. temperatures for shorter periods.
where • Choose to take advantage of the • Longer column life: Lower tempera-
tR = Retention time of the peak being higher LGR available with hydrogen tures lead to less column bleed and can
measured to speed up your analysis as the higher provide to longer column life. In addi-
w = Width of the peak. linear velocity used for hydrogen leads tion, hydrogen is a reducing gas and can
Measure the peak width for packed to shorter retention times and a shorter remove out potential acidic sites inside of
columns at the base line and for capillary analysis. the column. The removal of these sites
columns at the half height of the peak. Comparing the Use of Hydrogen leads to less sample absorption and less
and Helium at the Same LGR: The generation of phase breakdown (column
Determination of HETP chromatograms in Figure 3 compare the bleed). The result is a longer usable life
The chromatographer would desire con- separation of a complex sample of bac- for the column.
4 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 OCTOBER 2010 www.chromatographyonline.com

raphers can switch to hydrogen readily if

flame ionization detection (FID) or other
flame-based detection methods such as
phosphorus, nitrogen, electron-capture,
or Hall detection are employed for the
separation. If the separation requires a
helium detector, it will be necessary to
maintain the use of helium. The use of
mass spectrometry (MS) might allow or
not allow the use of hydrogen and it is
best to check with the manufacturer of
your unit about its capability. Thermal
conductivity detection (TCD) typically
uses helium for the best thermal differ-
ences between the carrier gas and other
compounds to be detected. Some anal-
yses do use hydrogen as a carrier such
as with oxygen, helium, and other very
light gases. Therefore, the use of hydro-
gen for TCD is application dependent.
Delivering Hydrogen to the Chro-
matograph: When switching the carrier
Figure 5: Plot of gas viscosity versus pressure (9). gas from helium to hydrogen, it might
be necessary to change the external tub-
ing connections to the GC system. If the
GC system employs a flame-ionization
detector, a hydrogen line is already in
place. First, vent the line and then cut it
and install a tee. Connect the other side
of the tee to the supply carrier gas.
If you are using copper tubing for
delivery of the carrier gas (as is common
in many facilities), replace it with stain-
less steel tubing as copper tubing will
oxidize and harden with time. Hardened
copper tubing is quite brittle and may
break if it is bumped while stainless steel
tubing is much more robust. To avoid
contamination to the GC system be sure
to use clean, preferably GC-quality tub-
ing.
The purity of the fuel gas also should
be a consideration. If fuel-grade hydro-
gen is used, it will be necessary to
include a purifier in the system to reduce
moisture and oxygen levels so that the
Figure 6: Flow schematic of a hydrogen generator with a palladium membrane. gas is 99.9999% pure. The other choice
is to switch to carrier-gas grade as the
• Environmental concerns: Hydrogen • Cost savings: The cost of hydrogen is carrier gas. Several inline purifiers are
is available readily via the electrolysis significantly lower than that of helium. available that will reduce the impurities
of water and is not a critical national (Comparisons of cost are best made in- to the desired levels and include indica-
resource. In contrast, helium is a by- house due to differing cost structures tors to notify the user when the purifier
product of natural gas or petroleum pro- from site to site.) is expended and needs to be changed.
duction and there are environmental • Availability: Because the generation If the GC system automatically adjusts
concerns with the production and purifi- of hydrogen is from water, the chroma- for LGR: Many modern GC systems
cation of the gas. Hydrogen is a green gas tographer need not be concerned about include electronic pneumatics and it
in that its production does not contribute availability issues. simply necessary to indicate the gas used
to environmental pollution. Switching to Hydrogen: Chromatog- so that automatic adjustments based on
www.chromatographyonline.com OCTOBER 2010 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 5

the gas to make sure you know the split

Table I: Typical detector fuel gas flow rates*
ratio you were using. After changing the
Detector Flow rate
gas, it will be necessary to measure and
Flame ionization 30–40 cm3/min
adjust your split vent flow to allow for
60–75 cm3/min (sulfur mode); 100–175cc/
Flame photometric
min (phosphorus mode)
the same split ratio you previously used.
Note: The split flow does not always
2–3 cm3/min (nitrogen compounds only)
Nitrogen–phosphorus 300 cm3/min for both nitrogen and phos- need to be on. With splitless injection
phorus compounds techniques, the flow is off for a short
period after injection. Use this same
*Consult your GC manufacturer for your specific unit flow requirements.
technique with a split injection tech-
nique. After about 2 min, the entire
the density differences of the gases are the column to an acceptable level. When sample that is going into the column is
considered. Indicate that hydrogen is the switching the carrier gas to hydrogen, it in the column, and the split flow can be
carrier gas in the control program of the may be necessary to adjust the split ratio turned off at this time. Turn it back on as
GC system and the unit will make the (which is the ratio of sample and carrier you prepare for the next injection. This
necessary density adjustments in con- gas that enters the column versus how can provide huge savings in gas usage.
trolling the carrier gas. Typically, the much is vented) and increase the LGR Note: If you are doing splitless injec-
system will control the LGR in the col- to obtain the best possible analysis and tions you will still need to know the
umn, the split ratio, and the amount of the shortest possible run time. amount of gas exiting the vent port
flow of fuel gas to the FID system. Split ratios: To calculate the split ratio when the port is open (typically 20–60 s
If you are using a short column and a you most know the flow of the column after an injection). Make adjustments to
flow controller: Some units use flow con- and the split vent flow. With this tech- duplicate the split flow after the switch
trollers in combination with pressure nique, it is desired to reduce the amount to hydrogen.
controllers to control the LGR. If you of sample down to a level where the on- Splitless injection techniques: Hydro-
are using a short column or wide bore column concentration of the individual gen is preferred over helium for splitless
column, the LGR for hydrogen might components due not saturate and cause injection techniques as it carries the sol-
lead to a column head pressure that is wide and often tailing peaks. ute from the inlet into the column faster
below 10 psig. In this case, it might be than helium. This results in sharper
necessary to change the flow controller split ratio = split vent flow/column peaks (higher efficiencies) and reduces
to allow flow control below 10 psig. flow [5] band broadening with the resulting
If the operation of the GC system is wide and shorter peaks, which allows for
pressure: The operation of simple GC To calculate the column f low use lower detection limits.
systems and some older GC systems equation 5. Direct injection: There is no concern
is related to the pressure of the carrier on the conversion when using direct
gas (that is, do not automatically adjust Flow = πr 2L/tM [6] injection.
for LGR); in this case, it will be neces-
sary to make adjustments to the head where Temperature Programming
pressure. To achieve the same LGR for π = 3.1416 Concerns
hydrogen as you used for helium, it will r = Radius of the column (in centi- Many analyses use temperature program-
be necessary to set the head pressure to meters converted) ming to allow the later eluted compounds
approximately 45% of the pressure used L = Length of the column (in centi- to be eluted at a reasonable temperature
for helium. meters) to obtain sharp symmetric peaks. The
Changes needed for various injection tM = Retention time of a non retained changeover from helium to hydrogen
techniques: Adjusting the split ratio: If peak typically methane has significant implications with tem-
you desire to shorten your analysis time Where L/tM = LGR = μ [7] perature programming runs. There is a
by increasing your LGR, then you will significant difference in the viscosity of
need to reestablish your vent flow to Simplified: helium and hydrogen and this difference
maintain your desired split ratio. This Flow = πr 2 μ (Remember to use cen- is temperature dependent as indicated in
adjustment to the split ratio is necessary timeters as units) [8] Figure 5. Both gases increase in viscosity
to allow for only the correct amount of as temperature increases, but hydrogen
sample to enter the column; the rest of With a column that has an internal has a much lower viscosity than helium
the sample goes to a vent. The ratio of diameter of 0.25 mm, the split ratio is throughout the temperatures shown. The
sample entering the column versus that typically 100/1 (that is, only 1 part in lower viscosity of hydrogen means that
going to the vent is the split ratio. The 100 of the sample enters the column and lower pressures are required for hydro-
typical injection size of 1 μL of sam- the rest of the sample and carrier gas gen. Because the viscosity of hydrogen is
ple saturates most columns and leads flow is vented). approximately 45% lower than helium,
to broad peaks. splitting the sample Always measure the column f low the pressure needed to run the analysis is
reduces the amount of sample entering and vented carrier gas before changing about 45% lower when hydrogen is used.
6 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 OCTOBER 2010 www.chromatographyonline.com

order of elution of compounds. If you

choose to use the same LGR and temper-
ature as used with helium, typically, you
should not see any problems. However,
with polar columns, such as Carbowax
or the highly polar Cyano phase columns
it may be necessary to check the elution
order as some column phases, at differing
temperature, exhibit different polarities
or orders of peak elution.
Detector Optimization Concerns:
Flame detectors need an optimum flow
of hydrogen to optimize the flame sensi-
tivity and other detectors can have simi-
lar requirements on how much hydrogen
can be used. With the flame ionization
detector, the flow optimum is 30–40
cm3/min of hydrogen. When you switch
to hydrogen as a carrier gas, you will have
to take the flow from the column into
consideration so that you do not exceed
Figure 7: Hydrogen generator with a proton exchange membrane. the optimum flow range of hydrogen for
the detector. With packed columns or
large-bore capillary columns, this might
mean reducing the fuel gas flow so that
the combination of carrier and fuel gas
is at that rate previously used for the
separation. For typical detector fuel flow
ranges see Table I.
Make-Up Gas for Detectors: If you
do use hydrogen as the make-up gas, it
will be necessary to consider this flow
with the carrier gas and fuel gas to opti-
mize the detector sensitivity. Take care
not to saturate the detector with too
much hydrogen, as this will affect both
base line noise and sensitivity.
Hydrogen is not the best choice for
make-up gas; the best gas for a make-up
gas with flame detectors is 99.9999%
pure nitrogen. Its use leads to lower base-
line noise and better flame performance.
Figure 8: Hydrogen collected via a GC system equipped with a discharge ionization
detector. Safety Concerns When Using
Hydrogen
When running capillary columns with a the LGR and using a 5 °C/min tempera- General Considerations: Hydrogen gas
system using LGR, you can use the same ture program rate, it might be desirable is used commonly in the laboratory for
LGR but the resulting head pressure for to increase the program to 10 °C/min. a variety of purposes and is the carrier
the hydrogen is 45% lower. If the peaks are coming out rapidly and gas of choice for gas chromatography in
If you choose to use higher flow rates are sharp, you can take advantage of the countries other than the U.S. It is the
for hydrogen, it might be necessary to lower column temperatures and stop the fuel used in the most commonly used
make corrections to the temperature temperature programming just before or detectors (flame ionization, nitrogen,
program when desiring a rapid analysis after the last peak is eluted. This might and phosphorus detectors) and therefore,
time. Some compounds might be eluted mean a lower final run temperature and already in the laboratory and in use with
faster but provide broader peaks than will often extend column life. most gas chromatographs.
desired if the temperature program rates Elution Order of Peaks: With most If the analyst changes from helium to
are not increased to match the higher analyses, the change of linear gas rate hydrogen, the safety issues should be well
flows. If, for example, when doubling and temperature might not change the understood to ensure safe operation. The
www.chromatographyonline.com OCTOBER 2010 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 7

flammability of the gas ranges from 4 hydrogen. hydrogen gas collects can be a metal elec-
to 74% in air, with an explosion limit of Safety Concerns: Gas Generators trode or a polymeric membrane, while
18.3–59%, so there are real hazards if a Versus Cylinders: The concern with the anode, where oxygen is collected, is
build-up of hydrogen were to occur. Sim- flammable gases is with the build up of a metal electrode.
ilarly, if a large buildup of hydrogen or these gases to flammable or explosive Electrolysis of water using two metal
helium were to occur in the laboratory, limits. Consider as one of the primary electrodes: The electrolysis of water can
the oxygen concentration for breathing concerns the total volume of hydro- be performed readily using a metallic
might be compromised. As we describe gen in your lines. If a break in the line cathode and metallic anode immersed in
in the following, the use of a hydrogen occurs, an explosive level of the gas in a strong, water-soluble electrolyte such as
generator obviates many of the safety the lab could be present. Gas generators 20% sodium hydroxide. The base is an
concerns, as only a small quantity of gas with their safety shutoffs and monitor- electrolyte, as pure water does not con-
is present at a given time, in contrast a ing safety features only allow for small duct a current very effectively, and the
significant amount of hydrogen is pres- volumes of gas in their lines and units. quantity of hydrogen generated is very
ent when a tank is used. If there is a sudden release of pressure low. To provide hydrogen of high purity,
Although hydrogen can form an or flows, the gas generators will turn off the cathode consists of a bundle of pal-
explosive mixture with air, it diffuses (some modern GC systems also incorpo- ladium tubes. The cathodes are palla-
rapidly. It dilutes quickly by combining rate this feature). dium tubes because only hydrogen (and
with air into a nonflammable concen- Cylinders often involve long lines lead- its isotopes) is capable of passing through
tration. Hydrogen rises two times faster ing to GC systems and the hook-ups are it and ultra-high-purity hydrogen gas is
than helium at a speed of almost 45 mph often at the end of benches or in other obtained.
(20 m/s). In a laboratory with good air rooms. With a long run of tubing, you As an alternative to the use of a palla-
turnover, it would be very difficult to will have large volumes of gas in the dium cathode, some systems that gener-
achieve flammable limits. In addition, lines, under pressure, and the possibility ate hydrogen via the electrolysis of water
most modern GC systems incorporate a of venting of these lines with a line break. via a metal electrode use a stainless-steel
turn-off system when flows or pressures This could allow for the entire venting cathode and employ a desiccant as the
suddenly increase or decrease (as in the of the volume of one or more cylinders final drying agent. While the initial cost
case of a column breakage in the GC into the lab. With the proper installa- of such approach is lower, the hydrogen
oven) and help to reduce the possibility tion of cylinders, it is unlikely that you gas collected in this manner is less pure
of a problem. will see cylinders taking off like rock- as it contains significantly more oxygen
In the case of a column or line break ets and shooting across laboratories. Be and nitrogen than hydrogen gas gener-
when using a gas generator, the available sure to review your operating procedures ated via a palladium electrode (see Fig-
volume of gas is low, and also the genera- and safety concerns before switching ure 6). In addition, systems that employ
tion of gas will be terminated. Genera- to hydrogen. There are codes and stan- a desiccant, require regeneration on a
tors only store about 60 cm3 of gas. dards for safe building and installation periodic basis.
Proper Venting: It is best to con- practices. Any new hydrogen component Presented in Figure 6 is a typical
sider special venting systems to remove installations should follow strict guide- hydrogen generator (Parker Balston
the chance of any build up of hydro- lines and undergo third-party testing for Model H2PD-30, Parker Hannifin Cor-
gen. When using hydrogen as a carrier safety and structural integrity. To make poration, Haverhill, Massachusetts). It
gas you need to consider all of the flows sure you have the latest guidelines you generates hydrogen via the electrolysis of
exiting the unit. In many detectors, the can check your standards against the fol- water using a metal electrode. This sys-
carrier gas burns in the flame and is not lowing sources on the Internet. tem generates hydrogen with a purity of
a problem, but you should consider the Internet sources of safety information 99.99999+%, oxygen content of <0.01
venting of the gas from detectors that do include www.hydrogenSafety.info; www. ppm, and moisture content of 0.01 ppm
not burn the hydrogen. fuelcellstandards.com; and www.eere. at a maximum flow rate of 300 mL/min
A source of venting is the septum vent energy.gov/hydrogenandfuelcells/codes. with a maximum outlet pressure of 60
port. The typical septum purge is 1–5 Ways of Supplying Hydrogen Gas psig.
cm3/min. It is easy to vent this flow with via an In-house System: To obtain Electrolysis of water using a proton
the split vent exhaust. The split exhaust hydrogen gas for GC, use high-pressure exchange membrane: In recent years, ionic
port will have the highest vented flow. cylinders or an in-house generator. The polymeric materials such as Nafion (a
split vent ports can have flows of 50–500 in-house generation of hydrogen is based sulfonated tetrafluoroethylene polymer)
cm3/min. This can mean a lot of vented upon the electrolysis of water, as shown or polybenzimidzole (PBI) have been
hydrogen and will need special venting. in equation 9. found to conduct protons while being
Many laboratories already have special impermeable to gases such as hydrogen
fume hood vents over the split vent to 2H2O + 2e- → 2H2 + O2 [9] and oxygen. Proton exchange mem-
allow for the venting of hazardous sam- branes (PEMs) made from such poly-
ple components. If you do not have such Connecting a power source to two mers are used in fuel cells to generate
vents in place, you should consider them electrodes placed in water performs the electricity from oxygen and hydrogen. If
for both the sample and the venting of electrolysis of water. The cathode, where a potential is applied to a system contain-
8 LCGC NORTH AMERICA VOLUME 28 NUMBER 10 OCTOBER 2010 www.chromatographyonline.com

ing a PEM in the presence of water and a with cylinders in the laboratory and to
counterelectrode, the water will be disso- obtain the best, most convenient source
ciated to form hydrogen ions, which are of hydrogen, consider the use of a hydro-
then converted into hydrogen gas. The gen gas generators.
primary benefit of using a PEM is that
deionized water can be used instead of References
the 20% sodium hydroxide used when (1) N. Pacheco, U.S. Bureau of Mines, U.S
two metallic electrodes are used and Geological Survey Minerals Yearbook, 1 –2,
sodium hydroxide, which is caustic, is not (2007).
required. When a PEM is used to gener- (2) The Helium Privatization Act of 1996, Pub-
ate hydrogen, a palladium membrane can lic Law 104-273.
be used to purify the hydrogen further (3) M Rose, Photonics 1–12, 2008.
by reducing the oxygen concentration to (4) J.J. van Deemter, F.J. Zuiderweg, and A.
less than 0.01 ppm and moisture down Klinkenberg, Chem. Eng. Sci. 5, 271 (1956).
to <1.0ppm. (5) E. Glueckauf, M.J.E. Goley, and J. H. Pur-
Shown in Figure 7 is the general design nell, Ann NY Acad. Sci. 72, 612 (1956).
of a hydrogen generator based upon PEM (6) L. Sidisky, “Carrier Gas Selection: Helium
membrane technology (Parker Model vs. Hydrogen,” Pittcon 2008, Orlando,
H2PEM-510). This system is capable Florida.
of generating 99.9995% pure hydrogen
(noncarrier grade) at a flow rate of 510 Reginald Bartram is presently a
mL/min at pressures up to 100 psi. consultant for gas chromatography
and is semiretired. He is a past
Figure 8 shows the chromatograms of president of the Chromatography
hydrogen gas collected via a gas chro- Forum of Delaware Valley and the
matograph equipped with a discharge recipient of the 1999 Chromatography
ionization detector. The red trace is from Forum of Delaware Valley Award for
gas generated via a palladium cathode Contribution to Theory, Instrumenation,
and Application of Chromatography.
,while the black trace is from gas col- He has been widely published on
lected using a stainless-steel electrode the subject of gas handling and gas
and a desiccant drying tube. purification. In his 35 years of service
The large black peaks indicate the to GC, he has worked at Supelco and
presence of a combined concentration of Alltech as a scientist and marketing
manager.
12 ppm of O2 and N2 in the hydrogen,
which is not present in the hydrogen that Peter Froehlich is President of Peak
was dried with the Pd tubes. It is clear Media, Franklin, Massachusetts. He
that the palladium tube cathode pro- received the Ph.D. in chemistry from
vides a very considerable improvement Purdue University, West Lafayette,
in purity. indiana, and has over 30 years of
marketing and technical support
experience in the scientific instrument
Conclusion industry, with an emphasis on a broad
The process of switching from helium to range of chromatographic techniques
hydrogen involves many issues but with including GC and LC. ◾
attention to detail, one can switch suc-
cessfully and duplicate previous analysis
with little to no problems. If desired, the
analysis can be run at higher LGRs and
greatly reduce the analysis time. The
switch from helium to hydrogen will
allow reduced cost of analysis due to
Visit ChromAcademy on LCGC’s Homepage
the lower cost of hydrogen and allow for www.chromacademy.com
longer column lifetimes. For most chro-
matographers, hydrogen is a gas already
in the lab and is not an increased safety
issue. Consider venting hydrogen, along For more information on this topic,
please visit
with any sample vapor, to provide the saf-
www.chromatographyonline.com/majors
est, cleanest environment for the analyst
to work within. To avoid the problems