Micromeritics VacPrep 061 User manual

VacPrep 061
Operator’s Manual
061-42802-01
Feb 2013

© Micromeritics Instrument Corporation 2002-2013. All rights reserved.

Form No. 008-42104-00
Rev. 12/95
WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each
instrument it manufactures to be free from defects in material and workmanship impairing its usefulness under
normal use and service conditions except as noted herein.
Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any
instrument or defective parts when returned prepaid to us and which our examination discloses to have been
defective. The purchaser is responsible for all transportation charges involving the shipment of materials for war-
ranty repairs. Failure of any instrument or product due to operator error, improper installation, unauthorized
repair or alteration, failure of utilities, or environmental contamination will not constitute a warranty claim. The
materials of construction used in MICROMERITICS instruments and other products were chosen after extensive
testing and experience for their reliability and durability. However, these materials cannot be totally guaranteed
against wear and/or decomposition by chemical action (corrosion) as a result of normal use.
Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of
shipment.
No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and
authorization to return the instrument or product. All repairs or replacements are made subject to factory inspec-
tion of returned parts.
MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications
are made by persons other than its own authorized service personnel unless such work is authorized in writing by
MICROMERITICS.
The obligations of this warranty will be limited under the following conditions:
1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their
respective brand names or trade names. We, therefore, make no express or implied warranty as to such prod-
ucts. We shall use our best efforts to obtain from the manufacturer, in accordance with his customary prac-
tice, the repair or replacement of such of his products that may prove defective in workmanship or materials.
Service charges made by such manufacturer are the responsibility of the ultimate purchaser. This states our
entire liability in respect to such products, except as an authorized person of MICROMERITICS may other-
wise agree to in writing.
2. If an instrument or product is found defective during the warranty period, replacement parts may, at the dis-
cretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check
valves, seals, etc.
3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and
stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects.
Such items which perform satisfactorily during the first 45 days after the date of shipment are assumed to be
free of manufacturing defects.
Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manu-
factures a special product to the purchaser’s specifications.
MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of
its products other than the liability stated above. This warranty is in lieu of all other warranties, express or
implied, including, but not limited to, the implied warranties of merchantability or fitness for use.
4356 Communications Drive Norcross, GA 30093-1877 Fax [phone]
Domestic Sales - [phone] Domestic Repair Service - [phone]
International Sales - [phone] Customer Service - [phone]

VacPrep 061 Table of Contents
Feb 2013 i
TABLE OF CONTENTS
1. INSTALLATION
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-2
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-3
Unpacking and Inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4
Equipment Damage or Loss During Shipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4
Equipment Return . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Selecting the Input Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-5
Rear Panel Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8
Attaching Flexible Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-11
Attaching Vacuum Fittings for Vacuum Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-11
Attaching Gas Delivery Tubes for Flowing Gas Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-12
Calibrating the Vacuum Gauge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-13
Creating a Sorption Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-14
2. OPERATION AND SAMPLE PREPARATION
Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
Front Panel Features. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Rear Panel Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Controlling the Temperature of Heating Stations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-3
Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4
Cleaning Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4
Weighing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-6
Inserting and Removing Heating Station Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-8
TriStar and ASAP Series Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-11
Inserting Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Removing Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Gemini Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-13
Inserting Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
Removing Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
Degassing Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-14
Vacuum Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
Alternating Vacuum-Backfill Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-19
Flowing Gas Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-21
3. TROUBLESHOOTING AND MAINTENANCE
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1
Temperature Controller Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-4
Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-5
Checking Gas Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-5
Cleaning and Replacing Gas Delivery Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-6

Table of Contents VacPrep 061
ii Feb 2013
Replacing Flexible Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Cleaning and Replacing Vacuum Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
Connecting or Replacing Valve Inlet Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Calibrating the Vacuum Gauge. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
4. ORDERING INFORMATION
INDEX

VacPrep 061 Description
Feb 2013 1-1
1. INSTALLATION
Description
The VacPrep 061 Degasser prepares samples for adsorption analysis. Moisture and other con-
taminants are removed by heating the sample while using any of the following methods:
• applying a vacuum to the sample
• passing a flowing gas over the sample
• using an alternating combination of vacuum and flowing gas techniques
The degasser has six heating stations for degassing samples and six cooling stations. The
desired degassing temperature is easily set and checked at the temperature controller located
on the front of the instrument. Control valves are readily accessible and provide a constant
indication of the valve state. A built-in vacuum gauge provides a constant indication of the
system vacuum.
Figure 1-1. VacPrep 061 Degasser

Conventions VacPrep 061
1-2 Feb 2013
Conventions
This manual uses the symbols shown below to identify notes of importance, warnings, and
cautions.
Notes contain important information pertinent to the subject matter.
Warnings contain information that help you prevent actions that may cause personal
injury.
Cautions contain information that help you prevent actions that may damage the
analyzer.

VacPrep 061 Specifications
Feb 2013 1-3
Specifications
The following table gives the specifications of the VacPrep 061 Degasser.
Table 1-1. Specifications
Characteristic Specification
Sample Tubes Up to 3.0-cm (1 3/16-in.) OD bulbs with 1/4-,
3/8-, or 1/2-in., 9mm, 12mm OD stems.
Heating Block
Temperature:
Temperature Accuracy:
10 ºC above ambient to 400 ºC
10 ºC
Electrical
Voltage:
Power:
Frequency:
100, 120, 220, 240 VAC 10%
250 VA maximum
50/60 Hz
Environment
Temperature:
Humidity:
10 to 35 ºC operating;
0 to 50 ºC non-operating
Up to 90% relative, non-condensing
Gases Used Helium, nitrogen, argon, or any other pure gas that does
not adsorb at room temperature.
Flow Rate
(flowing gas preparation)
Up to 50 cm3/min.
Vacuum System A vacuum source achieving better than 20 mHg at the
instrument inlet, and having a device to reduce oil vapor
backstreaming is recommended.
The vacuum system must also have an anti-suckback
valve to prevent oil from flowing into the VacPrep
should there be a power failure.
Sample Capacity Six ports, each with a heating and a cooling station
Physical
Height:
Width:
Depth:
Weight:
43 cm (16.95 in.)
36 cm (14.3 in.)
30 cm (11.87 in.)
10 kg (22 lbs)

Unpacking and Inspection VacPrep 061
1-4 Feb 2013
Unpacking and Inspection
When you receive the shipping cartons, carefully compare the Packing List with the equip-
ment actually received and check the equipment for any damage during shipment. Be sure to
sift through all packing material before declaring equipment missing.
Equipment Damage or Loss During Shipment
If equipment is damaged or lost in transit, you are required to make note of the damage or loss
on the freight bill. The freight carrier, not Micromeritics, is responsible for all damage or loss
occurring during shipment. If you discover damage or loss of equipment during shipment,
report the condition to the carrier immediately.
Equipment Return
Micromeritics strives to ensure that all items arrive safely and in working order. Occasionally,
due to circumstances beyond our control, a customer may receive equipment which is not in
working order. When equipment has been damaged (either during shipment or in use) and you
wish to return the equipment to Micromeritics for repair or replacement, please follow the
steps below:
1. Tag or otherwise identify the defective equipment, noting the defect and, if possible, the
circumstances under which the defect occurred.
2. Make reference to the sales order or purchase order for the equipment, and provide the
date the equipment was received.
3. Notify a Micromeritics Service Representative of the defect and request shipping
instructions. The Service Department will assign a Return Authorization (RA) number to
your return and provide shipping information.
If you need to declare equipment as damaged or lost, save the shipping cartons. The
claims investigator must examine the cartons in order to complete the inspection
report.
When the VacPrep leaves the factory, stabilizing tubes are placed in heating stations 1
and 6 to prevent the heater block from shifting during shipment. Be sure to remove
these tubes before turning on the VacPrep.

VacPrep 061 Selecting the Input Power
Feb 2013 1-5
Selecting the Input Power
All instruments leave the factory set for 120 VAC and with the line fuse removed. The correct
setting of the universal power entrance must be checked and the appropriate fuse installed
before the degasser can be operated. The degasser is designed to operate with 100, 120, 220, or
240 VAC at 50 or 60 Hz. Voltage selection and fusing are made at the power connector, which
is located on the rear panel of the unit.
1. Make sure the power cord is disconnected from the degasser.
2. Using a pointed object, remove the fuse block and cover assembly from the power
connector at the rear of the degasser.
3. Pull the voltage selector card straight out of the power connector housing.
The power cord should be disconnected from the degasser before removing the cover
from the input power connector. Failure to disconnect the power cord could result in
electrical shock.
Pointed Object

Selecting the Input Power VacPrep 061
1-6 Feb 2013
4. Orient the voltage selector card so that the desired voltage is indicated at the bottom.
Orient the indicator pin so that it points upward as shown in the following illustration.
5. Insert the voltage selector card into the power connector housing with the edge containing
the desired voltage first and with the printed side facing the POWER ON/OFF switch.
6. Fuse the power line according to local safety practices.
Indicator Pin
Voltage
Fuse
Fuse
Fuses
Cover
Cover
Cover
Fuse Block Fuse Block
Retaining Screw
Fuse Block
The power cord must be disconnected from the degasser when installing or replacing
fuses. Failure to do so could result in electrical shock.

VacPrep 061 Selecting the Input Power
Feb 2013 1-7
a. Observe the position of the fuse block (shown on previous page) for reference. If the
single-fuse arrangement is desired, the fuse block should be positioned such that the
side with the single fuse slot and the jumper bar is away from the cover.
If the double-fuse arrangement is desired, the fuse block should be positioned such that
the side with the double fuse slots is away from the cover.
b. If the fuse block is positioned properly for the fusing desired, proceed to Step c.
If the fuse block is not positioned properly for the fusing desired:
1) Remove the fuse block retaining screw.
2) Lift the fuse block from the cover.
3) Rotate the fuse block.
4) Mount the fuse block to the cover.
5) Replace the retaining screw.
c. Insert appropriate fuse(s) for the input power source. Refer to the chart below for the
appropriate fuse rating.
7. Insert fuse block and cover assembly into input power connector and snap it into place.
Once the fuse block and cover assembly are in place, the position of the indicator pin
shows the input power selected.
The fuses used in the degasser must be identical in type and rating to that specified.
Use of other fuses could result in electrical shock and/or damage to the analyzer.
Power Source Fuse
100-120 VAC 2.5 Amp, slow-blow
220-240 VAC 1.25 Amp, slow blow (Type T, Time lag)

Rear Panel Connections VacPrep 061
1-8 Feb 2013
Rear Panel Connections
1. Insert one end of the power cord into the input power connector at the rear of the degasser
and the other end into the appropriate power source.
2. Attach an appropriate regulator to the gas bottle. Leave the gas bottle shut-off valve closed
until instructed otherwise.
3. If the regulator has a -in. outlet, proceed to Step 4. If the regulator has a -in. outlet, attach
the reducer fitting to the outlet of the regulator shut-off valve.
4. Tighten the regulator shut-off valve nut.
5. Attach the copper tubing to the brass reducer fitting.
When the VacPrep leaves the factory, stabilizing tubes are placed in heating stations 1
and 6 to prevent the heater block from shifting during shipment. Be sure to remove
these tubes before turning on the VacPrep.
Bottle Shut-Off Valve
Reducer Fitting
Two-Stage Pressure
Reducing Regulator
Gas Bottle
Brass Reducer
Fitting
Copper Tubing
Regulator
Shut-Off Valve
Pressure
Control Knob
Do not overtighten the fittings. Doing so can collapse the brass ferrule and cause a
leak.

VacPrep 061 Rear Panel Connections
Feb 2013 1-9
6. Attach the other end of the copper tubing to the fitting on the back of the degasser.
7. Open the gas bottle shut-off valve.
8. Use the regulator pressure control knob to adjust the pressure. The following table shows
pressures and their resulting flow rates (tested with helium and nitrogen). If you do not
know the flow rate you want to use, start with about 10 cm3/min for flowing gas
preparation or for backfilling samples after vacuum preparation. Experience with your
samples will help you determine whether a change is required.
Table 1-2. Gas Flow Rate
A flow rate of 10-15 cm3/min is the maximum flow rate that would generally be used in
normal operation.
9. Close the gas bottle shut-off valve. Check the pressure. If it decreases, gas is probably
leaking at the fitting. Tighten the fitting. Then check the pressure again.
Flow Gauge Pressure
cm3/min psi kPa
10 3 21
15 5 35
Copper Tubing
Vacuum Port
Gas Fitting
Backfilling the sample tube increases its pressure to a level greater than atmospheric
pressure. If the gas pressure is greater than the recommended maximum of 5 psig (35
kPag), the sample tube could be ejected from the fitting or broken.

Rear Panel Connections VacPrep 061
1-10 Feb 2013
10. Open the regulator shut-off valve. The pressure should stabilize after about five minutes.
If it does not, gas is probably leaking at the brass reducer fitting or at the gas port on the
rear panel of the degasser. Tighten the fittings. Then check the pressure again.
11. Open the gas bottle shut-off valve.
12. Attach an adequate length of vacuum pump tubing (that will fit over the 1/2-in. degasser
connector) to a vacuum pump and to the port labeled on the back of the degasser. Use
hose clamps to keep the hose in place. (An appropriate vacuum pump is available from
Micromeritics. Refer to Ordering Information in Chapter 4. The vacuum pump system
offered by Micromeritics includes hose clamps and tubing. Cut the tubing to the length
needed. Follow the installation instructions provided with the pump.)

VacPrep 061 Attaching Flexible Tubing
Feb 2013 1-11
Attaching Flexible Tubing
Six pieces of flexible tubing are included in the accessories kit. Attach one piece of tubing to
the barbed vacuum/gas fitting at each degas station on the front panel.
Attaching Vacuum Fittings for Vacuum Preparation
Six vacuum fittings, with knurled retaining nuts, ferrules, and O-rings, are included in the
accessories kit. Attach a fitting to the flexible tubing at any degas station that will be used for
vacuum or vacuum-backfill sample preparation. Press the flexible tubing completely over the
barbed nipple on the end of the fitting. Loosely attach the knurled retaining nut, ferrule, and O-
ring.
If your sample fluidizes easily and you are using a Flow Control Valve, install it at this
time using the instructions provided with the valve.
1/2-in. or 12mm
O-ring and ferrule
(for 1/2-in. or
12 mm sample
tubes)
3/8-in. or 9mm
O-ring and ferrule
(for 3/8-in. or 9mm
sample tubes)
Fitting
Nut

Attaching Gas Delivery Tubes for Flowing Gas Preparation VacPrep 061
1-12 Feb 2013
Attaching Gas Delivery Tubes for Flowing Gas Preparation
Six stainless steel gas delivery tubes are included in the accessories kit. Attach a gas delivery
tube to the flexible tubing at any degas station that will be used for flowing gas preparation.
Attach the tube by pressing the flexible tubing completely over the ferrule at the end of the gas
delivery tube.

VacPrep 061 Calibrating the Vacuum Gauge
Feb 2013 1-13
Calibrating the Vacuum Gauge
The vacuum gauge on the VacPrep 061 was calibrated and tested at the factory using a 115 V,
60 Hz electrical supply. When powered by other voltages and frequencies, the gauge must be
recalibrated. The calibration procedures are briefly described below and on the following
page. For additional information about vacuum gauge calibration and theory of operation,
refer to the manufacturer’s instruction manual, which is shipped with the VacPrep 061.
1. Place the degasser power switch in the ON (|) position.
2. Turn all VACUUM/GAS control knobs to the OFF (O) position.
3. Place the power switch for the attached vacuum pump in the ON position and allow the
pump to run for at least two hours.
4. Insert the small, flat-blade screwdriver (included in the VacPrep 061 accessories kit)
through the opening on the back of the degasser and into the slot on the adjustment screw.
5. Turn the adjustment screw to obtain a reading on the vacuum gauge that matches the
pressure level achieved by the vacuum pump.
To confirm the accuracy of the vacuum pump gauge, attach an independent gauge to
the end of your vacuum pump hose. Most good quality vacuum pumps can achieve a
vacuum of less than 10 millitorr (10 mHg). A better vacuum may be obtained for
calibration purposes by using a sorption pump, described in the next section.
Slotted Adjustment
Screw

Creating a Sorption Pump VacPrep 061
1-14 Feb 2013
Creating a Sorption Pump
You can improve the vacuum in the VacPrep 061 by creating a sorption pump using a sample
tube and a microporous material with a high surface area. The following steps describe how to
create a sorption pump.
1. Partially fill a sample tube with material of a high surface area, such as aquarium charcoal,
other forms of activated carbon, or zeolite. Avoid using fine powders.
2. Attach the sample tube to one of the degas stations.
3. Set the temperature controller to approximately 150 ºC.
4. Turn the appropriate VACUUM/GAS control knob to VAC and allow the sample tube to
be evacuated for approximately one hour or until the vacuum gauge reading falls below 50
millitorr (50 mHg).
5. Leave the VACUUM/GAS control knob in the VAC position and move the sample tube to
a cooling station.
6. After the sample tube has cooled sufficiently, immerse the lower two-thirds of the tube
into a liquid nitrogen bath.
7. The resulting sorption pump will reduce the pressure in the VacPrep to less than 1 millitorr
(1 mHg).
8. The vacuum gauge may be recalibrated with the sorption pump attached.
9. Turn the VACUUM/GAS control knob to GAS for about 30 seconds, then to OFF before
removing the sorption pump from the fitting.
For sample tubes having a capacity greater than 6 cm3, and for tubes containing high
surface area materials, a longer backfill time will be required.
Backfilling the sample tube increases its pressure to a level greater than atmospheric
pressure. If the gas pressure is greater than the recommended maximum of 5 psig (35
kPag), the sample tube could be ejected from the fitting or broken.