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Installation and Operations Manual Power+Energy Hydrogen Purifier 6000 / 7000 Series POWER+ENERGY Palladium Diffusion Hydrogen Purifiers PEDOCM-0005 v2.00 Rev REL-02.A

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Page 1: Installation and Operations Manual Power+Energy Hydrogen

Installation and Operations Manual

Power+Energy Hydrogen Purifier 6000 / 7000 Series

POWER+ENERGY Palladium Diffusion Hydrogen Purifiers

PEDOCM-0005 v2.00 Rev REL-02.A

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Important Notice

In order to maximize purifier lifetime, it is recommended that the purge gas

pressure be set to at least 70% of the inlet hydrogen pressure.

For example, if the inlet hydrogen pressure is 180 psig, the nitrogen purge pressure should

be 126 psig.

For some installations, it may be easier to slightly reduce the hydrogen inlet pressure to

meet this criterion. Power+Energy, Inc 106 Railroad Drive Ivyland, PA 18974-1449 Phone: (215) 942-4600 Fax: (215) 942-9300 e-mail: [email protected] Website: www.purehydrogen.com

“Quality, Service & Innovation” 2004 Power+Energy, Inc

PEDOCM-0005 v2.00 Rev REL-02.A

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Table of Contents Back-diffusion........................................................ 16

Chapter 1 ....................................................................2 Table of Contents ......................................................... ii

Contaminants.......................................................... 16 Oxygen / water .................................................... 16

Theory of Operation..................................................2 Introduction ...................................................................2

Low flow ................................................................ 17 Figure 1. P+E 6000 and 7000 Series Hydrogen Purifiers ..........................................2

UPH Output Flow Decrease ................................... 17 Contamination ........................................................ 17

Applications ..............................................................3 Ventilation.............................................................. 17 Packing List ..............................................................3 Chapter 4.................................................................. 18 Shipping damage.......................................................3

Chapter 2 ....................................................................4 Startup procedure ................................................... 18

6000/7000 Series Hydrogen Purifier Cell Operations...................................................................................... 18

Gas Pressure and Specifications................................4

6000/7000 Series Hydrogen Purifier Cell Specifications and Features ..........................................4 Shut down............................................................... 19

Chapter 5.................................................................. 20 Purifier connections ..................................................4 Tubing material and surface treatment......................4 Filter specifications ...................................................4 Preventative Maintenance ...................................... 20

6000/7000 Series Hydrogen Purifier System Maintenance................................................................ 20

Mechanical specifications .........................................5 Input ports ........................................................... 20 Feed Hydrogen Purity ......................................... 20 Table 1. 6000/7000 Series Mechanical

Specifications and Dimensions .......................5 Periodic helium leak............................................... 21 Electrical Specifications............................................5 External Leak Detection (Inboard)...................... 21

Table 2. 6000/7000 Series Hydrogen Purifier Cell Heater Data ..............................................5

Across-the-Membrane Leak Detection ............... 22 Potential Interference with Leak Rate Measurements ..................................................... 22 Heater/Temperature Control .....................................6

Thermocouples..........................................................6 Troubleshooting the System................................... 24 6000/7000 Series Hydrogen Purifier Cell Plumbing Diagram ....................................................................7 UPH Output Flow Decrease................................ 24

Symptoms That Require Cell Replacement............ 24 6000/7000 Series Hydrogen Purifier Cell .................8 Heater Failure...................................................... 24 P+E 6000/7000 Series Hydrogen Purifier Cell Flow Diagram ....................................................................9 Leak test failure................................................... 24

Degraded UPH output ......................................... 24 Figure 4. P+E 6000/7000 Series Hydrogen Purifier Cell Flow Diagram.............................9 Tubular Flow Restrictor Anomalies ....................... 24

Replaceable Spare Parts ......................................... 25 Chapter 3 ..................................................................10 Recommended Spare Parts..................................... 25

Suggested gas connections......................................11

6000/7000 Series Hydrogen Purifier Cell Installation.......................................................................................10 Chapter 6.................................................................. 26

Limited warranty .................................................... 26 Power+Energy Warranty and Return Information 26

External Gas Connections....................................11 Return Authorization and Repairs .......................... 27 Table 3. Face Seal Fittings Table ..................11 Shipping damage .................................................... 27 Tubing dimensions..................................................11 Install 0.5 micron Filters .........................................11 Wiring Diagrams and Technical Drawings........ 28

Appendix A.................................................................. 28

Hydrogen input .......................................................11 6000/7000 Series Hydrogen Purifier Cell Wiring Diagram.................................................................. 29 Check valves ...........................................................12

Purge gas input........................................................12 6000/7000 Series Hydrogen Purifier Cell Dimensional Drawings Front View........................ 30 Ultra Pure Hydrogen outlet (UPH) .........................12

Vacuum pump connection ......................................12 6000/7000 Series Hydrogen Purifier Cell Dimensional Drawings Back View ........................ 31 Bleed outlet .............................................................13

Figure 5. Tubular Flow Restrictor .............13 6000/7000 Series Hydrogen Purifier Cell Dimensional Drawings Side View ......................... 32 Heat exchanger coil on the UPH output..................14

Cautions ..................................................................14 Appendix B.................................................................. 33Reverse pressurization .........................................15

Figure 6. Tubular Flow Restrictor .............15

6000/7000 Series Hydrogen Purifier Cell ii

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6000/7000 Series Hydrogen Purifier Cell ii

Safety Precautions.................................................33 Characteristics of Compressed Gases..................... 35 Equipment Usage ................................................... 36 Hydrogen .............................................................34

Hazardous Materials ............................................34 Glossary.................................................................. 38

Appendix C.................................................................. 38Avoid Serious Bodily Injury and Equipment Damage................................................................................35 Index....................................................................... 39 Use Only Trained Personnel ...................................35 Notes ............................................................................ 42

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Chapter

1Introduction

Congratulations. You have purchased the most reliable device of its kind in the industry, the Power+Energy (P+E) hydrogen purifier cell. This manual will guide you through proper operating procedures.

Theory of Operation The P+E hydrogen purifier consists of a 316 L grade stainless steel cell, incorporating a large diameter palladium (Pd) alloy tube as the diffusion element. Hydrogen gas is brought into contact with the inner surfaces of the palladium alloy tube which acts as a selective barrier, passing only atomic hydrogen through the tube wall, while excluding all other gases. Molecular hydrogen is adsorbed onto the surface where it is dissociated to become atomic hydrogen. The hydrogen atom shares its electron with the palladium metal lattice and diffuses through the lattice in a direction determined by the pressure gradient. The hydrogen atom recombines on the low pressure side of the membrane with another hydrogen atom, reclaims an electron, and is desorbed as an ultra pure hydrogen molecule.

Figure 1. P+E 6000 and 7000 Series Hydrogen Purifiers

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Applications Power+Energy hydrogen purifiers are ideal for installation in OEM equipment and in laboratories, fabs and plants where ultra-pure hydrogen is required for applications involving R&D, MOCVD and Si-based CVD semiconductor processes.

Packing List Each shipping crate should contain the following items:

• P+E Hydrogen Purifier

• Installation and Operations Manual (this manual)

• “Hydrogen Purifier Test Certificate” document

Shipping damage Each Power+Energy hydrogen purifier has been carefully tested and inspected before shipment. The purchaser should make visual checks upon receipt. Any physical damage should be noted and a claim filed immediately with the carrier. Most carriers will not honor any claim made after 7-15 days from the shipping date. If the equipment is received in damaged condition, request an immediate inspection by the carrier employee.

Power+Energy will assist in ensuring a satisfactory settlement from the carrier. Upon receipt of the carrier damage/inspection reports, Power+Energy will arrange, at our option, for either equipment repair or replacement. Please read the section on Return Authorization and Repairs located on page 27.

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26000/7000 Series Hydrogen Purifier Cell Specifications and Features

Gas Pressure and Specifications Maximum hydrogen feed gas inlet pressure (port A) 200 PSIG Minimum hydrogen feed gas purity ~99.95% Minimum nitrogen feed gas purity ~99.95% Ultra-pure hydrogen gas purity 99.9999999% Nitrogen feed gas inlet pressure (port A) >70% of hydrogen feed gas pressure Hydrogen bleed outlet flow rate (port C)

• Operating Typically 1 – 4% of Flow Rate NOTE: The lower the source gas purity the higher the bleed rate needs to be set.

Purifier connections All tubing connections on the cell are ¼" metal gasket face seal fittings.

Tubing material and surface treatment Finish of all UPH lines 316L electro-polished Finish on all UPH cell surfaces 316L micro-polished

Filter specifications Hydrogen / Nitrogen filter (F1) - 0.5 micron High Flow Sintered Filter (Swagelok ® part #SS-4F-VCR-05 or equivalent) shown as Filter 1 (F1) on “Figure 4. P+E Hydrogen Purifier Cell Flow Diagram” on page 8.

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Mechanical specifications

Model Number Length in inches Width in inches Weight in pounds

(approximate) PE6030 10.66 13.7 PE6060 15.34 13.7 PE6080 20.04 13.7 PE6100 20.04 13.7 PE6130 24.73 13.7 PE6160 29.42 13.7

Table 1. 6000/7000 Series Mechanical Specifications and Dimensions

Electrical Specifications

P+E 6000/7000 Series Hydrogen Purifier Cell Heater Data

P+E 6000 Series 6060 6080 6100 6115 6130 6145 6160

Number of Membranes 4 5 6 7 8 9 10

Number of Heaters 2 4 4 4 4 4 4

Rated Watts per Heater at 220 VAC 625 625 625 625 625 625 625

P+E 7000 Series 7080 7160 7240 7320 7400

Maximum Number of Membranes 5 10 15 20 25

Number of Heaters 2 4 4 6 6

Rated Watts per Heater at 220 VAC 625 625 825 825 825

Table 2. 6000/7000 Series Hydrogen Purifier Cell Heater Data

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Heater/Temperature Control The barrel band heaters are rated at 625 watts, 240 VAC. The heater wires at each end of cell are to be wired in parallel, and then connected to the controller. The hydrogen purifier cell should be heated at a rate that does not exceed 0.5 degrees C per second, averaged over any one-minute period, as indicated by the thermocouple. With the thermocouple sensing an external hydrogen purifier cell temperature of 405 degrees C during operation it should not exceed 475 degrees C. The P+E cell reaches operating temperature quickly because its design is thermodynamically efficient. Typically, from start up to operate takes approximately 15 minutes. Once operational, additional benefits are gained from this thermodynamically efficient design when additional flow is required. The P+E cell can respond in seconds.

Thermocouples Two “K” thermocouples measure the hydrogen purifier cell exterior temperature. Thermocouple placement has a direct bearing on the temperature reading. Temperature readings taken at different points on the hydrogen purifier cell exterior will vary. P+E positions the thermocouple in the hottest part of the cell exterior, under the heater. One thermocouple is typically used to control the cell temperature. The second thermocouple can be used as a backup if the first should fail.

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6000/7000 Series Hydrogen Purifier Cell Plumbing Diagram

palladium cell

Diffusion

tubu

lar f

low

rest

ricto

r

F1

tube

in tu

be h

eat e

xcha

nger

5/28/02gas

Representation not to scale

H2 feedport A

UPH port D

port E do not remove cap

port G do not remove cap

Bleed port C

checkvalve 1CK 1

checkvalve 3CK 3

cust

omer

to in

stal

lbl

eed

flow

met

er

customerto install

filter

Figure 2. 6000/7000 Series Hydrogen Purifier Cell Plumbing Diagram

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6000/7000 Series Hydrogen Purifier Cell

Contains the Tubular Flow Restrictor

Thermocouples

Support Bleed output port C

port G cap

Helium leak check port E

CK3

UPH output Port D

Tube-In-Tube Heat Exchanger H2 Feed Input Port A CK1

Support (Base of Heat Exchanger)

Figure 3 6000/7000 Series Hydrogen Purifier Cell

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UPH output Port D

Impurities exitthrough Bleedoutput Port C

H2 Feedinput Port A

center collection tube

rear support

front support

tube insidetube heatexchanger

Helium leakcheck port E

port G

tubularflowrestrictor

P+E 6000/7000 Series Hydrogen Purifier Cell Flow Diagram

Figure 4. P+E 6000/7000 Series Hydrogen Purifier Cell Flow Diagram

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36000/7000 Series Hydrogen Purifier Cell Installation Mount the purifier in the horizontal position on a supported surface with the aluminum mounting brackets provided. There is one 316 L stainless steel tube attached to the front center of the Bleed port C side of the cell that is used as a support, with the second support being the heat exchanger tubing (see Figure 3 on page 8) nearest the cell end cap. The cell has five (5) face seal fitting ports. There is one standard ¼” male face seal fitting attached to one end of the hydrogen purifier cell (see Figure 3 on page 8) labeled “Bleed output port C”, and four (4) face seal fittings; two (2) with check valves coming off the heat exchanger coil. These four (4) stainless steel face seal fittings are labeled “UPH output port D”, “H2 Feed Input Port A”, “Helium leak check port E”, and a capped port labeled “port G”. The cap on port “port G” should never be removed. This port is used in automated P+E systems.

IMPORTANT!

The cap on port “G”

should never be removed!

If leak test port E is not used it should also remain capped. Removal of the cap on port “G” can cause damage to the cell from reverse pressurization.

REVERSE PRESSURIZATION

Reverse pressurizing the palladium cell to a differential pressure greater than 50 PSIG will damage the palladium silver tubing in the purifier’s diffusion cell. Do not break open any fittings on the purifier piping while the purifier is pressurized. The palladium cell can be destroyed by the pressure differential caused by suddenly venting one side to atmosphere.

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Suggested gas connections External Gas Connections The recommended gas connections to the hydrogen purifier cell are shown in (see Figure 2 on page 7).

Face Seal Fittings 6000 female face seal male face seal

feed port A with check valve bleed port C UPH port D with check valve Leak port E port G

7000 feed port A with check valve bleed port C UPH port D with check valve Leak port E port G

Table 3. Face Seal Fittings Table

Tubing dimensions All face seal fittings are 1/4” stainless steel tubing. Best results are obtained by using 316 L grade electro polished, low-carbon stainless steel tubing on the UPH connections and lines.

Install 0.5 micron Filters Install a 0.5 micron High Flow Sintered Filter (Swagelok ® part #SS-4F-VCR-05 or equivalent) shown as Filter 1 (F1) on “Figure 2. P+E Hydrogen Purifier Cell Plumbing Diagram” on page 7.

Hydrogen input Connect the hydrogen gas stream that is to be purified through a 0.5 micron filter (Swagelok part # SS-4F-VCR-05) Filter1 and a normally closed (N.C.) valve with a “tee” to the 1/4” face seal fitting labeled “H2 feed port A”.

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IMPORTANT!

The pressure at “H2 feed port A” must always be greater than or equal to the pressure in the “UPH outlet port D”.

Check valves P+E uses two (2) Swagelok check valves #6L-CW4VR4 on the “H2 feed port A” (CK1), and on the UPH port D (CK3). A dual-stage regulator is recommended on the hydrogen feed to ensure greater accuracy and control of the delivery pressure. A single-stage regulator may show slight variation in the delivery pressure as the cylinder pressure falls.

Purge gas input Connect nitrogen or purge gas supply through a normally open (N.O.) valve and connect to the tee attached the hydrogen input line you assembled. The nitrogen purge gas pressure can be greater than or equal to the Hydrogen input but it must be greater than or equal to the UPH Outlet pressure. The maximum nitrogen pressure is 200 PSIG.

Ultra Pure Hydrogen outlet (UPH) A high purity check valve (CK3) is installed on UPH outlet port D (see Figure 2 on page 7). This will prevent the hydrogen purifier cell from accidentally being reversed pressurized and limit the amount of hydrogen that must back-diffuse through the palladium tube when the hydrogen purifier cell is shut down.

Vacuum pump connection Connect your vacuum pump and helium leak detector through a shutoff valve (V3) to the LEAK TEST PORT (port E) on the heat exchanger.

For immediately producing UPH, an external valve (valve 1) connected to the port labeled Leak Test Port (port E) allows a vacuum pump to remove the initial atmosphere of the cell.

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Bleed outlet A tubular flow restrictor is inserted in Bleed outlet port C. This device restricts the bleed rate so the cell tubing cannot be vented too quickly.

Figure 5. Tubular Flow Restrictor

IMPORTANT!

Removal of the tubular flow restrictor voids the warranty and can lead to reverse pressurization.

REVERSE PRESSURIZATION

Reverse Pressurization is defined as a pressure on the outside of the membrane that is greater than the pressure on the inside of the membrane. This state can cause damage to the membrane.

Reverse pressurizing the palladium cell to a differential pressure greater than 50 PSIG will damage the palladium silver tubing in the purifier’s diffusion cell. Do not break open any fittings on the purifier piping while the purifier is pressurized. The palladium cell can be destroyed by the pressure differential caused by suddenly venting one side to atmospheric pressure.

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Using a Rotameter or similar device, set the bleed flow rate at Bleed outlet port C high enough to ensure that impurities in the feed stream are flushed from the inside of the palladium tube. Typically, the lower the source gas purity (normally 1 to 4%) the higher the bleed rate needs to be set. Impurities are constantly flushed through the palladium tube inside the hydrogen purifier cell and exit through ¼” face seal fitting labeled “Bleed outlet port C”. Impurities will build up on the inside surface of the palladium tube and reduce the flow of UPH at UPH outlet port D if the Bleed outlet port C is closed.

IMPORTANT!

Do not shut off any valve connected to the Bleed outlet port C while the purifier is in operation,

r during shutdown and purgingo .

Heat exchanger coil on the UPH output The Tube-In-Tube Heat Exchanger installed before the check valve on the UPH outlet port D limits the outlet temperature of the gas to less than 50 degrees C. P+E uses the heat exchanger to lower the temperature of the outlet gas by warming the inlet feed gas, making the P+E cell more thermodynamically efficient.

The hydrogen purifier cell body contains a palladium tube. Hydrogen entering the cell through Hydrogen/Nitrogen feed port A is adsorbed by the inner surface of this palladium tube and diffuses through the metal lattice of the palladium tube and is available at UPH output port D. Since palladium is a selective filter for hydrogen, impurities are left behind and exit the hydrogen purifier cell through Bleed outlet port C.

Cautions On the Tube-In-Tube Heat Exchanger there are four (4) face seal fittings. The one on the end of the hydrogen purifier cell will be a permanently capped face seal fitting at “port G” (see Figure 3 on page 8). Do not remove the other three (3) protective caps on the end of the fittings “port A”, “port C”, and “port D” until you are ready to install the hydrogen purifier cell. “Port E” and “port G” are plugged. DO NOT REMOVE THE PLUG FROM PORT G. “Port E” may be unplugged and used to helium leak check the cell, but should remain closed (capped or plugged) during all other conditions. Particulate contamination cannot be allowed to enter the tubing. On the Bleed Port C end of the hydrogen purifier cell is a single tube used as a support.

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Reverse pressurization The pressure at the UPH PORT (port D) should never exceed the pressure on the H2 FEED (port A).

A tubular flow restrictor is inserted in Bleed outlet port C. This restricts the bleed rate so that the cell cannot be vented too quickly.

Figure 6. Tubular Flow Restrictor

IMPORTANT!

Removal of the tubular flow restrictor voids the warranty and can lead to reverse pressurization.

The feed pressure for the hydrogen and nitrogen to the cell should always be greater than or equal to UPH PORT (port D) pressure.

Reverse pressurizing the palladium cell to a differential pressure greater than 50 PSIG will damage the palladium silver tubing in the purifier’s diffusion cell. Do not break open any fittings on the purifier panel while the purifier is pressurized. The palladium cell can be destroyed by the pressure differential caused by suddenly venting one side to atmospheric pressure.

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Back-diffusion Back diffusion is defined as hydrogen diffusing in the reverse direction (from the outside of the palladium tube to the inside). When power is lost, or the hydrogen purifier cell is shutdown, the purifier must be purged with dry nitrogen entering the system through hydrogen feed port A. The ultra-pure hydrogen that has diffused through the palladium tube along with the ultra-pure hydrogen in the UPH outlet port D tubing between the hydrogen purifier cell and the in-line check valve CK3 will begin back diffusing through the palladium tube (see Figure 4 on page 9). This happens because the UPH pressure is greater on the outside of the palladium tube than the partial pressure of the nitrogen gas on the inside of the palladium tube. Typically, using a P+E microcontroller within 15 minutes or less, the hydrogen will be completely purged from the UPH side of the hydrogen purifier cell and the metal lattice of the palladium tube. A purge gas input pressure of greater than or equal to the maximum hydrogen input pressure will ensure this condition.

Contaminants

The UPH cell can be damaged if the feed gas contains halogens, unsaturated hydrocarbons, iron salts, halides, lead, mercury, sulfur compounds, or zinc. These contaminants must be eliminated from the feed gas. A feed gas purity of at least 99.95% is recommended.

The flow rate of UPH through the diffusion cell will be reduced if the palladium tubing becomes coated with solvents, oils, organic compounds, grease, pipe compounds, lubricants, or detergents. Do not allow these types of contaminants to enter the cell.

Oxygen / water

Hydrogen containing over 500 ppm of oxygen or water should never be allowed to enter the cell. Oxygen and hydrogen react exothermally on the surface of the Pd to form water. This may cause overheating and damage the diffusion cell. If the water vapor concentration builds up because the bleed rate is set too low, the water vapor may condense and form liquid water in the cell. Over time, this will cause embrittlement of the Pd membrane. In the case of contamination by back diffusion of materials such as saline or arsine the cell will need to be replaced.

If the contamination occurs on the feed side, it may be possible to restore the cell. Please call Power+Energy Customer Service at 215-942-4600 Mon – Fri, 8:00 a.m. – 5:00 p.m., U.S.A. EST (fax 215-942-9300) or email Customer Service at [email protected] before attempting to resolve a contamination related problem.

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Low flow A reduction in the UPH outlet flow at UPH port D indicates one or more of the following:

1. The diffusion cell is contaminated, typically with water vapor pressure due to high oxygen or water vapor concentration in the feed hydrogen.

2. The input pressure at H2 FEED (port A) has dropped.

3. The output pressure at UPH PORT (port D) has increased.

UPH Output Flow Decrease UPH output flow is a function of the partial pressure of hydrogen in the feed gas. The most common cause of reduction of output flow is the presence of water vapor in the feed gas. The effect of water vapor in the gases is temporary. The UPH output flow rate will be restored when the input feed gas has been changed to proper purity levels. The third cause for reduced UPH output flow rate is contamination by certain materials. See the Contamination section of this manual for more details.

Contamination In the case of contamination by back diffusion of gasses such as saline or arsine the cell will need to be replaced. If the contamination occurs on the feed side, it may be possible to restore the cell. Please call Power+Energy Customer Service at 215-942-4600 Mon – Fri, 8:00 a.m. – 5:00 p.m., U.S.A. EST (fax 215-942-9300) or email Customer Service at [email protected] before attempting to resolve a contamination related problem.

Ventilation For proper ventilation of this equipment, a distance of 1.2” (3.0 cm) must be maintained from the fans on the panel to any other surface. The palladium cell produces heat, and if it is installed in a closed area, such as a cabinet, fans may be required.

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46000/7000 Series Hydrogen Purifier Cell Operations

Before starting up the Power+Energy hydrogen purifier, be sure to read the sections labeled “Cautions” and “Contaminants” section of Chapter 3.

Connect all gas and vacuum pump lines as shown in the Figure 4. on page 8. The UPH Port D is shipped under vacuum. Evacuate the UPH port D side of cell through the check valve (CK3).

Startup procedure Make the correct connections and install the valves and filters. The hydrogen gas input valve should be closed. Open the nitrogen or purge gas input valve and adjust the bleed flow rate at Bleed outlet port C to 4% of total flow volume when starting up or shutting down (nitrogen), and 1 to 4% (depending on the purity of the feed hydrogen), when operating (hydrogen).

Apply power to the heater and heat the hydrogen purifier cell. Begin to supply hydrogen to H2 feed port A by closing the nitrogen gas input valve and opening the hydrogen gas input valve when the hydrogen purifier cell exterior reaches a temperature of 365 degrees C. Continue to heat the hydrogen purifier cell until the thermocouple is sensing an external hydrogen purifier cell temperature of 405 degrees C.

CAUTION

The cell should be heated at aone-minute period.

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DO NOT EXCEED 475 degrees C.

rate that does not exceed 0.5 degrees C per second averaged over any

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An increasing or decreasing pressure at UPH outlet (port D) and H2 feed (port A) will alter the flow rate at UPH outlet (port D). Do not ever completely close the Bleed outlet (port C). This will damage the cell by allowing impurities to build up on the inside surface of the palladium tube.

IMPORTANT!

Shut down When shutting down ttrapped in the palladiutube and allow impurit

To shutdown the purifFirst close the hydrogetemperature without dflow rate at Bleed outand the tubing betweetake approximately 15

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Do not ever completely close the Bleed outlet(port C). This will damage the cell by allowingimpurities to build up on the inside of thepalladium membrane!

he hydrogen purifier cell, water can remain in the palladium tube and hydrogen can be m tube’s metal lattice. The trapped water and hydrogen can destroy the palladium ies to contaminate the ultra pure hydrogen flow.

ier, purge the cell through H2 feed (port A) with an oxygen free purge gas (nitrogen). n feed valve and open the nitrogen or purge gas feed valve. This can be done at any amage to the hydrogen purifier cell. When shutting the purifier down, the bleed gas let (port C) should be 4% until the ultra-pure hydrogen in the hydrogen purifier cell n the hydrogen purifier cell and the UPH check valve has back diffused. This should minutes. Then turn off the power to the heaters.

19

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56000/7000 Series Hydrogen Purifier System Maintenance

Preventative Maintenance

Input ports

Install a 0.5 micron High Flow Sintered Filter (Swagelok ® part #SS-4F-VCR-05 or equivalent) shown as Filter 1 (F1) in “Figure 2. P+E Hydrogen Purifier Cell Plumbing Diagram” on page 7.

This will improve the long-term reliability of the check valves, solenoid valves, Rotameter and system. NOTE:

• Feed Hydrogen (port A) pressure should not exceed 200 PSIG.

Feed Hydrogen Purity For reliable cell operation, the following feed hydrogen limits should be observed:

• Carbon Monoxide less than 50 ppm • Halogens/compounds less than 1 ppm • Total Hydrocarbons less than 100 ppm • Mercury/compounds less than 0.01 ppm • Oxygen less than 500 ppm • Sulfur/compounds less than 0.02 ppm • Water vapor less than 500 ppm

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Periodic helium leak Prior to initial start-up, during routine maintenance or after power outages and other system upsets, helium leak tests are recommended to verify the integrity of the purifier. Highest sensitivity is obtained with helium leak detectors based on mass spectrometers that are specifically tuned for helium. A high vacuum pumping system is used to evacuate one side of the purifier and the external surface is exposed to helium at ambient or elevated pressure. The small helium atoms will easily penetrate even minuscule leaks and will be detected by the mass spectrometer that is connected to the pumping system. Even though highly unlikely when operated correctly, two types of leaks can potentially occur as a result of material failure:

• Defects in the external housing and connections of the purifier, in this context denoted as ‘external leaks’, as a result of leaking fittings or failed welds that can be detected by attaching the leak detector to the UPH side. By sequentially spraying of all external welds with helium or enclosing the unit in a He filled bag (inboard tests) while pumping on the UPH side, leaks can be located.

• The second and more common leak type in commercial Palladium membrane diffusers is a

result of rupture from exceeding pressure ratings of the membrane tubes, pinhole defects of the membrane or failure of the brazing joints of the membrane with the feed tube structures. These ‘across the membrane” leaks can be also detected by attaching the leak test instrument to the UPH port but instead of external application, the Helium is supplied through the feed inlet of the purifier and vented through the bleed.

Detailed step-by-step instructions for detecting external and across-the-membrane leaks are listed in the following procedures. Both measurements can also be performed while the purifier is at operating temperature. External Leak Detection (Inboard) 1. Cap the bleed and feed port of the purifier or alternatively maintain inert purge flow from the

feed port to the bleed and vent line. 2. Attach the leak detector to the UPH vacuum port and initiate pump-down. 3. After achieving 10-5 – 10-6 torr, the leak detector should display a measuring range of 10-9 – 10-

10 cc/sec, depending on the instrument sensitivity. 4. Spray all external welds and face seal fittings for at least 5 seconds each. Spray gaps in the

purifier housing for 15 seconds to detect defective welds on the diffusion cell. Helium will rapidly penetrate the thermal isolation material. If possible, prior to initial installation, cap feed and bleed ports, place the unit in a plastic bag and inflate the bag with helium for highest sensitivity.

5. A leak-tight unit will not display any detectable rise during the spraying (<1×10-9 cc/sec, depending on the detector sensitivity).

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6. Keep the leak detector connected to the UPH port for further “across-the-membrane” leak tests or:

7. If across-the-membrane leak measurements are not desired, close the valve to the vacuum/leak-test port, remove leak detector and proceed with purifier installation.

8. If a leak is detected above the specified rate on the external face seal fittings, replace gaskets and repeat test procedure. In case of leaks of the welds or housing, please contact Power+Energy Tech. Support at 215-942-4600, Mon – Fri, 8:00 a.m. – 5:00 p.m., U.S.A. EST or email at [email protected].

Across-the-Membrane Leak Detection 1. Initiate inert purge flow on the feed side and install a port for switching from inert purge to

helium purge. 2. If this procedure is performed after external leak tests and the leak detector is still connected to

the UPH vacuum port, initiate pump-down and proceed to step 4. 3. Attach the leak detector to the UPH vacuum port and initiate pump-down 4. After achieving 10-5 – 10-6 torr, the leak detector should display a measuring range of 10-9 – 10-

10 cc/sec, depending on the instrument sensitivity 5. Close the inert purge and initiate helium flow on the feed line at 20-100 psig for 10 minutes. 6. A leak-tight unit will not display any detectable rise during helium flow on the feed side

(<1×10-9 cc/sec, depending on the instrument sensitivity). 7. If a rise in leak rate above the specified rate is detected, please contact Power+Energy Tech.

Support at 215-942-4600, Mon – Fri, 8:00 a.m. – 5:00 p.m., U.S.A. EST or email at [email protected].

8. Close the vacuum port valve and disconnect the leak detector. 9. Proceed with purifier installation. Potential Interference with Leak Rate Measurements Several effects are known to potentially interfere with He leak rate measurements: • Slow out-gassing of hydrogen still dissolved in the palladium from previous operation can prevent

the leak detector from achieving the necessary vacuum for high sensitivity. Since high vacuum pumping systems typically are very inefficient in pumping hydrogen, several hours of pumping can be required to remove residual hydrogen from the system if insufficient purge time was provided prior to the leak tests. Slow but steady decrease in the displayed measuring range indicates removal of residual hydrogen and leak tests should be continued after the readings have stabilized prior to helium application.

• Additional interference with artificially high readings can be a result of high Helium backgrounds

in the ambient environment due to excessive spraying during testing. Back-diffusion of helium through the exhaust ports of the leak detector pump system causes slowly rising low-level response that could be mistaken for a small leak.

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• Even a defect-free membrane permits small amounts of helium to diffuse between grain boundaries, and in an enclosed system, helium could penetrate the membrane at very small rates. This effect is typically not large enough to be detected in routine tests as described above but could be measured if the purifier remains closed off for an extended time period for accumulation of helium on the UPH side.

No other preventative maintenance is required

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Troubleshooting the System UPH Output Flow Decrease UPH output flow is a function of the partial pressure of hydrogen of the feed gas. The most common cause of reduction of output flow is the presence of water vapor in the feed gas. The effect of water vapor in the gases is temporary. The UPH output flow rate will be restored by increasing the bleed flow rate or when the input feed gas has been changed to proper purity levels. The third cause for reduced UPH output flow rate is contamination by certain materials. See the Contamination section of this manual for more details (page 17.)

Symptoms That Require Cell Replacement Heater Failure Heater band failure may prevent the cell from maintaining the operating temperature and a steady flow rate. Generally, the system can tolerate failure of one or two heaters. A clamp-on ammeter is needed to check heater elements during operation or a resistance test can be done with the system un-powered. Leak test failure Leaks detected during He leak test based on isolation of the source of the leak to the purifier cell. Degraded UPH output Degraded UPH output flow rate due to contamination other than water. (Most reduced flow problems are due to water vapor in the system. See UPH Output Flow Decrease section above.) See Contamination section of manual for more information (page 17).

Tubular Flow Restrictor Anomalies The tubular flow restrictor in the bleed line (port C) is maintained at an elevated temperature to prevent the condensation of moisture in the flow restrictor. However, certain operating conditions, such as loss of electrical power in conjunction with a low bleed flow rate, may cause condensation of moisture in the flow restrictor.

This phenomenon is irreversible. If condensation of moisture in the tubular flow restrictor is suspected, the flow restrictor must be replaced before using the cell again.

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Replaceable Spare Parts

• Thermocouples • Check valves • Solenoid valves

Recommended Spare Parts

• Thermocouples • Check valves • Tubular flow restrictor

NOTE: Cell thermocouples are field-replaceable and do not require cell replacement.

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6Power+Energy Warranty and Return Information

Limited warranty P+E warrants that each palladium hydrogen purifier will be free from defects in workmanship, design, materials, and quality for a period of one year from the date of delivery to the customer. In the event, and only in the event, that any such defect is discovered and reported within the warranty period, P+E will repair or replace the defective Product, at its sole option, and at its sole expense. THIS WARRANTY IS IN LIEU OF ANY OTHER WARRANTY, EXPRESS OR IMPLIED, INCLUDING ANY IMPLIED WARRANTY OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE, AND WILL CONSTITUTE THE SOLE REMEDY OF CUSTOMER UPON ANY CLAIM OR DAMAGE ARISING FROM SUCH DEFECT. THIS WARRANTY WILL NOT APPLY TO DEFECTS OR DAMAGE ARISING FROM (i) PERIPHERAL SYSTEMS; (ii) IMPROPER OR NEGLIGENT USE OR OPERATION; (iii) IMPROPER MAINTENANCE; (iv) IMPROPER INSTALLATION; (v) IMPURITIES IN THE FEED GAS IN QUANTITIES BEYOND THOSE PERMITTED, OR OF A TYPE NOT PERMITTED, BY P+E’s OPERATING MANUAL; (vi) REVERSE PRESSURIZATION; (vii) EROSION OR CORROSION; (viii) MODIFICATIONS OF THE PRODUCT BY CUSTOMER, OR BY ANY PERSONNEL NOT TRAINED BY P+E, OR (ix) REMOVAL OF THE TUBULAR FLOW RESTRICTOR. IN NO EVENT WILL P+E BE LIABLE FOR CONSEQUENTIAL DAMAGES, INCLUDING LOST PROFITS, OR INCIDENTAL DAMAGES INCURRED BY ANY CUSTOMER, DIRECTLY OR INDIRECTLY, IN CONNECTION WITH THE PURCHASE, HANDLING OR USE OF ANY PALLADIUM HYDROGEN PURIFIER. There are no user serviceable parts in the palladium hydrogen purifier. Only P+E trained and authorized personnel should be allowed to service P+E equipment. THIS WARRANTY IS VOID IF P+E EQUIPMENT IS SERVICED BY PERSONNEL NOT TRAINED AND NOT AUTHORIZED BY P+E. Palladium hydrogen purifiers must be used only authorized personnel, in a controlled environment. Refer all questions to the Power+Energy operations manual or call our Customer service department at 215-942-4600 Mon – Fri, 8:00 a.m. – 5:00 p.m., U.S.A. EST (e-mail [email protected]).

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Return Authorization and Repairs If a fault develops, notify Power+Energy and provide us with a complete description of the problem, including the purifier Model Number and Serial Number. On receipt of this information, service or shipping instructions will be issued. ONLY IF RETURN OF THE UNIT IS AUTHORIZED, send it to us prepaid and repairs will be made at the factory. If the unit is not covered by warranty, or if it is determined that the fault is caused by misuse, repairs will be made at the expense of the customer. An estimate of the cost of these repairs will be submitted for approval prior to beginning any work.

Shipping damage Each Power+Energy hydrogen purifier has been carefully tested and inspected before shipment. The purchaser should make visual and operational checks upon receipt. Any physical damage should be noted and a claim filed immediately with the carrier. Most carriers will not honor any claim made after 7-15 days from the shipping date. If the equipment is received in damaged condition, request an immediate inspection by the carrier employee.

Power+Energy will assist in ensuring a satisfactory settlement from the carrier. Upon receipt of the carrier damage/inspection reports, Power+Energy will arrange, at our option, for either equipment repair or replacement. Please read the section on Return Authorization and Repairs located on page 27.

If you have any questions or if we can be of further service, Customer Service can be reached at 215-942-4600 (fax: 215-942-9300) Mon – Fri, 8:00 a.m. – 5:00 p.m., U.S.A. EST. Or e-mail us at [email protected]

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Appendix A

Wiring Diagrams and Technical Drawings

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Page 33: Installation and Operations Manual Power+Energy Hydrogen

"DIM A"

6.4

5.0

1.2

1.0

2.8

5.5

" DIM B"

7.8

"DIM D"

.8

UPH

FEED

BLEED

FRONT VIEW

MODEL NUMBERPE6060PE6080PE6100PE6130PE6160

DIM A6.316.316.316.316.31

DIM B13.213.213.213.213.2

DIM C15.620.420.425.230.0

DIM D10.510.510.510.510.5

THIS DRAWING APPLIES TO THE FOLLOWING MODELS

D

C

B

AA

B

C

D

12345678

8 7 6 5 4 3 2 1

REVISIONS

REV. DESCRIPTION DATE APPROVEDZONE

UNLESS OTHERWISE SPECIFIED:

SCALE: 1:2 WEIGHT: SHEET 1 OF 3

REVDWG. NO.

BSIZE

TITLE:

NAMEDATE

Q.A.

MFG APPR.

ENG APPR.

CHECKED

DESIGNED

FINISH

MATERIAL

INTERPRET GEOMETRICTOLERANCING PER:

APPLICATION

USED ONNEXT ASSY

1-28-02

B6000

6000 SERIES CELL

106 RAILROAD DRIVEIVYLAND, PA 18974

T - 215-942-4600F - 215-942-9300

www.purehydrogen.com

POWER & ENERGY

POWER & ENERGYDIMENSIONS ARE IN INCHESTOLERANCES:

FRACTIONAL 1/64ANGULAR: 1

.XX .01.XXX .005

.XXXX .0005

SEE NOTES

SEE NOTES

PROPRIETARY AND CONFIDENTIAL

THE INFORMATION CONTAINED IN THISDRAWING IS THE SOLE PROPERTY OF

POWER & ENERGY. ANY REPRODUCTION IN PART OR AS A WHOLE

WITHOUT THE WRITTEN PERMISSION OFPOWER & ENERGY IS

PROHIBITED.

+EWD

. ....

Page 34: Installation and Operations Manual Power+Energy Hydrogen

"DIM C"

27.7 1.4

SIDE VIEW

DIM D10.510.510.510.510.5

DIM C15.620.420.425.230.0

DIM B13.213.213.213.213.2

DIM A6.316.316.316.316.31

THIS DRAWING APPLIES TO THE FOLLOWING MODELS

MODEL NUMBERPE6060PE6080PE6100PE6130PE6160

D

C

B

AA

B

C

D

12345678

8 7 6 5 4 3 2 1

REVISIONS

REV. DESCRIPTION DATE APPROVEDZONE

UNLESS OTHERWISE SPECIFIED:

SCALE: 1:3 WEIGHT: SHEET 2 OF 3

REVDWG. NO.

BSIZE

TITLE:

NAMEDATE

Q.A.

MFG APPR.

ENG APPR.

CHECKED

DESIGNED

FINISH

MATERIAL

INTERPRET GEOMETRICTOLERANCING PER:

APPLICATION

USED ONNEXT ASSY

1-28-02

B6000

6000 SERIES CELL

106 RAILROAD DRIVEIVYLAND, PA 18974

T - 215-942-4600F - 215-942-9300

www.purehydrogen.com

POWER & ENERGY

POWER & ENERGYDIMENSIONS ARE IN INCHESTOLERANCES:

FRACTIONAL 1/64ANGULAR: 1

.XX .01.XXX .005

.XXXX .0005

SEE NOTES

SEE NOTES

PROPRIETARY AND CONFIDENTIAL

THE INFORMATION CONTAINED IN THISDRAWING IS THE SOLE PROPERTY OF

POWER & ENERGY. ANY REPRODUCTION IN PART OR AS A WHOLE

WITHOUT THE WRITTEN PERMISSION OFPOWER & ENERGY IS

PROHIBITED.

+EWD

. ....

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SUPPORT BRACKET PLACEMENT

11.3

2.8

5.0

13.2

BACK VIEW

D

C

B

AA

B

C

D

12345678

8 7 6 5 4 3 2 1

REVISIONS

REV. DESCRIPTION DATE APPROVEDZONE

UNLESS OTHERWISE SPECIFIED:

SCALE: 1:2 WEIGHT: SHEET 3 OF 3

REVDWG. NO.

BSIZE

TITLE:

NAMEDATE

Q.A.

MFG APPR.

ENG APPR.

CHECKED

DESIGNED

FINISH

MATERIAL

INTERPRET GEOMETRICTOLERANCING PER:

APPLICATION

USED ONNEXT ASSY

1-28-02

B6000

6000 SERIES CELL

106 RAILROAD DRIVEIVYLAND, PA 18974

T - 215-942-4600F - 215-942-9300

www.purehydrogen.com

POWER & ENERGY

POWER & ENERGYDIMENSIONS ARE IN INCHESTOLERANCES:

FRACTIONAL 1/64ANGULAR: 1

.XX .01.XXX .005

.XXXX .0005

SEE NOTES

SEE NOTES

PROPRIETARY AND CONFIDENTIAL

THE INFORMATION CONTAINED IN THISDRAWING IS THE SOLE PROPERTY OF

POWER & ENERGY. ANY REPRODUCTION IN PART OR AS A WHOLE

WITHOUT THE WRITTEN PERMISSION OFPOWER & ENERGY IS

PROHIBITED.

+EWD

. ....

Page 36: Installation and Operations Manual Power+Energy Hydrogen

"DIM A"

2.8

1.7 5.3

11

3.8

5.5

7.8

"DIM B"

"DIM D"

1.0

UPH

FEEDTHIS DRAWING APPLIES TO THE FOLLOWING MODELS

MODEL NUMBERPE7080PE7100PE7115PE7130PE7145PE7160PE7180PE7195PE7210PE7220PE7245PE7260PE7280PE7290PE7310PE7325PE7340PE7360PE7375PE7390PE7405

DIM A8.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.50

DIM B14.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.8

DIM C8.0

13.013.013.013.013.018.018.018.018.018.023.023.023.023.023.028.028.028.028.028.0

DIM D10.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.5

D

C

B

AA

B

C

D

12345678

8 7 6 5 4 3 2 1

REVISIONS

REV. DESCRIPTION DATE APPROVEDZONE

UNLESS OTHERWISE SPECIFIED:

SCALE: 1:2 WEIGHT: SHEET 1 OF 3

REVDWG. NO.

BSIZE

TITLE:

NAMEDATE

Q.A.

MFG APPR.

ENG APPR.

CHECKED

DESIGNED

FINISH

MATERIAL

INTERPRET GEOMETRICTOLERANCING PER:

APPLICATION

USED ONNEXT ASSY

2-14-02

B7000-5-25

7000 SERIES CELL

106 RAILROAD DRIVEIVYLAND, PA 18974

T - 215-942-4600F - 215-942-9300

www.purehydrogen.com

POWER & ENERGY

POWER & ENERGYDIMENSIONS ARE IN INCHESTOLERANCES:

ANGULAR: 3.X .5

.XX .05.XXX .005

SEE NOTES

SEE NOTES

PROPRIETARY AND CONFIDENTIAL

THE INFORMATION CONTAINED IN THISDRAWING IS THE SOLE PROPERTY OF

POWER & ENERGY. ANY REPRODUCTION IN PART OR AS A WHOLE

WITHOUT THE WRITTEN PERMISSION OFPOWER & ENERGY IS

PROHIBITED.

+EWD

. ....

Page 37: Installation and Operations Manual Power+Energy Hydrogen

1.1DIM C

18.0

BLEED

SIDE VIEW

DIM D10.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.510.5

DIM C8.0

13.013.013.013.013.018.018.018.018.018.023.023.023.023.023.028.028.028.028.028.0

DIM B14.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.814.8

DIM A8.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.508.50

MODEL NUMBERPE7080PE7100PE7115PE7130PE7145PE7160PE7180PE7195PE7210PE7220PE7245PE7260PE7280PE7290PE7310PE7325PE7340PE7360PE7375PE7390PE7405

THIS DRAWING APPLIES TO THE FOLLOWING MODELSD

C

B

AA

B

C

D

12345678

8 7 6 5 4 3 2 1

REVISIONS

REV. DESCRIPTION DATE APPROVEDZONE

UNLESS OTHERWISE SPECIFIED:

SCALE: 1:2 WEIGHT: SHEET 2 OF 3

REVDWG. NO.

BSIZE

TITLE:

NAMEDATE

Q.A.

MFG APPR.

ENG APPR.

CHECKED

DESIGNED

FINISH

MATERIAL

INTERPRET GEOMETRICTOLERANCING PER:

APPLICATION

USED ONNEXT ASSY

2-14-02

B7000-5-25

7000 SERIES CELL

106 RAILROAD DRIVEIVYLAND, PA 18974

T - 215-942-4600F - 215-942-9300

www.purehydrogen.com

POWER & ENERGY

POWER & ENERGYDIMENSIONS ARE IN INCHESTOLERANCES:

ANGULAR: 3.X .5

.XX .05.XXX .005

SEE NOTES

SEE NOTES

PROPRIETARY AND CONFIDENTIAL

THE INFORMATION CONTAINED IN THISDRAWING IS THE SOLE PROPERTY OF

POWER & ENERGY. ANY REPRODUCTION IN PART OR AS A WHOLE

WITHOUT THE WRITTEN PERMISSION OFPOWER & ENERGY IS

PROHIBITED.

+EWD

. ....

Page 38: Installation and Operations Manual Power+Energy Hydrogen

8.9

11.5

1.7

2.8

8.5

5.5

14.8

BLEED

D

C

B

AA

B

C

D

12345678

8 7 6 5 4 3 2 1

REVISIONS

REV. DESCRIPTION DATE APPROVEDZONE

UNLESS OTHERWISE SPECIFIED:

SCALE: 1:2 WEIGHT: SHEET 3 OF 3

REVDWG. NO.

BSIZE

TITLE:

NAMEDATE

Q.A.

MFG APPR.

ENG APPR.

CHECKED

DESIGNED

FINISH

MATERIAL

INTERPRET GEOMETRICTOLERANCING PER:

APPLICATION

USED ONNEXT ASSY

2-14-02

B7000-5-25

7000 SERIES CELL

106 RAILROAD DRIVEIVYLAND, PA 18974

T - 215-942-4600F - 215-942-9300

www.purehydrogen.com

POWER & ENERGY

POWER & ENERGYDIMENSIONS ARE IN INCHESTOLERANCES:

ANGULAR: 3.X .5

.XX .05.XXX .005

SEE NOTES

SEE NOTES

PROPRIETARY AND CONFIDENTIAL

THE INFORMATION CONTAINED IN THISDRAWING IS THE SOLE PROPERTY OF

POWER & ENERGY. ANY REPRODUCTION IN PART OR AS A WHOLE

WITHOUT THE WRITTEN PERMISSION OFPOWER & ENERGY IS

PROHIBITED.

+EWD

. ....

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Appendix B

Safety Precautions

DANGER !

FOLLOW ALL SAFETY PRECAUTIONS

Under no circumstances should attempts be made to circumvent compressed gas safety

equipment.

Compressed gases and associated equipment are potentially dangerous; persons that have not been formally trained must not use them.

Risk of personal injury or damage to

equipment may be avoided only by a strict adherence to all safety precautions.

This manual cannot replace formal training in compressed gas equipment safety principles and, accordingly, is intended only as a reminder to adequately trained personnel that already understand applicable safety practices.

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WARNING!

Hydrogen

Hydrogen is combustible at concentrations of 4.0 % to 75.0 % in air Hydrogen has an auto ignition temperature of 571°C (844°K or 1,060°F) Hydrogen detonates at concentrations between 18% and 59% in air. Hydrogen can be ignited with an electrical discharge exceeding the energy equivalent to 200mA at 24 volts DC. Hydrogen is nontoxic; hence OSHA PEL (TWA or C) are not listed. But hydrogen can act as an asphyxiant by displacing the necessary amount of oxygen required to support life.

Hazardous Materials Hazardous materials must be managed properly. Hydrogen is classified as hazardous production materials (HPM) according to the Uniform Fire Code (UFC); all requirements of that code, where adopted, must be observed. These requirements, among others, include:

• Installation of suitable facility exhaust equipment, use of welded external piping connections, and installation of hazardous gas detectors.

• Operate the unit in a well-ventilated area equipped with hydrogen leak detector and alarm system, and a fire protection system that meets the criteria of NFPA 30.

• Never use cylinders of hydrogen in areas where flames, excessive heat, or sparks, may occur. • Electrical equipment in the vicinity, such as fans and motors, must meet Class I, Div 1

standards. Utilize only explosion-proof equipment and spark-proof tools in areas where hydrogen is handled.

• Commonly used personal equipment for communication, such as cellular phones and beepers, are capable of producing electrical sparks and should not be used near hydrogen lines.

• Ground all equipment and lines used with hydrogen. • Suitable equipment, such as flash arrestors in vent lines, is strongly recommended. • Label all hydrogen lines with appropriately color-coded labels (ANSI Code: Black lettering on

yellow background)

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Avoid Serious Bodily Injury and Equipment Damage

Modification of equipment, failure to follow

recommended procedures or circumvention of instructions in this manual can result in serious

bodily injury and equipment damage.

Follow all instructions carefully; should a question arise, consult with an authorized Power+Energy Applications Engineer by calling Power+Energy, Inc. at (215) 942-4600, Monday-Friday from 8:00 a.m. to 5 p.m., U.S.A. EST.

Use Only Trained Personnel Installation, operation, and maintenance of gas control equipment should be executed by trained personnel only. All compressed gases are potentially hazardous and must be handled only by trained personnel.

CPtEc

Incorrect execution of ostensibly simple operations can cause fire, explosion, or atmospheric release of hazardous/toxic gas. An explosion or a leak may also cause costly contamination of process equipment from exposure of metal alkyls (typically used on MOCVD Tools) to atmospheric air.

haracteristics of Compressed Gases hysical characteristics of compressed gases and approved compressed gas equipment handling

echniques are described in the Compressed Gas Association’s Handbook of Compressed Gases, 4th dition, Van Nostrand Reinhold, NYC (1998). This useful book should be readily available for onsultation at all facilities where compressed gases are used or stored.

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Equipment Usage Use of this equipment with other than intended gases (hydrogen, nitrogen and helium) may create potentially hazardous conditions. This equipment is designed to purify hydrogen gas from a liquefied source or from cylinders, only. Do not use this equipment with any other gas. • Unless otherwise designated, Power+Energy purifiers are rated for a maximum operating

pressure of 200 psig. An upstream process gas source pressure regulator and overpressure relief device must be installed when a potential exists for over-pressurization of the Power+Energy purifier.

• To minimize post-purification contamination and facilitate purging, the purifier should be installed as close as possible to the process tool. Typically, for MOCVD applications, the Power+Energy purifier is directly mounted on the tool.

• DO NOT, under any circumstance, operate purifier without installation of the flow restrictor provided with the Power+Energy purifier. Operation of purifier without the flow restrictor will cause failure of the purifier and contamination of the process lines.

• DO NOT operate the purifier with oxygen concentrations exceeding 500 ppm. on average. Overheating of the cell and potential damage to the palladium membrane may result.

• Avoid using hydrogen from petroleum refineries. Sulfur-containing compounds or unsaturated hydrocarbons in the feed hydrogen will poison the surface of the palladium membrane. If the flow rate drops and poisoning of the cell is suspected, contact Power+Energy, Inc. Applications Engineer at (215) 942-4600, Monday-Friday from 8 a.m. to 5 p.m. U.S.A. EST.

• Preferably use hydrogen that is free from compressor oils, grease, and lubricants. Mercury, iron, zinc, and lead particulates in hydrogen may cause irreparable damage to the palladium membrane. A particulate filter must always be used in the feed hydrogen line. If the factory-installed filter (if provided, some Models only) on the feed hydrogen is blocked, replace filter before operating the purifier again.

• Do not allow the palladium cell to cool below 300°C when hydrogen is still present in the cell. • Ensure nitrogen is always available to purge the cell in the event of a power failure. Increase

bleed flow rate to ~ 10% of feed when shutting down the cell. • Always replace all components, fasteners, labels, and other items exactly as originally installed;

don’t modify any equipment without proper authorization from Power+Energy, Inc. • Do not tamper with the purifier cell or the controller (if provided). Unauthorized repairs or

modification may cause a hazardous situation and void the warranty. • Store spare equipment in a cool, dry, and secure place. • Purifiers or controllers not in adequate operating condition must not be used. Do not attempt to use

equipment that is not operating properly. • Never attempt to defeat interlocks or other safety devices. • Do not attempt to open manual valves, or otherwise allow air to contact the purifier, prior to

installation. Valves must remain closed until installation is complete and all equipment has been suitably helium leak tested and purged.

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• Material Safety Data Sheets for all gases and purification media used in the facility should be available for consultation by all concerned personnel. These data sheets are obtainable from gas suppliers.

• Vent all equipment of hydrogen prior to disassembly. Be aware that unexpected jet noise accompanying gas release can frighten workers and precipitate accidents. Accidental process gas release is more likely to occur during maintenance than during routine operation.

• Equipment used in hazardous gas service must be purged immediately prior to disassembly. • Personnel working with hazardous gases or contaminated components must be provided with

suitable protective gear. • Disconnect electric power before attempting any repairs.

NOTE: Other than the thermocouples and the flow restrictor, the palladium cell (5000 Series, 6000 Series and 7000 Series, cell only) does NOT contain any user-serviceable parts. Attempts to repair any other components will void the warranty of the cell.

• Should fire, release of toxic or otherwise hazardous gases, or other potentially dangerous situation arise, close the process gas cylinder valve, if possible, and then evacuate the region.

• Personnel installing and moving equipment must follow proper lifting and manipulation techniques per NIOSH publication 81-122.

• Mechanical or electrical maintenance procedures should follow lockout / tagout practices appropriate for the hazard level and facility complexity. Reference OSHA document 29 CFR 1910.147 (Control of Hazardous Energies, Lockout / Tagout) and 29 CFR 1910.331-335 (Electrical Safety-Related Work Practices) as concerns lockout/ tagout procedures.

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Appendix C

Glossary ACGIH American Council of Governmental Industrial Hygienists C OSHA Ceiling exposure limit . HPM Hazardous production material process gas as defined by the Uniform Fire Code

standards. Kgf/cm2 Kilogram force per square centimeters. Units of pressure. µm Micron or Micro-Meter = 1 x 10-6 Meters. N/m2 Newtons per square meters. Units of pressure. OSHA Occupational Safety & Health Agency PEL Permissible Exposure Limit. Established by OSHA and may be expressed as either a

time-weighted average (TWA) or as a ceiling (C) exposure limit. ppb parts per billion. Units of impurity concentration in gas (= 10 -9). ppm parts per million. Units of impurity concentration in gas (= 10 -6). psia Pounds per square inch (absolute). Units of pressure (absolute pressure). psig Pounds force per square inch (gauge). Units of Pressure (gauge pressure). sccs standard cubic centimeters per second. Leakage rate expressed in cm3/sec at 25°C and

1 atm pressure. slpm standard Liters per minute. Flow rate expressed in lit/min at 25°C and 1 atm pressure. STEL Short Term Exposure Limit. Recommended by ACGIH. Maximum concentration for a

continuous exposure period of 15 minutes with a maximum of 4 such periods per day, with at least 60 minutes between exposure periods.

TLV Threshold Limit Value. Term used by ACGIH to express the airborne concentration of a material to which nearly all workers can be exposed day after day.

TWA Time Weighted Average VCR A metal gasket face-seal connection consisting of a replaceable metal crush gasket and

toroid-shaped glands. Trademark of Cajon Company, Crawford Fittings, Solon, OH.

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Index 3 embrittlement................................................................ 16

exothermally ................................................................. 16 316L ................................................................................4 F 4 fans ............................................................................... 17 4000 Series ..........................4, 7, 8, 10, 18, 29, 30, 31, 32 fax..................................................................... 16, 17, 27 feed ..........4, 11, 12, 14, 15, 16, 17, 18, 19, 20, 21, 22, 24 7 feed gas............................................................... 4, 16, 24 7000 Series .................. 2, 4, 5, 7, 8, 10, 18, 29, 30, 31, 32 female ........................................................................... 10 filter .................................................................... 4, 11, 14 A fittings........................................................... 4, 10, 14, 21

aluminum.......................................................................10 flow..................4, 6, 14, 15, 16, 17, 18, 19, 21, 22, 24, 25 Appendix A ...................................................................28 flow rate.......................................4, 14, 16, 17, 18, 19, 24 arsine .......................................................................16, 17

G atomic hydrogen..............................................................2

gas......................................2, 4, 11, 12, 14, 16, 18, 19, 24 B gas purity .................................................................. 4, 16

back diffusion..........................................................16, 17 gasket.............................................................................. 4 bleed ......................................4, 13, 14, 15, 16, 18, 19, 21

H bleed port.......................................................................21 brackets .........................................................................10 H2 ........................................................................... 15, 17 brazing joints .................................................................21 halides........................................................................... 16

halogens........................................................................ 16 C He ..................................................................... 21, 22, 24

C 28 heater failure................................................................. 24 carbon............................................................................11 heaters....................................................................... 6, 19 carrier ........................................................................3, 27 helium......................................................... 12, 21, 22, 23 case....................................................................16, 17, 22 helium leak test............................................................. 21 cell .. 2, 4, 6, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 24,

25 hydrogen .2, 3, 4, 6, 10, 11, 12, 14, 15, 16, 17, 18, 19, 20,

22, 24, 26, 27 check valve................................10, 12, 14, 16, 18, 19, 20 hydrogen purifier2, 3, 6, 10, 11, 12, 14, 16, 18, 19, 26, 27 CK3 .........................................................................12, 18 hydrogen purifiers..................................................... 3, 26 close.........................................................................19, 22

I closed.....................................................11, 14, 17, 18, 23 connections....................................................4, 11, 18, 21 impurities................................................................ 14, 19 contaminants .................................................................16 [email protected] .............................. ii, 16, 17, 26 contamination ..............................................14, 16, 17, 24 inlet pressure................................................................... 4 controller .........................................................................6 input.................................................11, 12, 16, 17, 18, 24

input pressure.......................................................... 16, 17 D inspected ................................................................... 3, 27

damage ....................................................3, 10, 16, 19, 27 inspection.................................................................. 3, 27 date ......................................................................3, 26, 27 installation .......................................................... 3, 21, 22 detector..............................................................12, 21, 22 iron................................................................................ 16 diffusion ..................................................2, 16, 17, 21, 22 iron salts........................................................................ 16 diffusion cell......................................................16, 17, 21 Ivyland............................................................................ ii dimensions.....................................................................11

L display .....................................................................21, 22

large diameter ................................................................. 2 E lead ............................................................................... 16

electro-polished ...............................................................4

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purehydrogen.com .............................................. ii, 26, 27 leak ........................................................10, 12, 21, 22, 24 purge................................................12, 16, 18, 19, 21, 22 leak test........................................................10, 21, 22, 24

leak test port ..................................................................10 Q low pressure ....................................................................2 quality ........................................................................... 26 M R maintenance.............................................................21, 23

manual ...................................................................2, 3, 24 repairs ........................................................................... 27 measurements ..........................................................21, 22 reverse pressurization ................................................... 10 membrane................................................2, 16, 21, 22, 23 Rotameter ............................................................... 14, 20 mercury .........................................................................16

S metal lattice ...................................................2, 14, 16, 19 microcontroller ..............................................................16 saline....................................................................... 16, 17 micron .................................................................4, 11, 20 service..................................................................... 26, 27 micro-polished.................................................................4 shipping date............................................................. 3, 27

shutdown................................................................. 16, 19 N solenoid ........................................................................ 20 nitrogen .............................................4, 12, 15, 16, 18, 19 solenoid valves ............................................................. 20 nitrogen feed....................................................................4 specifications .............................................................. 4, 5

stainless steel ...................................................... 2, 10, 11 O sulfur............................................................................. 16 sulfur compounds ......................................................... 16 O 12 surface treatment............................................................. 4 off ......................................................................10, 19, 23 Swagelok ...................................................... 4, 11, 12, 20 on 2, 3, 4, 6, 10, 11, 12, 14, 15, 16, 17, 18, 19, 20, 21, 22,

23, 24, 27 T OP..................................................................................26 open...................................................................12, 19, 24 temperature ........................................6, 14, 18, 19, 21, 24 operate .............................................................................6 test .......................................................................... 22, 24 operations manual .........................................................26 tested......................................................................... 3, 27 outlet................................ 4, 12, 13, 14, 15, 16, 17, 18, 19 testing ........................................................................... 22 output.................................................................14, 17, 24 thermocouple ............................................................ 6, 18 output pressure ..............................................................17 time................................................................... 16, 22, 23 oxygen ...............................................................16, 17, 19 tube ..............................................2, 10, 12, 14, 16, 19, 21

tubing.................................................4, 11, 13, 14, 16, 19 P tubular flow restrictor ............................................. 13, 15 P+E........................ 2, 3, 4, 5, 6, 10, 11, 12, 14, 16, 20, 26 U PA................................................................................... ii palladium...............................2, 12, 14, 16, 17, 19, 22, 26 ultra-pure ............................................................ 3, 16, 19 Pd ..............................................................................2, 16 ultra-pure hydrogen ............................................ 3, 16, 19 PE6080 ............................................................................5 unsaturated hydrocarbons ............................................. 16 PE6100 ............................................................................5 UPH...............4, 12, 14, 15, 16, 17, 18, 19, 21, 22, 23, 24 PE6130 ............................................................................5 UPH port..................................................... 12, 18, 21, 22 port A .................. 4, 10, 11, 12, 14, 15, 16, 17, 18, 19, 20

V port B...............................................................................4 port C...............................................10, 13, 14, 15, 18, 19 V3 ................................................................................. 12 port D ........................................10, 12, 14, 15, 16, 17, 19 VAC............................................................................ 5, 6 port E.......................................................................10, 12 vacuum pump ............................................. 12, 18, 21, 22 power...........................................................16, 18, 19, 21 valves................................................................ 18, 20, 25 Power+Energy.........................ii, 3, 16, 17, 18, 22, 26, 27 vapor........................................................... 16, 17, 20, 24 powered .........................................................................24 VCR.............................................4, 10, 11, 14, 20, 21, 22 ppm..........................................................................16, 20 VCR fittings................................................ 10, 14, 21, 22 pressure gradient .............................................................2 ventilation ..................................................................... 17 PSIG ....................................................................4, 12, 20

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W

warranty...................................................................26, 27 water............................................................16, 17, 19, 24

watts................................................................................ 6 welds....................................................................... 21, 22 www.purehydrogen.com ................................................ ii

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Notes

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Power+Energy, Inc.106 Railroad Drive

Ivyland, PA USAP 215 942 4600 F 215 942 9300

e-mail: [email protected] web site: www.purehydrogen.com

Represented in Japan by:Richmore International Corporation

Shiroganedai Central Building. 4F, 3-6 Shiroganedai, 5 Chrome Minato-ku, TokyoP (03)3440-0027 F (03)3440-0127