Millipore Labscale User Manual

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Labscale

™

Tangential

Flow Filtration System

User Guide

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Notice

The information in this document is subject to change without notice and should not be construed as a commitment by Millipore Corporation. Millipore Corporation assumes no responsibility for any errors that may appear in this document. This manual is believed to be complete and accurate at the time of publication. In no event shall Millipore Corporation be liable for incidental or consequential damages in connection with or arising from the use of this manual.

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Labscale Tangential Flow Filtration System User Guide 3

Contents

Introduction 5

Operator and Equipment Safety 5 Labscale Stirbase Setup 6 Module set up 6 Operating Requirements 7

System Overview/Unpacking Lists 8

Labscale TFF System 8 Labscale 500 mL Reservoir 9 Labscale Stir Base 11 Labscale Pump Module 12 Pellicon XL 50 Device 13 User Supplied Materials 13

Labscale TFF System Setup 14

Labscale 500 mL Reservoir Setup 16 Labscale Stir Base Set Up 19 Labscale Pump Module Set Up 21

Install Cleaning Tubing 25

Install Cleaning Tubing 25 Clean System 26 Drain System 27 Flush System 29

Flushing Device 30

Install Pellicon XL Device 30 Flushing 31 Drain System 33 Integrity Testing—Pellicon XL Device on System 33 Preconditioning 34 Concentration 35 Product Recovery 37

Dialtration—Vacuum 38

Shutdown 40

Cleaning Device 40 Clean System 40 Drain System 42 Flushing Device 42 Clean Base 42

Specications 43

Materials of Construction 43

ECComplianceCerticate 44

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Labscale TFF SystemOrdering Information 45

Labscale TFF system kit 45 Compatible pumps and pump head 46 Pellicon XL Devices 46

Labscale TFF System Maintenance 47

Labscale Stir Base Spare Parts 47 Labscale 500 mL Reservoir Spare Parts 47 Labscale Pump Module Spare Parts 49

PumpCheckValveFlushing 50

Diaphragm Pump Maintenance 51 Electrical Schematic 53

Labscale TFF SystemTroubleshooting 54

Electrical/Control 54 Performance 55 Pressure 56 Technical Assistance 58

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Labscale Tangential Flow Filtration System User Guide 5

Introduction

The Labscale TFF system is a simple, easy to use system, designed specifically for the Pellicon® XL device. This modular system includes a 500 mL acrylic reservoir with pressure gauges, device docking manifold and retentate valve; system base with integral magnetic stirrer and diaphragm pump. The design of this system allows Millipore’s Pellicon XL device to dock directly onto the side of the reservoir, making tubing connections short, minimizing holdup and recirculation volumes.

Operator and Equipment Safety

Anyone operating or working near the Labscale system must be aware of the following:

• Read and understand this Operators Manual before performing maintenance on the system. Failure to follow instructions could result in user injury or system damage.

• Read and understand all maintenance instructions in this operating instruction manual before performing maintenance on the system. Failure to follow instructions could result in user injury or system damage.

• Prior to operation, ensure the Labscale system is fully assembled as described in Labscale TFF System Setup. Ensure all pumps and sensors are properly conected to their connection ports on the system.

• Never operate the Labscale system in a hazardous environment or use with flammable, combustible or solvent liquids.

• Any alteration of the Labscale system from factory specification may cause unsafe conditions and will void the product warranty.

• Use appropriate power supply cable and fuses for the area where the Labscale system is operated for information, see Labscale Stirbase Setup.

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Labscale Stirbase Setup

• If you order the pump module separatly, ensure pump module wiring connections are correctly installed, see Chapter “Labscale Pump Module set up”.

Module set up

Risk of electric shocks

• Unplug power cord prior to opening the blank panel from system base.

• There are no user-serviceable parts inside the Labscale system.

• Service should be performed only by trained and authorized

personnel.

Risk of rupture

• Use caution when opening and closing valves. Failure to open or close valves at the appropriate times could result in trapped high pressure, product loss, damaged cassettes, chemical spills, and pump damage. Carefully follow all operating instructions

• Prior to each use, carefully inspect all hoses and tubing for kinks or restrictions that could result in pressure buildup and possible rupture of hoses or tubing.

• Prior to each use, carefully check that tubing at pump outlet to feed in port (FEED IN) and cleaning tubing are Sta-Pure (white) tubing. Failure in correctly installing Sta-Pure (white) tubing can result in overpressurized tubing and burst.

• Transfer pump tubing can rupture due to continuous contact with moving parts. Follow tubing manufacturer’s recommended replacement interval.

• Never move the system while there is liquid in the tank, while system processes are running or the cassettes is in place.

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Labscale Tangential Flow Filtration System User Guide 7

• Never operate the system without the tank cover in place. Never

operate the system if any moving parts are exposed. Never operate the system with the pump housing open.

• Use appropriate personal protective equipment, including eye

protection, when operating the system.

This equipment can potentially be used with biohazardous products.

Operating Requirements

The system needs to be connected to electrical power and have fuses installed to operate.

The Labscale system must only be uesd with the Millipore wall transfomer provided and Millipore accessories.

Location Power Supply Reference

North America

Japan

115 VAC 50/60Hz, 1-phase XX42LSS11

Europe,

China

230 VAC 50/60Hz, 1-phase XX42LSS12

United Kingdom 230 VAC 50/60Hz, 1-phase XX42LSS13

Operating Conditions

The maximum operating altitude 2000 m

The over voltage category 2

The temperature operating range 40 to 25 °C (39 to 77 °F)

in a non-condensing

environment

Storage Conditions

The temperature storage range -10 C to 55 °C (14 to 131

°F) in a non-condensing

environment

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System Overview/Unpacking Lists

Labscale TFF System

The Labscale TFF System is shipped in an overpack carton that contains three separate cartons. One carton contains the Labscale 500 mL Reservoir, one contains the Labscale Stir Base with the Labscale pump module installed, one contains the AC Adapter.

Figure 1: The Labscale TFF System, Catalog No. XX42LSS11(115V), XX42LSS12(230V), XXL425513(230V GB).

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Labscale Tangential Flow Filtration System User Guide 9

Labscale 500 mL Reservoir

The reservoir manifold and instruments are an integrated system. The feed pressure gauge indicates the pressure of the fluid being pumped into the Pellicon XL device. The retentate pressure gauge indicates the pressure of the fluid exiting the Pellicon XL device. The upper manifold includes a retentate back pressure valve. The fittings used are polypropylene and stainless steel.

Retentate Pressure Gauge

Retentate Back Pressure Valve

Feed Pressure Gauge

Figure 2: Labscale 500 mL Reservoir, Catalog No. XX42RES01

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The following items are also packed with your Labscale 500 mL Reservoir:

1 Shut-o Valve

10 Fittings

10 Clamps

1 Syringe

1 Stir Bar

1 Millex

Vent

1 Operating Manual

3 Rotating Lock Rings

6 feet (1.8 m) of Silicone

(translucent) tubing

1/8 in. (3 mm) ID

2 x 1 ft (0.3m) of Sta-Pure® peristaltic pump tubing 1/8 in. (3 mm) ID.

Figure 3: Labscale 500 mL Reservoir Accessories

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Labscale Tangential Flow Filtration System User Guide 11

Labscale Stir Base

A magnetic stirrer is installed inside the base housing. A stir bar is packed with the Labscale Stir Base unit. The speed control knob for the stirrer is located on the front of the stir base.

1 Stir Bar

2 Thumbscrews

1 Operating Manual

1 Stir Bar

2 Thumbscrews

1 Operating

Manual

Figure 4: Labscale Stir Base Assembly No. 29755

1 Stir Bar

120 V

230V GB

230V

2 Thumbscrews

1 Operating Manual

Figure 4b:Labscale Stir Base Accessories

Figure 4c:AC Adapter Assembly No. 29209, (120V), 29781 (230V), 29913 (230V GB)

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Labscale Pump Module

The Labscale Pump Module consists of a panel mounted electronic diaphragm pump and a panel mounted speed controller that can be installed in the Labscale Stir Base. The Labscale Pump Module is mounted inside the base if a complete system was purchased. If the pump unit was purchased separately, it is packed as shown in figure 5.

Note: This Labscale Pump Module can only be used with the

Millipore Labscale Stir Base.

Figure 5: Labscale Pump Module Catalog No. XX42PMP01

4 clamps 4 ttings

1 Installation Instructions

3 feet of Silicone (translucent) tubing 1/8" (3mm) ID

1 x 1 ft (0.3m) of Sta-Pure® peristaltic pump tubing 1/8 in. (3 mm) ID.

Figure 6: Labscale Pump Module Accessories

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Labscale Tangential Flow Filtration System User Guide 13

Pellicon XL 50 Device

The Pellicon XL device is not included with the Labscale TFF System. It must be purchased separately. The Pellicon XL device includes an Accessories Kit that is packed in the Pellicon XL box below the device. The parts in the accessory kit are not required for this system installation.

User Supplied Materials

You will need to supply the following items for system setup: suitable containers for retentate, permeate and waste collection, scissors, a Pellicon XL Device.

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Labscale TFF System Setup

See “Labscale 500mL Reservoir Setup” section for detailed setup instructions.

COVER

MILLEX VENT FILTER

VENT PORT

FEED PRESSURE GAUGE

RETENTATE PRESSURE GAUGE

RESERVOIR SHUT-OFF VALVE

TANK OUT PORT

FEED IN PORT

RET OUT PORT

PERM 2 OUT

PERM 1 OUT

RET IN PORT

RETENTATE TUBING

PERMEATE TUBIN

RETENTATE BACK PRESSURE VALVE

DIA RECIRC

Figure 7: Labscale 500 mL Reservoir set up.

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Labscale Tangential Flow Filtration System User Guide 15

COVER

MILLEX VENT FILTER

VENT PORT

FEED PRESSURE GAUGE

RETENTATE PRESSURE GAUGE

RESERVOIR SHUT-OFF VALVE

TANK OUT PORT

FEED IN PORT

RET OUT PORT

PERM 2 OUT

PERM 1 OUT

RET IN PORT

RETENTATE TUBING

PERMEATE TUBIN

RETENTATE BACK PRESSURE VALVE

DIA RECIRC

Figure 8: Labscale 500 mL Reservoir set up with Labscale TFF System.

FEED PRESSURE GAUGE

RETENTATE PRESSURE GAUGE

RET OUT PORT

PERM 2 OUT

PERM 1 OUT

RET IN PORT

RETENTATE TUBING

PERMEATE TUBIN

DIA RECIRC

Figure 9: Labscale 500 mL Reservoir set up with user supplied peristaltic pump.

Install the Sta-Pure (white) tubing on the pump outlet and feed in port of the reservoir.

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Labscale 500 mL Reservoir Setup

Note: All tubing lengths are recommended to minimize

recirculation volume. Longer lengths may be used.

After prolonged storage, the tubing may absorb a small volume of water. As a result, the tubing color may change from translucent to opaque, which is normal. Air or oven drying will return the color to translucent.

Install Retentate Tubing

1. Cut silicone (translucent) tubing and install fittings as shown in figure 10.

L = 15 cm (6 inches)

Fittings: 1 male, 1 female

MALE

FEMALE

Figure 10: Set-up of retentate tubing, ttings and clamps.

2. Remove plugs from retentate outlet (RET OUT) and retentate inlet (RET IN) ports.

3. Insert the male luer end of the retentate tubing into the RET OUT port and the female luer end of the retentate tubing into the RET IN port. Turn fittings until snug.

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Labscale Tangential Flow Filtration System User Guide 17

L = 15 cm (6 inches)

Fittings: 1 male, 1 female

MALE

FEMALE

RET OUT PORT

RET IN PORT

RETENTATE TUBING

Figure 11: Install retentate tubing.

Install Permeate Tubing

1. Cut silicone (translucent) tubing and install fittings as shown in figure 12.

L = 15 cm (6 inches)

Fittings: 1 male, 1 female

MALE

FEMALE

L = Appropriate length to reach collection vessel. Fittings: 2 male

MALE

RET OUT PORT

RET IN PORT

RETENTATE TUBING

Figure 12: Set-up of permeate tubing, ttings and clamps.

2. Remove the plug from the permeate outlet port (PERM 2) and insert the male luer end of the permeate silicone (translucent) tubing into the PERM 2 port. Turn fitting until snug.

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PERM 2 OUT

PERMEATE TUBIN G

Figure 13: Install permeate tubing.

InstallTankOutletValve

Remove plug from the tank outlet port (TANK OUT) and insert the female luer end of the tank outlet valve over the TANK OUT port. Turn the lock nut until snug.

TANK OUTLET VALVE

TANK OUT PORT

PERM 2 OUT

PERMEATE TUBIN

Figure 14: Install tank outlet valve.

InstallVentFilter

If a sterile vent is required, remove plug from the vent (VENT) port and insert male luer end of MILLEX filter into the VENT port.

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Labscale Tangential Flow Filtration System User Guide 19

Install Stir Bar

If mixing is required, open reservoir cover and drop stir bar to the bottom of the reservoir.

MILLEX VENT FILTER

VENT PORT

PERM 2 OUT

PERMEATE TUBIN

Figure 15: Install Millex vent.

Labscale Stir Base Set Up

Power Connection

1. Turn stirrer and pump (if equipped) speed controls to the off position.

2. Connect power cord to power cord receptacle located at the rear of the system base.

3. Align detent on connector with receptacle.

4. Press connector into receptacle and turn lock ring to secure.

5. Inspect transformer label, checking for proper voltage. The wall transformer serves as a means of cutting the power to the system.

Note: The system should not be located in a place that may

allow liquid to be splashed under the enclosure.

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Figure 16: ower Connection

Check Operation

1. Remove the plugs from the pump inlet and pump outlet ports.

2. Turn on the pump speed control, set to 2, and listen for pump motor.

3. Turn off the pump speed control.

4. Turn on the stirrer speed control, listen for the stirrer motor.

5. Turn off the stirrer speed control.

PUMP SPEED CONTROL KNO B

STIRRER SPEED CONTROL KNO B

PUMP INLET PO RT

PUMP OUTLET PORT

]

Figure 17: Check operation.

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Labscale Tangential Flow Filtration System User Guide 21

Labscale Pump Module Set Up

Labscale Pump Module Installation

If you ordered the Labscale Pump Module separately, you will need to install it in the Labscale Stir Base.

WARNING: Disconnect power connection before proceeding.

1. Remove the blank panels from the system base as shown in figure 18.

2. Install gasket and make wiring connections as shown in figure 19.

3. Secure the pump panel and pump speed control panel into the base as shown in figure 20.

Figure 18: Remove blank panels from system base.

Figure 19: Labscale Pump Module wiring connections

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Figure 20: Labscale Pump Module installation

Speed Control

Connector

WIRE

Number Color

+ FIELD not used

AC1 1 Black AC2 2 White

-FIELD not used

-ARM 6 Black

+ ARM 5 Red

Pump Control

+ 5 Red

- 6 Black

1. Cut silicone (translucent) tubing and install fittings and clamps.

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Labscale Tangential Flow Filtration System User Guide 23

L = 20 cm (8 inches) (cut 2) Fittings: 4 female (2 per length)

FEMALE

Figure 21: Set-up of pump inlet and outlet tubing, ttings and clamps.

2. Cut one of the two Sta-Pure (white) tubing and install fittings and clamps as shown in figure 21. Use only one Sta-Pure (white) tubing for pump outlet. The other Sta-Pure (white) tubing is used for cleaning.

Install Pump Inlet and Outlet Tubing

1. Insert one female luer end of the silicone (translucent) tubing over the PUMP INLET port and the other female luer end of the silicone (translucent) tubing over the Tank Outlet Valve and turn the lock nut until snug.

2. Insert one female luer end of the Sta-pure (white) tubing over the PUMP OUTLET port and insert the other female luer end of the Sta-pure (white) tubing over the Feed Inlet (FEED IN) port and turn the lock nut until snug.

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L = 20 cm (8 inches) (cut 2) Fittings: 4 female (2 per length)

FEMALE

PUMP INLET TUBING

PUMP INLET PORT

PUMP OUTLET TUBING

PUMP OUTLET PORT

FEED IN PORT

TANK OUTLET VALVE

Figure 22: Install pump inlet and outlet tubing.

INSTALLATION TIP:

To reduce pump pulsation, increase tubing length. 100mm (4 in) of additional tubing will only increase fill volume by 0.8 mL.

Note: Failure to place Sta-Pure (white) tubing at the pump

outlet may result in overpressurized tubing and bursting of tubing.

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Labscale Tangential Flow Filtration System User Guide 25

Install Cleaning Tubing

1. Cut Sta-Pure (white) tubing and install fittings and clamps as shown in figure 23.

L = 25 cm (10 inches) Fittings: 2 female

FEMALE

Figure 23: Setup of cleaning tubing, ttings and clamps.

Remove the plug from the Device Feed port (FEED) and insert one of the female luer ends of the cleaning tubing over the FEED port. Turn the lock nut until snug.

2. Remove the plug from the Device Retentate port (RET) and insert the other female luer end of the cleaning Sta-Pure (white) tubing over the (RET) port. Turn the lock nut until snug.

L = 25 cm (10 inches) Fittings: 2 female

FEMALE

CLEANING TUBE

DEVICE RETENTATE PORT

DEVICE FEED PORT

Figure 24: Install cleaning tubing.

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Note: Failure to place Sta-Pure (white) tubing at the pump

outlet can result in overpressurized tubing and bursting of tubing.

Clean System

1. Disconnect retentate silicone (translucent) tubing from RET IN port and place in waste collection vessel.

2. Open retentate valve by turning counterclockwise

L = 25 cm (10 inches) Fittings: 2 female

FEMALE

RETENTATE BACK PR ESSURE VALVE

VENT PORT

WASTE COLLECTION VESSEL

TANK OUTLET VALVE

CLEANING TUBE

DEVICE RETENTATE PORT

DEVICE FEED PORT

Figure 25: System Cleaning steps 1–6

3. Remove reservoir cover and fill reservoir with 500 mL of 0.1N Soduim Hydroxide at 45 °C.

Note: Follow solution manufacturer.s directions for proper

handling.

4. Remove plug from VENT port and open tank outlet valve.

5. Turn pump on - set pump speed to 2.

Note: Check system connections for leaks—tighten connec-

tions if required

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Labscale Tangential Flow Filtration System User Guide 27

6. Continue pumping the cleaning solution to the waste collection vessel until the level in the reservoir drops to 250 mL. Turn pump off.

7. Reconnect the retentate silicone (translucent) tubing to the RET IN port. Turn pump on and set pump speed to 2.

Note: Check system connections for leaks—tighten connec-

tions if required

8. Set pump speed to 2. Recirculate for 15–30 minutes. Turn pump off.

RETENTATE TUBING

Figure 26: Setup for system cleaning steps 7 & 8

Drain System

1. Disconnect pump outlet Sta-pure (white) tubing from pump outlet port and place in waste collection vessel.

2. Disconnect retentate silicone (translucent) tubing from RET IN port. Fluid should now drain by gravity. If additional drainage is required, a syringe can be placed on the end of the retentate tube and fluid can be blown down.

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RETENTATE TUBING

Figure 27: Setup for system draining steps 1 and 2.

3. Replace retentate silicone (translucent) tubing in retentate port. Reconnect pump outlet Sta-Pure (white) tubing.

4. Disconnect pump outlet Sta-Pure (white) tubing from FEED IN port and place in collection vessel. Open tank outlet valve, turn pump speed up to drain reservoir.

5. Reconnect the pump outlet Sta-Pure (white) tubing to the FEED IN port.

RETENTATE TUBING

PUMP OUTLET TUBING

COLLECTION VESSEL

Figure 28: Setup for system draining steps 3–5.

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Labscale Tangential Flow Filtration System User Guide 29

Flush System

Repeat instructions for System Cleaning substituting purified water in place of cleaning solution.

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Flushing Device

Install Pellicon XL Device

1. Remove plug from FEED, RET, PERM 1, and PERM 2 ports.

2. Align Pellicon XL device ports with Labscale 500 mL Reservoir ports being sure that PERM and RET DEVICE ports of device and reservoir match. Press device firmLy onto reservoir ports. Turn the lock nuts until snug.

RESERVOIR FEED PORT

RESERVOIR PERM 1 PORT

RESERVOIR PERM 2 PO RT

RESERVOIR RET PORT

DEVICE FEED PORT

DEVICE PERM 1 PO RT

PELLICON XL DEVICE

DEVICE PERM 2 PO RT

DEVICE RET PORT

Figure 29: Install Pellicon XL Device

Note: Be sure pump tubing is installed before proceeding

and Sta-Pure (white) tubing is installed between pump outlet and feed in port (FEED IN).

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Labscale Tangential Flow Filtration System User Guide 31

Flushing

1. Disconnect retentate silicone (translucent) tubing from RET IN port and place end of retentate tubing in waste collection vessel.

2. Place end of permeate silicone (translucent) tubing into waste collection vessel. Open retentate valve—turn counterclockwise

3. Remove reservoir cover and fill reservoir with 500 mL of purified water. Remove plug from VENT port and open tank outlet valve.

PERMEATE TUBING

RETENTATE TUBING

RESERVOIR FEED PORT

RESERVOIR PERM 1 PORT

RESERVOIR PERM 2 PO RT

RESERVOIR RET PORT

DEVICE FEED PORT

DEVICE PERM 1 PO RT

PELLICON XL DEVICE

DEVICE PERM 2 PO RT

DEVICE RET PORT

Figure 30: Flushing the Pellicon XL Device, steps 1–6.

4. Turn pump on - increase pump speed until feed pressure gauge reads 1.38 Bar (20 psi).

Note: Check system connections for leaks—tighten connec-

tions if required

5. Continue pumping to the waste collection vessel until level in the reservoir drops to 350 mL. Turn pump off.

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6. Reconnect the retentate silicone (translucent) tubing to the RET IN port and turn pump on - increase pump speed until feed pressure gauge reads 1.38 Bar (20 psi).

Note: Check system connections for leaks—tighten connec-

tions if required

7. Adjust retentate valve restriction by slowly turning retentate valve clockwise

until the retentate pressure gage reads

0.69 Bar (10 psi).

8. Adjust pump speed and retentate valve restriction to achieve

2.07 Bar (30 psi) feed pressure and 0.69 Bar (10 psi) retentate pressure.

RETENTATE TUBING

Figure 31: Flushing System Setup.

9. Continue flushing until the level in the reservoir drops to 50 mL. Turn pump off.

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Labscale Tangential Flow Filtration System User Guide 33

Drain System

See “Drain System” section, page 27.

Integrity Testing—Pellicon XL Device on System

Integrity Test Set Up

1. Close tank outlet valve and disconnect pump inlet tubing (silicone, translucent) from the tank outlet valve. Close the retentate valve.

Integrity Test Procedure

1. Obtain air integrity test pressure and airflow specifications from the Certificate of Quality supplied with the device.

2. Insert syringe in the female luer end of the pump inlet tubing. (silicone, translucent). Inject air into the tubing until the feed pressure gauge reading reaches the recommended air integrity test pressure.

Figure 32: Integrity Test Setup

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3. Add 0.1 mL of water to a 1 mL pipette. Insert bottom of pipette into the end of the permeate tubing (silicone, translucent).

4. Measure airflow by measuring the displacement of water in the pipette for 30 seconds. Multiply the displaced volume by 2 to calculate the airflow (mL/min) and record.

5. Remove the pipette from the permeate tubing (silicone, translucent). Open the retentate valve slowly to release the air pressure in the system.

6. Reconnect the pump inlet tubing (silicone, translucent) to the tank outlet valve.

The Pellicon XL device is integral if the measured airflow is lessthan or equal to the airflow specification on the Certificate of Quality.

Preconditioning

1. Place end of permeate tubing silicone (translucent) in waste collection vessel.

2. Remove reservoir cover and fill reservoir with 50 mL of an appropriate buffer. Remove plug from VENT port.

3. Open tank outlet valve. Turn pump on - increase pump speed until feed pressure gauge reads 1.38 Bar (20 psi).

Note: Check system connections for leaks—tighten connec-

tions if required

4. Continue pumping to the waste collection vessel until the level in the reservoir drops to the bottom of the reservoir stir bar well.(Stop pump before air is pumped into the system.). Turn pump off.

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Labscale Tangential Flow Filtration System User Guide 35

RETENTATE TUBING

Figure 33: Preconditioning Setup.

Drain Permeate Tubing

1. Disconnect the permeate tubing (silicone, translucent) from the permeate outlet (PERM 2) port. Drain permeate tubing into the waste collection vessel.

2. Reconnect the permeate tubing to the PERM 2 port.

Concentration

1. Remove reservoir cover and fill reservoir with sample to be concentrated.

2. Ensure vent port is open by removing plug from VENT port and leaving open or install a Millex Filter. Open tank outlet valve.

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3. Turn pump on—increase pump speed until feed pressure gauge reads 1.38 Bar (20 psi).

Note: Check system connections for leaks—tighten connec-

tions if required

4. Adjust retentate valve restriction by slowly turning retentate valve clockwise

until the retentate pressure gauge reads

0.69 Bar (10 psi).

5. Adjust pump speed and retentate valve restriction to achieve desired feed retentate pressures (recommend 2.07 Bar (30 psi) feed / 0.69 Bar (10 psi) retentate).

RETENTATE TUBING

Figure 34: Concentration Setup.

Note: Do not exceed 4.14 Bar (60 psi) feed pressure.

6. Continue processing until the desired concentration or volume is reached. Turn pump off.

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Labscale Tangential Flow Filtration System User Guide 37

Product Recovery

1. Disconnect pump outlet tubing (Sta-Pure, white) from pump outlet port and place in product recovery collection vessel.

2. Disconnect retentate tubing (silicone, translucent) from retentate in port. Fluid should now drain by gravity. If additional drainage is required, a syringe can be placed on the end of the retentate tube and fluid can be blown down

RETENTATE TUBING

Figure 35: Product Recovery Setup.

3. Replace retentate tubing (silicone, translucent) in retentate port. Reconnect pump outlet tubing (Sta-Pure, white).

4. Disconnect FEED IN tubing and place in collection vessel. Open tank outlet valve, turn pump speed up to drain reservoir.

5. Reconnect the pump outlet tubing (Sta-Pure, white) to the FEED IN port.

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Figure 36: Product Recovery Setup.

Diafiltration—Vacuum

InstallDialtrationTubing

1. Cut silicone (translucent) tubing and insert a male luer x 1/8. barb port in one end of the tubing as shown here. MALE Place the other end of the diafiltration tubing in a vessel of appropriate buffer.

L = 50 cm (20 inches) Fittings: 1 male

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Labscale Tangential Flow Filtration System User Guide 39

2. Connect male luer end of diafiltration tubing to the diafiltration (DIA/RECIRC) port. Plug VENT port.

3. Insure that the end of the tubing remains below the buffer level at all times.

As you remove permeate, a vacuum is created in the reservoir which will siphon diafiltrate into the reservoir to maintain constant volume.

L = 50 cm (20 inches) Fittings: 1 male

Figure 37: Dialtration

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Shutdown

Cleaning Device

Recommended Cleaning Solutions

Note: Follow solution manufacturer’s directions for proper

handling. Please refer to the Pellicon XL Device instructions packed with the device for the most current cleaning solution information.

Cleaning

Agent

Concen-

tration

CatalogNos.withprex

PXBBiomax

(polyether-sulphone)

CatalogNos.withprex

PXC PL

(regenerated cellulose)

Temp

ºC

Time (min)

NaOH 0.1-

0.5N

X 40-45 13-13.7 30-60

NaOH 0.1N X 25-40 13 30-60 NaOC1 250

ppm

X 40-45 10-11 30-60

Note: Do not exceed 2.07 Bar (30 psi) feed pressure during cleaning cycle.

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Labscale Tangential Flow Filtration System User Guide 41

Clean System

1. Disconnect retentate tubing (silicone, translucent) from RET IN port and place in waste collection vessel. Place end of permeate tubing in waste collection vessel.

2. Open retentate valve turn counterclockwise .

3. Remove reservoir cover and fill reservoir with 500 mL of cleaning solution. Ensure vent port is open by removing plug from VENT port and either leaving open or installing a Millex Filter.

4. Open tank outlet valve.

5. Turn pump on - increase pump speed until feed pressure gauge reads 1.38 Bar (20 psi).

Note: Check system connections for leaks—tighten connec-

tions if required

6. Continue pumping to the waste collection vessel until the level in the reservoir drops to 250 mL.Turn pump off.Reconnect the retentate (silicone, translucent) tubing to the RET IN port.

7. Connect the male luer end of the permeate tubing to the recirculation (DIA/RECIRC) port. Turn pump on increase pump speed until feed pressure gauge reads 1.38 Bar (20 psi).

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PERMEATE TUBING

RETENTATE TUBING

Note: Check system connections for leaks—tighten connec-

tions if required

8. Adjust retentate valve restriction by slowly turning retentate valve clockwise

until the retentate pressure gage reads

0.69 Bar (10 psi). Adjust pump speed and retentate valve restriction to achieve 2.07 Bar (30 psi) feed pressure and 0.69 Bar (10 psi) retentate pressure.

9. Recirculate the cleaning solution for 30 - 60 minutes. Turn pump off.

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Labscale Tangential Flow Filtration System User Guide 43

Drain System

See “Drain System” section, page 27.

Flushing Device

Repeat flushing procedure detailed in “Flushing” section, page 31.

See instructions enclosed with the Pellicon XL device for storage information.

Clean Base

1. Disconnect power.

2. Exterior surfaces of the Labscale 500 mL Reservoir and the Labscale System Base may be cleaned with a mild soap and water solution.

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Specications

Specifications

All wetted parts meet the requirements of USP Class VI testing and CFR 21 regulations.

Dimensions

21.6 x 27.9 cm (8.5 x 11 inches)

Height: 45.7 cm (18 inches) Weight 5.9 kg (13 lb) Maximum pump outlet pres-

sure

5.86 Bar (85 psig)

Maximum gauge pressure: do not exceed gauge scale Maximum Pellicon XL Device

operating pressure

see instructions

supplied with device Operating temperature range 4.45°CFeedowrate:10.100

mL/min at 4.14 Bar (60 psi) Minimum recirculation vol-

ume:

20 mL

Power 115V, 60 Hz or 230V, 50 Hz CE mark

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Labscale Tangential Flow Filtration System User Guide 45

Materials of Construction

500 mL reservoir acrylic Reservoir cover polypropylene Reservoir cover gasket EPDM Luerttings 316 stainless steel

and polypropylene

Tubing Platinum-cured silicone (translu-

cent) and Sta-Pure (white) tubing Diaphragm pump housing glass-lledpolypropylene Diaphragm pump dia-

phragm

PTFE coated

Diaphragm pump check valve

polypropylene and Simriz® elas-

tomer Housing/enclosure polyurethane

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EC Compliance Certificate

Certificate of Compliance

Millipore Corporation certifies that the part listed hereafter : Product name : LABSCALE

Catalogue # :

XX42LSS12

XX42LSS13

• Are manufactured (or supplied) by a Millipore facility whose Quality Management System is approved by an accredited registering body to the appropriate ISO 9001 Quality Systems Standard.

• Are manufactured in accordance with applicable Millipore Standard Procedures.

• Are tested in accordance with applicable Millipore Quality Specifications.

CE Compliance : Declaration of Conformity

We certify that this system is designed and manufactured in application of the following European Council directives :

• 73/23/CEE relating to Electrical equipment designed for used in certain voltage limits

• 89/336/CEE relating to Electromagnetic compatibility (EMC)

Standards to which conformity is declared applicable are the following : EMC emissions

• EN61000-3-2 : Harmonic currents

• EN61000-3-3 : Voltage fluctuations and flicker

• EN 55011 : Conducted disturbances on power ports

• EN 55011 : Radiated disturbances electric component

EMC Immunity

• EN 61000-4-2 : Electrostatic discharges immunity test

• EN 61000-4-3 : Radiated , radio-frequency, electromagnetic field immunity test

• EN 61000-4-4 : Electrical fast transient burst immunity test

• EN 61000-4-5 : Surge immunity test

• EN 61000-4-6 : Conducted disturbances, induced by radio-frequency fields, immunity test

• EN 6100-4-11 : Shot interruptions and voltage variations immunity test

Electrical safety

• IEC 61010-1:2001 : Safety requirements for electrical equipment for measurement, control and laboratory use - Part 1: General requirements

Guy Reymann Quality Manager

Millipore, Hardware Systems Operations Molsheim, France

Page 47

Labscale Tangential Flow Filtration System User Guide 47

Labscale TFF System Ordering Information

Labscale TFF system kit

Description Catalog Number

115V XX42LSS11 230V XX42LSS12

230V (GB) XX42LSS13

Includes: Labscale 500 mL Reservoir, Labscale Stir Base with Labscale Pump Module installed.

Labscale TFF system components are also available separately.

Description Catalog Number

Labscale 500 mL Reservoir

with gauges

XX42RES01

Labscale Stir Base

115V 230V

230V(GB)

XX42STR11 XX42STR12 XX42STR13

Labscale Pump Module

(can only be used with Millipore

Labscale Stir Base)

XX42PMP01

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Compatible pumps and pump head

Description Catalog Number

Peristaltic pump drive, 115V, variable speed, 60.600 rpm

XX8200115

Peristaltic pump drive, 230V, variable speed, 60.600 rpm

XX8200230

Pump head, 480 mL/min (3 roller) XX8000003 Labscale system 1/8 in. tubing kit XX80LFL25 After prolonged storage, the tubing may absorb a small volume

of water. As a result, the tubing color may change from translucent to opaque, which is normal. Air or oven drying will return the color to translucent.

Pellicon XL Devices

Please see instructions supplied with the Pellicon XL Device for ordering information.

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Labscale Tangential Flow Filtration System User Guide 49

Labscale TFF System Maintenance

Labscale Stir Base Spare Parts

Item

Number

Description

Qty per

Cat #

Catalog

Number

1 Fuse 10 XX42LSP40 2 Thumb Screw 10 XX42LSP41 3 Transformer – 115V 1 XX42LSP42 4 Transfromer – 230V 1 XX42LSP43 5 Transformer – 230V (Great

Britain)

1 XX42LSP44

6 Motor, Stirrer 1 XX42LSP45 7 Pump Assembly, Diaphragm 1 XX42LSP46 8 Speed Controller, Stirrer 1 XX42LSP47 9 Speed Controller, Pump 1 XX42LSP48

Labscale 500 mL Reservoir Spare Parts

Item

Number

Description

Qty per

Cat. #

Catalog Number

1 Pressure gauge 1 XX42LSP20 2 Stir Bar 5 XX42LSP21 3 Tank Outlet Valve 12 XX42LSP22 4 Valve Diapragm 1 XX42LSP23 5 Cover, Tank 1 XX42LSP24 6 O-Ring, Tank cover 5 XX42LSP25 7 Filter, Vent 50 SLFG025LS

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Item

Number

Description

Qty per

Cat. #

Catalog Number

8 Fitting, Luer-LokTM

Female x 10-32 St. St’l

10 XX42LSP26

9 Fitting, Luer-Lok Male x

10-32 St. St’l

10 XX42LSP27

10 10-1 10-2

Tubing:

Platinum-cured Sta-Pure Tubing

XX80LFL256 ft

2 ft

11 11-1 11-2 11-3 11-4 11-5

11-6

Plastic Fitting Kit:

Fitting, Female Fitting, Male Luer-Lok Plug Fitting, Luer-Lok Ring Fitting, Male Luer-Lok x 1/8 in. Barb Fitting, Female LuerLok x 1/8 in. Barb Clamp, Ratchet

XX42LSP28

10 10 10 10 10 10

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Labscale Tangential Flow Filtration System User Guide 51

Labscale Pump Module Spare Parts

Item Description

Qty per

Cat #

Catalog Number

1 Fitting, Male Luer-Lok x

10-32 St. St’l

10 XX42LSP27

2 Manifold, Pump 1 XX42LSP80

3 3-1 3-2 3-3

Pump Rebuild Kit Contains:

XX42LSP81

Diaphragm 1 Check Valve 2 Gasket, Check Valve 4

3-2

3-3

3-1

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PumpCheckValveFlushing

Note: The pump should be shut off during this procedure

1. Close the tank outlet valve

2. Disconnect the pump inlet tubing (silicone, translucent) from the tank outlet valve.

3. Disconnect the pump outlet tubing (Sta-Pure, white) from the reservoir FEED IN port and place the end in a waste collection vessel

4. Fill a syringe with warm water and inject the water through the pump and into the waste collection vessel.

5. Repeat Step 4 until approx. 100–200 mL of water flushed through the check valves

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Labscale Tangential Flow Filtration System User Guide 53

Diaphragm Pump Maintenance

Pump Panel Disassembly

1. Disconnect the AC adapter from its power source

2. Disconnect the AC adapter from the enclosure

3. Remove the Pump Panel from the enclosure

4. Disconnect the wires from the pump

CheckValveReplacement

1. Remove the (4) Pump Screws

2. Disasemble the pump from the pump manifold

3. Remove the (2) check valves and (4) gaskets from the check valve housing.

4. Install new check valves and gaskets as shown below

Diaphragm Replacement

1. Unscrew the diaphragm from the pump in a counterclockwise direction.

2. Install the new diaphragm by screwing the diaphragm in a clockwise direction until tight

Pump Reassembly

1. Seat the check valve housing onto the diaphragm

2. Seat the pump with check valve housing onto the pump manifold

3. Install the (4) pump screws and tighten

Pump Panel Installation

1. Reconnect the pump wires

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2. Reinstall the pump panel on the enclosure

C HEC K VALVE HO US ING

(1)

PUMP PA N EL

(1)

PUMP MA NIFO LD

(1)

DIAPH RAG M

(1)

C HEC K VALVE S

(2)

G AS KETS

(4)

PUMP SC REW S

(4)

IMPORTANT:

Check Valve orientation is as shown. Improper orientation of the check valves will damge the check valves and cause the pump not to function. The check valves are keyed to assist with proper orientation.

DO NOT FORCE CHECK VALVES INTO HOUSING!

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Labscale Tangential Flow Filtration System User Guide 55

Electrical Schematic

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Labscale TFF System Troubleshooting

Electrical/Control

Symptom Solution

Pump and stirrer do not operate

Check the following: AC adapter plugged into live receptacle

with appropriate voltage

AC adapter plugged into receptacle on the rear of system enclosure

Check fuse on the rear of the system enclosure

Pump operates but the stirrer does not

Haveaqualiedtechniciancheckthe

function of the stirrer speed controller and the stirrer motor.

Stirrer operates but the pump does not

Haveaqualiedtechniciancheckthe

function of the pump speed controller and the pump motor.

Page 57

Performance

Symptom Solution

MixingStirrer speed too slow

Haveaqualiedtechniciancheckthe

function of the stirrer speed controller.

FlowPumpow too low

If theuidmovesbackandforthinthe

pump inlet or pump outlet tubing, particulates may be impairing the pump check valves from closing. Ensure pump check

valvesareclean.Seecheckvalveushing

procedure in maintenance section “Pump check Valve Flushing” of this manual.

If ushingthecheckvalvesdoesnoteliminate the problem, replace pump check valves. See check valve replacement procedure in maintenance section “Diaphragm Pump Maintenance” of this manual.

Haveaqualiedtechniciancheckthe

function of the pump speed controller.

No Flow (Pump operating)

Ensure tank outlet valve is open.

Excessive pulsation Iftheuidmovesbackandforthinthe

pump inlet or pump outlet tubing, particulates may be impairing the pump check valves from closing. Ensure pump check

valvesareclean.Seecheckvalveushing

procedure in maintenance section “Pump check Valve Flushing” of this manual.

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Pressure

Symptom Solution

System pressure too low

Check the following: Pressure gauge calibration. Ensure tank outlet valve is open. Ensure pump inlet and outlet tubing are

connected correctly. Ensure Sta-Pure (white) tubing is connected from pump outlet to feed in port (FEED IN).

If theuidmovesbackandforthinthe

pump inlet or pump outlet tubing, particulates may be impairing the pump check valves from closing. Ensure pump check

valvesareclean.Seecheckvalveushing

procedure in maintenance section “Pump check Valve Flushing” of this manual

If ushingthecheckvalvesdoesnot

eliminate the problem, replace pump check valves. See check valve replacement procedure in maintenance section “Diaphragm Pump Maintenance” of this manual

System Pressure too high

Check the following: Pressure gauge calibration The retentate back-pressure valve is closed

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Labscale Tangential Flow Filtration System User Guide 59

Page 60

Technical Assistance

For more information, contact the Millipore office nearest you. In the U.S., call 1-800-MILLIPORE (1-800-645-5476). Outside the U.S., see your Millipore catalogue for the phone number of the office nearest you or go to our web site at www.millipore.com/ offices for up-to-date worldwide contact information. You can also visit the tech service page on our web site at http://www.millipore. com/techservice.

Millipore,Pellicon,BiomaxandMillexareregisteredtrademarksofMilliporeCorporation.TheMlogoand

Labscale are trademarks of Millipore Corporation. Sta-Pure is a trademark of W. L. Gore & Associates. Simriz is a trademark of Freudenberg & Company. Luer-Lok is a trademark of Becton, Dickinson and Company. ISO is a trademark of The International Organization for Standardization.