Micromeritics FlowPrep 060 User manual

FlowPrep 060
Operator’s Manual
060-42803-01
Nov 2010

© Micromeritics Instrument Corporation 2002-2010. All rights reserved. Printed in the U.S.A.

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]

FlowPrep 060 Table of Contents
May 2010 i
INDEX
1. GENERAL INFORMATION
Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-2
Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-3
2. INSTALLATION
Unpacking and Inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
Equipment Damage or Loss During Shipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
Equipment Return . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
Selecting the Input Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-2
Rear Panel Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4
Attaching the Gas Delivery Tubes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-6
3. OPERATION AND SAMPLE PREPARATION
Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1
Front Panel Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1
Rear Panel Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-2
Controlling the Temperature of Heating Stations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-3
Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-4
Cleaning Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-4
Weighing the Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-6
Inserting and Removing Heating Station Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-8
TriStar and ASAP Series Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-10
Inserting Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-10
Removing Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-11
Gemini Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-12
Inserting Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-12
Removing Adapters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-12
Degassing Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-13
4. TROUBLESHOOTING AND MAINTENANCE
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1
Temperature Controller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-3
Error Messages. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-3
Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-4
Checking Gas Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-4
Cleaning and Replacing Gas Delivery Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-5
Replacing Flexible Tubing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-6
Connecting or Replacing Valve Inlet Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-7

Table of Contents FlowPrep 060
ii May 2010
5. Ordering Information
INDEX

FlowPrep 060 Description
May 2010 1-1
1. GENERAL INFORMATION
Description
The FlowPrep 060 Degasser prepares samples for adsorption analysis. It uses flowing gas
passed over a heated sample to remove moisture and other contaminants. The degasser has six
heating stations for degassing samples and six cooling stations. The desired degassing temper-
ature is easily set on the temperature controller pad located on the front of the instrument. Gas
flow control valves are readily accessible and provide a constant indication of the valve state.
Figure 1-1. FlowPrep 060 Degasser

Conventions FlowPrep 060
1-2 May 2010
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.

FlowPrep 060 Specifications
May 2010 1-3
Specifications
The following table gives the specifications of the FlowPrep 060 Degasser.
Table 1-1. Specifications
Characteristic Specification
Sample Tubes Up to 3.0-cm (1.18-in.) OD
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 to50 ºC non-operating 45 to 80% relative, non-condensing
Gases Used Helium, nitrogen, argon, or any other pure gas that does
not adsorb at room temperature
Flow Rate Up to 50 cm3/min. No vacuum required
Sample Capacity 6 heating stations and 6 cooling stations
Physical
Height:
Width:
Depth:
Weight:
45 cm (16.93 in.)
36 cm (14.17 in.)
30 cm (11.81 in.)
8.6 kg (19 lbs)

FlowPrep 060 Unpacking and Inspection
May 2010 2-1
2. INSTALLATION
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 occurs.
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 FlowPrep 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 FlowPrep.

Selecting the Input Power FlowPrep 060
2-2 May 2010
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(s) 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. Insert the tip of a small pocket screwdriver (or pointed object) into the left side of the
power module located on the rear panel of the degasser.
3. Gently lift up until the cover lifts approximately 1/4 inch, then swing the cover to the left;
the cover is hinged and cannot be removed.
4. Remove the fuse block (you may have to use needle-nose pliers to grasp the fuse block).
5. The input power connector can be used with either a single-fuse arrangement (100-120
VAC) or a double-fuse arrangement (200-240 VAC). Insert the appropriate fuse(s) for the
input power source.
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.
The fuses used in the FlowPrep must be identical in type and rating to that specified.
Use of other fuses could result in electrical shock and/or damage to the degasser.

FlowPrep 060 Selecting the Input Power
May 2010 2-3
6. Position the fuse block so that the side containing the fuse(s) is facing the power module
and insert it into the connector. Do not close the cover.
7. Pull the voltage selector card straight out of the power connector housing.
8. 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.
9. 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.
10. Close the cover to the power entry module; ensure that the indicator pin is in the correct
position.
Power Source Fuse
100-120 VAC 2.5 Amp, slow blow (requires one)
200-240 VAC 1.25 Amp, slow-blow, Type T Time lag, (requires two)
Voltage selector card
Indicator Pin
Voltage

Rear Panel Connections FlowPrep 060
2-4 May 2010
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 1/8 in. outlet, proceed to Step 4. If the regulator has a 1/4 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 FlowPrep 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 FlowPrep.
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.

FlowPrep 060 Rear Panel Connections
May 2010 2-5
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. Experience with your
samples will help you determine whether a change is required.
Table 2-2. Gas Flow Rate
A flow rate of 50 cm3/min is the maximum flow rate that would generally be used in
normal operation. However, the degasser is capable of accepting up to 50 psi pressure. A
pressure of 50 psi (345 kPa) would produce a flow rate of approximately 250 cm3/min.
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.
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.
Flow Gauge Pressure
cm3/min psi kPa
10 4 28
20 6 41
30 8 55
40 10 69
50 13 90
Copper Tubing
Gas Fitting

Attaching the Gas Delivery Tubes FlowPrep 060
2-6 May 2010
Attaching the Gas Delivery Tubes
Six gas delivery tubes are included in the accessories kit. Attach one to each flexible tube by
pressing the flexible tube over the gas delivery tube. Make sure that the flexible tube com-
pletely covers the ferrule at the end of the gas delivery tube.
Flexible Tubing
Ferrule

FlowPrep 060 Operation
Nov 2010 3-1
3. OPERATION AND SAMPLE PREPARATION
Operation
Front Panel Controls
Temperature
Controller
Flow Control
Valves
Temperature Controller The temperature controller displays the current temperature
of the heating stations and enables you to change the
temperature set point. Refer to Controlling the
Temperature of Heating Stations, page 3-3 for
instructions.
Flow Control Valves Each heating station has a valve that controls the flow of gas
to the station. Place the valve in the up position to open the
valve and the down position to close the valve.
Open Closed

Operation FlowPrep 060
3-2 Nov 2010
Rear Panel Controls
Gas Port
On/Off Switch
On/Off Switch Place the switch in the up position ( | ) to turn on the
degasser, and in the down position (0) to turn off the
degasser.
Gas Port The gas port is used to connect the gas supply to the
degasser.

FlowPrep 060 Operation
Nov 2010 3-3
Controlling the Temperature of Heating Stations
The temperature controller, shown below, enables you to specify the temperature of the heat-
ing stations and displays the current temperature.
The controller always displays the current temperature (PV = Process Value) and the set point
(SV = Set Value).
Press to increase or to decrease the value until the desired temperature set
point is displayed. The keys may be held down to rapidly increase or decrease the setting.
Lights when power is being
applied to heating stations
Increases set
point temperature
Decreases set
point temperature
Displays current temperature
Displays set point temperature
The set point is retained when the degasser is turned off and turned back on.

Sample Preparation FlowPrep 060
3-4 Nov 2010
Sample Preparation
Cleaning Sample Tubes
Sample tubes must be clean in order to obtain accurate analysis results. Clean the tubes in an
ultrasonic cleaning unit as follows. The materials required for cleaning and weighing samples
are:
• Ultrasonic cleaning unit
• Alconox or other suitable detergent
• Rubber gloves or lint-free cloth
• Isopropyl alcohol (IPA) (or deionized water if IPA is unavailable)
• Nitrogen or helium
• Fume hood
• Balance for weighing sample
• Weighing support
• Sample tube brush
• Sample tube
• Sample tube stopper
• Funnel
1. Check the bowl of the ultrasonic unit to make sure it is clean.
2. Using a ratio of 5 grams of Alconox (or equivalent detergent) per 500 mL of warm water,
fill the bowl of the ultrasonic unit with enough water to cover the entire sample tube.
3. Ensure that the detergent is dissolved before placing the sample tube into the water. If too
much detergent is used, it may be difficult to rinse from the tube.
4. Fill the sample tube with warm water and place it in the bowl of the ultrasonic cleaning
unit. Turn on the unit and clean the sample tube for approximately 15 minutes.