and spring column manual - duratec

MODcol Corporation 155 East Main Avenue Suite 150 Morgan Hill, CA 95037 U.S.A.

Phone: (408) 782-5844 FAX: (408) 782-2336 Toll Free: (888) 349-9660

Series 2002 MultiPackerSeries 2002 MultiPacker and and Spring ColumnSpring Column Manual Manual

REVISION 2.0

Administrator

NOTICE

The information in this document is subject to change without notice and should not be construed as a commitment by MODcol Corporation. MODcol 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 MODcol Corporation be liable for incidental or consequential damages in connection with or arising from the use of this manual. MODcol, MultiPacker, and Spring Column are trademarks of MODcol Corporation. The MultiPacker and Spring Column are patented MODcol products.

Table of Contents

GETTING TO KNOW YOUR SERIES 2002 MULTIPACKER INSTRUMENT AND SPRING COLUMNS................................................................................................................ 1

SERIES 2002 MULTIPACKER

INSTRUMENTS ......................................................................................... 2 SERIES 2002 SPRING COLUMNS

........................................................................................................... 5

SPRING AXIAL COMPRESSION OVERVIEW ................................................................................. 7 OVERVIEW OF AXIAL COMPRESSION ...................................................................................................... 7 SPRING AXIAL COMPRESSION OPERATION THEORY ............................................................................... 8

USING YOUR SPRING COLUMN..................................................................................................... 11 INTRODUCTION................................................................................................................................... 11 IMPORTANT SLURRY PACKING HINTS .................................................................................................. 11 PREPARING THE SPRING COLUMN FOR PACKING .................................................................................. 16 PACKING THE SPRING COLUMN ........................................................................................................... 18 UNPACKING A SPRING COLUMN .......................................................................................................... 20 CLEANING THE UNPACKED SPRING COLUMN PARTS ............................................................................ 21

HOW TO REPLACE SEALS AND FRITS......................................................................................... 22 SEAL REPLACEMENT .......................................................................................................................... 22 FRIT REPLACEMENT ........................................................................................................................... 22

SPRING COLUMN CHROMATOGRAMS AND PACKING METHODS ....................................... 26 C18 BONDED PHASE ........................................................................................................................... 27 C8 BONDED PHASES............................................................................................................................ 30 C4 BONDED PHASES............................................................................................................................ 32 CHIRALCEL OD BONDED PHASE .......................................................................................................... 34

MULTIPACKER INSTALLATION ................................................................................................... 35 INITIAL SET-UP OF THE MULTIPACKER INSTRUMENT ........................................................................... 35 BLEEDING TRAPPED AIR FROM THE DAMPING MECHANISM ................................................................. 38

LIST OF PARTS AND ACCESSORIES ............................................................................................. 39

WARRANTY INFORMATION .......................................................................................................... 43

Getting to Know Your Series 2002 MultiPacker Instrument and Spring Columns

The MultiPacker is a column packing instrument from MODcol designed to pack MODcol spring column housings. Its ease of operation, low cycle time, economical nature and safety features deliver a versatile preparative column packing solution. The Spring Column offers convenience and flexibility when used with the MultiPacker Instrument. The ability to continuously vary bed length and the advantages of its spring-driven axial compression mechanism provide a high performance, adaptive solution for both the product development and the demanding process chromatography arenas. Furthermore, compared to traditional column packing processes, the MODcol Spring Column requires up to 20% less media per packing. The bed is formed from the entire quantity of media that is introduced into the column and no wastage of media occurs. More columns can be packed from the same batch of media, reducing lot-to-lot variation worries. Also, by reducing media requirements, the cost of the MultiPacker may be recouped in as little as a few months time. Unlike other axial compression systems, the MODcol Spring Column is self-contained. Once packed, the Spring Column is independent of the MultiPacker Instrument. Subsequently, one MultiPacker can be used to maintain an entire fleet of Spring Columns For the first time, the chromatographer has the ability to pack columns “on demand” in order to quickly respond to in-house column needs.

Series 2002 MultiPacker Instruments

The Series MultiPacker Instruments include the model IM2002-025IM1 for packing 25mm ID Series 2002 Spring Columns and the IM2002-050IM1 for packing 50mm ID Series 2002 Spring Columns. These instruments are similar in design, construction and appearance but are not interchangeable. A full view of the MultiPacker Instruments is shown in Figure 1. The control deck, identical for both instruments, is shown in Figure 2.

Figure 1 - A View of a the Series 2002 MultiPacker instruments for 25mm Spring Columns (left) and 50mm ID Spring Columns (right)

Figure 2 - The Series 2002 MultiPacker Control Deck

The Series 2002 MutiPacker Instruments are simple in design and purpose. The instrument consists of a vertically oriented cylinder that is powered by a compressed gas. The movement of the tip of the cylinder rod is guided by a sliding mechanism that rides along three fixed rods. This design constrains that cylinder rod to the axis of the Spring Column. Movement of the sliding mechanism is controlled using the rocker switch (to begin movement up or down) and speed control valve. While the packing pressure also has some influence on the speed of movement of the sliding mechanism, it is not meant to control it. The speed control valve restricts the fluid flow out of the two hydraulic cylinders mounted below the control deck. This damping mechanism can effectively slow or stop the movement of the sliding mechanism at any time. This allows safe and smooth operation of the apparatus. The gas pressure is adjustable from below 20 psi to 80 psi and is indicated on the gauge face located on the control deck. Increasing the pressure above 85 psi using the regulator on the control deck will cause a safety release valve to open. The setting of this safety valve cannot be changed and is preset to insure that operation takes place within the design limits of the instrument. The ultimate packing pressure that can be achieved within the chromatography column when the packing is complete is shown on the label around the outside of the gauge. The packing pressure can be adjusted between approximately 400 psi and 2000 psi.

Series 2002 Spring Columns

MODcol’s Series 2002 Spring Columns are available in several different configurations. The Columns are available in 25mm or 50mm inner diameter call outs (the actual inner diameter is 26.16mm and 51.56 respectively). Two lengths are available to accommodate different ranges of bed height; the 40cm column length allows the user to pack 5cm-15cm bed lengths while the 70cm column length allows the user to pack 5cm-30cm bed lengths. In certain situations bed lengths less than 5cm or more than 30cm in length can be packed successfully (for more information, see “Important Slurry Packing Hints” on page 11). All Spring Columns can be ordered with an integral water jacket that features internal baffles to homogeneously direct water flow around the column tube. A list of part numbers for all Spring Column configurations and replacement parts is provided on page 39 in the section “List of Parts and Accessories”. A photo of a disassembled Spring Column is shown with its internal components identified in Figure 3. The Spring Column consists of the following parts: • Spring Column Body – constructed of electropolished type 316 stainless steel • End Plate • Outlet Frits and PTFE Oring Seals • Piston Oring – Teflon coated elastomer for compatibility with all fluids • Piston Assembly – consists of a metal core, a Teflon sleeve and a frit • Guide Tube and Spring elements • Spacers – optional packing (5cm length) and unpacking spacers • Locking Mechanism - Threaded Spacer and Threaded Flange • Tubing and Connectors –stainless steel inlet tubing, union, nuts, ferrules and plugs • Assembly Hardware – set of three bolts, nuts and washers for the end plate and three

bolts for the locking mechanism (threaded spacer and threaded flange)

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Figure 3 – A disassembled spring column.

Parts shown in Figure 3:

1. Spring Column body 2. Spring Column piston assembly (piston, frit, PTFE sheath). Also shown:

PTFE encapsulated oring 3. Locking mechanism threaded spacer 4. Locking mechanism threaded flange 5. Locking mechanism bolts 6. Column (outlet) Endplate and assembly hardware (six bolts, flat washers, lock

washers and nuts) 7. Frit and orings for column outlet 8. Unpacking Spacer for 70cm Spring Column bodies 9. Unpacking Spacer for 40cm Spring Column bodies

Not Shown: packing spacer, inlet tubing and tubing connector accessories.

1

3

4

65

27

9

8

Spring Axial Compression Overview Overview of axial compression

Axial compression systems fulfill one main objective, namely to compensate for void formation that can occur under certain circumstances commonly found in preparative-scale chromatography columns. In traditional columns designed with fixed bed geometry, bed consolidation leads to an internal space or void that is filled with only mobile phase. The presence of a void leads to severe performance degradation under most types of chromatographic operation (e.g. not for ion-exchange resin under strong-binding conditions).

In the typical axial compression system, a piston is coupled to a linear drive mechanism. The piston is designed to enter and pass through a smooth-bore pipe or “column” to which the drive system is anchored. Column packing is accomplished by compressing a slurry with the piston, forcing out the liquid until the chromatographic media is compressed together tightly. If the linear drive mechanism continues to drive the piston after packing, an axial compression force is applied to the packed bed. In some circumstances this provides the additional benefit of preserving a high bed density or eliminating voids that may be generated when the bed increases in density or when solids are lost through the column outlet.

Axial compression systems use media efficiently because there is no waste. All of the media prepared as a slurry and charged into the column becomes part of the bed. Since the force that is developed within the bed during the packing is never dissipated or released, packing densities are higher for the same pressure when compared to traditional column packing techniques. Because of this, much lower packing pressures are used. This means that less physical damage is done to the media and the resulting media bed will be more robust. The “force” used to push the piston against the bed may be active or passive, mechanical or hydraulic. Most axial compression systems use a hydraulic piston that is continuously powered, e.g. an active system. The hydraulic system is used to pack the column and to maintain the axial compression force. In the MODcol system, a pneumatic system is used to pack the column (the MultiPacker system) while a system of spring elements is used to effect the axial compression. This design allows the spring column to be extremely fault tolerant since there are no components that can fail.

Spring Axial Compression Operation Theory

In general, axial compression systems must compensate for void formation as discussed above. A careful consideration of the void volume can be used to show that a spring driven system is completely adequate in providing a system for axial compression. Most columns used in modern preparative chromatography are 25cm and shorter in length. With modern chromatographic resins that suffer from bed consolidation, even the worst material will not consolidate more than five percent in a well-packed bed. At these high levels of bed settling, other problems such as frit blockage or media collapse would render the column unusable. It is therefore sufficient to compensate for on the order of one centimeter length of void. Over this length, a spring can be used to provide the force necessary for axial compression. A spring driven axial compression system does not operate in the same manner as a hydraulic powered one. In a spring, the restorative force is zero when the spring is at its equilibrium length and increases as the spring is compressed. In order for the spring to perform useful work it must be under a minimum amount of compression at all times. To advance the piston, the force generated by the spring must be greater than the static frictional forces. The spring force must also be sufficient to counteract the hydrostatic force that is generated by the pressure of the liquid within the column acting upon the piston head.

The limits discussed in the paragraph above define a “window” of operation for the spring. Consider Figure 4:

Spring Performance

Length

Fo

rce

Lmin

Fmax

Fo

Lo

w i n d o w o f o p e r a t i o n

F = 0

Figure 4 – Illustration of force vs. compression relationship for a spring. The spring follows the blue line during compression and extension.

The force that is stored in a spring increases from zero as it is compressed. When the spring is fully compressed, it is pushing back with a force that is indicated by Lmin, Fmax in Figure 4. As the spring uncompresses to push the piston along the column, the force it is generating decreases. In the spring column design, one end of the spring is locked in place while the other is free to push against the piston.

There are other forces to consider: The hydrostatic force generated by the pump pressure acting on the piston pushes back against the force generated by the spring. The seals in the piston experience friction with the inner wall of the column. This “static friction” also acts against the spring force by resisting movement. The spring force must be than the sum of the hydrostatic force and the static frictional force in order for axial compression action to occur. The limit is reached when the spring force is equal to the hydrostatic force plus the static friction. This situation is indicated by L0,F0 on the graph. If the hydrostatic pressure is reduced to zero, i.e. the pump is shut off, the piston could advance but when the pump was restarted the piston could be pushed back to L0. As a result of the design of the spring column, the system can easily be returned to the state indicated by Lmin, Fmax by returning the column to the MultiPacker instrument and recompressing the internal spring elements. It is important to understand that the spring elements are compressed only during the column packing. Using a spring that is unsuitable for the application at hand will lead to sub optimal performance. For instance, if the force applied by the MultiPacker is small

compared to the stiffness of the spring, only a small amount of compression will be achieved and therefore a small amount of axial compression action will be possible before L0 is reached. This could occur, for instance, if the system was used to pack soft-gel or other media at a low pressure using a stiff spring element. Another sub optimal condition will be attained if the column is packed at a pressure less than the use pressure. Under these conditions, the spring will not provide sufficient force to resist the hydrostatic pressure within the column and the piston will be pushed backwards. In short, the performance will be immediately degraded by the formation of a void. Thus, packing a spring column at a pressure lower than the use pressure should always be avoided. In order to allow the Spring Column to be as versatile as possible, various springs elements with different stiffnesses are available for use with the Spring Column. Each should be used within the appropriate packing pressure range only. Consult the section “List of Parts and Accessories” on page 39 to select the appropriate spring kit for your application.

Using Your Spring Column Introduction

The MODcol Spring Column and MultiPacker system has been designed to provide easy access to a wide variety of people. No previous knowledge of chromatography or column packing is needed. The MultiPacker instrument operates at the push of a button and columns can be packed in as little as 10 minutes, start-to-finish. Column unpacking, cleaning and frit replacement are also simple and straightforward. In general, column packing follows these steps:

1. Insert the piston into the column 2. Prepare the slurry and pour it into the column 3. Attach the column endplate 4. Insert spring elements and locking mechanism into the column 5. Pack the column using the MultiPacker 6. Secure the locking mechanism

Detailed, step-by-step instructions are given in the following pages that carefully illustrate how to pack and unpack MODcol Spring Columns. Review the next section entitled “Important Slurry Packing Hints” prior to the first use of the instrument. The Spring Column may also be used as a conventional column simply by omitting the spring elements and guide tube. The simplicity and convenience of self-packing is retained but the action of the spring axial compression is not. This may be advantageous if continuous operation at high pressures (e.g. near 2000 psi) is expected since little axial compression action would be possible from the spring system under those conditions.

Caution! Silica and other fine particulate media used in liquid chromatography poses an inhalation hazard in dry powder form. Avoid inhaling silica dust when handling this material. Many slurry solvents are flammable and toxic. Use caution when making slurries and wear appropriate safety clothing. Handling of media and solvents should be done in well-ventilated areas only. Important Slurry Packing Hints

The 2-1 Rule: A 2-1 ratio of the volume of slurry to the final bed volume in the packed column yields good results with particles near 10um in diameter. Somewhat more concentrated slurries can be used for larger particles. Also, with most bonded phases a slurry solvent consisting of ethanol, isopropanol or a mixture of the two is a good starting point. For bare silica, hexane or heptane is suitable. Other solvents that produce good results include acetone, tetrahydrofuran and chloroform. You can experiment and develop your own rules of thumb or “recipes” that work well with the media you will be using.

To obtain the best results when following the “2-1” volume rule, we recommend the following procedure. First, decide what bed height you would like to pack. Calculate the volume of the bed (V=h*Ac where h is the bed height and Ac is the cross sectional area of the 25mm and 50mm Spring Columns: 5.375 cm2 and 20.88 cm2 respectively) and double it. This is the volume that the Spring Column will receive when you charge it with the slurry. To set the spring column up for this volume we will position the piston at a distance that is twice the desired bed height removed from the “outlet” end of the column (with three plain holes in the flange). Insert the Spring Column in the MultiPacker with the coned end (having six threaded holes in the flange) up. Lubricate the inner wall of the Spring Column with a solvent such as ethanol or isopropanol. Insert a piston assembly including the oring with the frit side down into the coned opening and place the threaded spacer behind it. Close the speed control valve fully and fully depress the rocker switch so that it is in the “down” position. The cylinder may move a few inches and then it should stop. By slowly opening the speed control valve you will be able to control the speed at which the cylinder rod is lowered. Remember to close the speed control valve to stop the movement. Returning the rocker switch to the middle (OFF) position will not necessarily stop the movement of the cylinder rod! Using care, slowly lower the cylinder rod while positioning the threaded spacer below until the packing adapter on the end of the cylinder rod mates with the threaded spacer. Now slowly push the piston into the column. You should be measuring the space UNDERNEATH the piston where the slurry will be charged while the piston is moving. A flexible measuring tape is helpful for this purpose. When the piston reaches the desired depth, close the speed control valve and return the rocker switch to the middle position to vent the air from the cylinder. You can now remove the column from the MultiPacker, turn it over and charge it with the slurry following the procedures given under “Packing the Spring Column” on page 18. Hints that make slurry preparation easy: The spring column should be packed with all of the media that you add to the slurry. It is a good idea to reserve a little bit (50-75ml) of the slurry solvent that can be used to wash out the last bit of media from the container in which the slurry was prepared. This reserved liquid can then be added into the slurry to make up the total volume. If the desired slurry volume is unknown, the steps outlined above and in the section “Preparing the Spring Column for Packing” on page 16 can be postponed until after the slurry has been made, at which time its volume could be determined. The piston assembly can then be inserted to the proper depth before the column is charged with the slurry.

We find that a wide-mouth, screw top, tightly sealing container that is about 1.5-2 times the total slurry volume or more is helpful for preparing the slurry. The media and solvent are easily charged, the top screwed on tightly and the container vigorously shaken to thoroughly mix the contents. A container with volume markings on the side is very useful. While a container made of Teflon is helpful since it empties completely without leaving any residue behind, any inert plastic container is adequate. How much media should I use? This is not an easy problem to answer. The bed length depends upon the total mass and particle size of the media used, the packing pressure and speed and even the solvent. Usually we make an initial estimate based on experience and adjust the amount of media from there while keeping all other parameters fixed. This

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makes it easy to calculate the change in the amount of media that would be required to increase or decrease the bed length. For instance, if you have used a media and developed a “recipe” that works for a bed that is 5cm in length then a 15cm bed will require three times as much media. As long as you use the same solvent, slurry volume, packing pressure and speed the bed length is a linear function of media mass. Packed media densities can range from 0.5 g/cm3 or less to 0.8 g/cm3 or more depending upon the factors mentioned above. Small particles and high pressures yield higher packed densities. Large particles, very slow packing or low packing pressures yield lower densities. These densities are for bonded silica materials. Polymeric medias are even less dense. We have attempted to provide the user with a starting point from which they may form their own standard procedures. See the section “Spring Column Chromatograms and Packing Methods” on page 26 for examples. How to pack non-standard bed heights: Under certain circumstances, high performance beds with lengths less than 5cm or greater than 30cm can be packed successfully. Usually as the bed length increases over 30cm the performance will decrease however if larger particles are used (e.g. 15-20 microns or larger), successful packing of beds as long as 40cm or more may be possible. This requires quite concentrated slurries however and the use of acetone, THF or other low viscosity solvent is advised. Beds shorter than 5 cm can also be packed to create repackable guard columns. The “2-1” rule can still be followed for these short beds. An extra packing spacer may be required to reach below the 4-5cm bed length range but this is easily included in the normal packing setup. How long is the bed length that I have packed? It is a simple matter to measure the bed length of a packed column. The design of the Spring Column allows a small diameter rigid rod to be inserted into the space behind the piston and the distance between the top of the column flange and the back of the piston measured. To calculate the length between the outlet frit and the piston frit (the bed length) use the following formula:

D = distance measured between back of frit and top of column flange in centimeters (see drawing)

25cm ID, 40cm L column body: bed length = 37.85 – D centimeters




The piston does not move smoothly through the column. If a dry piston is inserted into a dry column and then pushed further using the MultiPacker, the friction that occurs between the Teflon sheath around the piston and the wall of the column will hinder its movement. Smooth movement of the piston requires that both the piston and the column wall must be LIBERALLY wet with a solvent such as isopropanol or ethanol. This provides a thin film of liquid lubrication that later evaporates. What spacers must I use to obtain the desired bed length? The Spring Column is supplied to the MultiPacker user with a variety of spacers. Certain combinations of these must be used to achieve a particular bed height. A guide that follows the 2-1 rule is shown below:

*NOTE: For 25-30cm beds use 1 packing spacer, for 20-25cm beds use 2 packing spacers, for 15-20cm beds use 3 packing spacers, for 10-15cm beds use 4 packing spacers and for beds 5cm and less use 5 packing spacers as shown below.

Packing a 30cm bed* in a 70cm Spring Column:

0 packing Spacers 1 Threaded Spacer for 70cm columns

Packing a 5cm bed in a 70cm Spring Column:


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I am unpacking the column but I can’t get the piston to move! What do I do? This is sometimes encountered, especially if the column has been allowed to dry out. When fine particles are packed into a tube, the forces that are applied to the bed at one end cause it to push outwards against the walls of the column. The piston cannot be moved because the static friction that exists along the bed at the column wall cannot be overcome. Luckily there is a simple solution! Proceed normally by removing the end plate, outlet frit, guide tube and spring elements. Reconnect the piston inlet tubing to an HPLC pump and pump some mobile phase (or even water) through the bed until liquid has emerged from the exposed end of the bed for 1-2 minutes. The flowing liquid softens and lubricates the bed so that the unpacking can proceed normally. When I pack a column the results do not meet my expectations. I hope that this doesn’t happen to anyone! The MultiPacker and Spring Column are simple and effective tools for making great columns. But when faced with a problem that you cannot solve, please do not hesitate to contact MODcol’s staff for advice. We can draw on over 20 years of experience with all kinds of chromatographic media to develop a packing method with a sample of media that you send to us. We are here to help you.





Packing a 5cm bed in a 40cm Spring Column when the spring is omitted: 2 packing Spacers 1 Threaded Spacer for 40cm columns

Preparing the Spring Column for Packing

1. Check to see that all required parts are clean and in working order before proceeding to pack a spring column (see Figure 3 for help with part identification) 1.1. Piston Body assembly (including frit) 1.2. Tubing Connectors and inlet tubing 1.3. Guide Tube 1.4. Spring elements 1.5. Threaded Spacer and flange 1.6. Packing Spacers (if required) 1.7. Endplate 1.8. Assembly hardware 1.9. Tools (wrenches for the bolts and tubing connectors)

2. Assemble the Belleville spring washers on the Guide Tube using the following information: 2.1. Each washer is manufactured to have a slight conical shape. By inspecting each

washer, one can determine if the cone is in the “up” or “down” orientation. This is easily observed by placing the washers on a flat surface such as a table.

2.2. To assemble the washer stack, slide each washer on to the guide tube in the opposite configuration as the previous washer, e.g. one “down”, the next “up”, the next “down” and so on.

NOTE: Correctly orientating the washers is important for proper performance of the axial compression system. Please consult Figure 5 for a helpful i l lustration of an assembled washer stack and guide tube.

Figure 5 – Illustration of the proper way to orient a stack of Belleville washers on the Guide tube

3. Mount a Clean spring column body on to the Mounting Plate on the MultiPacker Bracket with the coned end facing up. The coned end of the spring column is identified by the six threaded holes in the flange.

4. If no inlet tubing is attached to the piston body tubing connector section, perform the following steps: 4.1. Obtain the desired tubing connector fittings supplied by MODcol Corporation 4.2. Slip the nut and ferrule on to the end of a new section of tubing 4.3. Using the column endplate and a wrench, install the fitting and tighten firmly

until the ferrule is swaged tightly on to the tubing 4.4. Remove the assembled fitting from the endplate 4.5. Thread the assembled fitting in to the Spring Column piston 4.6. Tighten the fitting with a wrench ¼ turn to seal the fitting

5. Press the round, PTFE coated o-ring into the gland on the head of the piston body. The oring may need to be slightly stretched before it will slip on easily. To stretch the oring, pull with moderate pressure equally around the ring until it is just able to slip over the piston body. The fit should be tight.

6. Wet the internal wall of the spring column at the coned end using a lubricating solvent such as ethanol or propanol

7. Insert the piston body insert into the coned opening in the column so that it is not tilted 8. Apply additional lubricating solvent to fill the coned opening around the piston 9. Place the threaded spacer on top of the piston body 10. Align the piston and threaded spacer so that the top of the threaded spacer lies

directly underneath the cylinder rod

11. Close the speed control valve 12. Bring the cylinder rod into contact with the threaded spacer by moving the toggle

switch on the MultiPacker unit into the “DOWN” position and then slowly opening the speed control valve. To stop the cylinder rod, first close the speed control valve and then return the control lever to the middle (OFF) position.

13. Push the entire assembly into the column to the desired depth (see notes, below).

NOTE 1: The depth wil l depend upon the volume of slurry that is to be charged into the column. See the “2-1 rule” in the section entit led “Important Slurry Packing Hints” for more information.

NOTE 2: If the desired slurry volume is unknown, the steps used to insert the piston assembly into the column can be delayed unti l after the slurry has been made, at which time its volume could be determined. The piston assembly can then be inserted to the proper depth before the column is charged with the slurry.

14. Fully retract the hydraulic cylinder rod by moving the toggle switch to the “UP” position until the sliding mechanism comes to a stop in its fully retracted position.

15. Remove the threaded spacer from the column and invert it. 16. Seal the end of the tube leading to the piston. This can be done with an additional

tubing connector and a union that is terminated with a plug. You are now ready to charge the column with the slurry and pack!

Packing the Spring Column

Before proceeding with this section, first follow the steps outlined in the preceding section “Preparing the Spring Column for Packing”

1. Locate the parts required to bolt the end plate on to the column and place them nearby. These include the endplate, frit, outer and inner o-rings, and three bolts, nuts and washers.

2. Locate the spring column parts, including the guide tube, spring elements and threaded spacer. Place them nearby.

3. Check that the desired packing pressure has been set by following these steps: 3.1. Move and hold the toggle switch in the “UP” position and allow the sliding

mechanism to fully retract. 3.2. Adjust the regulator knob to achieve the desired pressure indicated on the gauge. 3.3. Return the toggle switch to the middle position.

4. Prepare the required volume of slurry for the spring column. 5. Place the Spring Column in the MultiPacker with the open end up and charge the

column with the slurry. 6. Clean the frit recess and o-ring groove in the column flange of any spilled slurry if

necessary.

7. Place the bed support frit, disperser frit (for 50mm columns only), inner o-ring and outer o-ring into the column flange.

8. Place the end plate on to the column flange 9. Place a flat washer over the threaded shaft of each bolt and insert it through the bolt

holes in the column flange. 10. Thread the nut on to each bolt and hand tighten. 11. Using a wrench, tighten the bolts. The recommended torque specification for the bolts

is 25-30 foot-pounds for the bolts used with the 50mm Spring Column endplate and 20-22 foot-pounds for the bolts used with the 25mm Spring Column endplate.

12. This step is optional: Thread a plug into the hole in the endplate. Invert the column assembly several times to remix the slurry. Make sure to remove the plug before packing!

13. Place the column in the MultiPacker mounting plate oriented so that the endplate is down

14. Insert the guide tube and spring elements, any packing spacers (if used) and then the threaded spacer and flange behind the piston. Make sure that the threaded flange has been moved to the top of the threads (away from the column) so it will not interfere during the packing

15. Close (shut off) the speed control valve and move the toggle switch to the “DOWN” position.

16. Hold the top of the threaded spacer with one hand and use the other hand on the speed control valve. Lower the sliding mechanism into position above the top of the connector rod by slowly opening the speed control valve to allow the cylinder rod to descend. Stop the sliding mechanism at an appropriate height by closing the speed control valve.

17. Align the threaded spacer and the packing adaptor of the sliding mechanism. Take care not to pinch the hands or fingers.

18. Close the speed control valve and return the toggle switch to the “OFF” (middle) position.

19. Set the speed control valve to the desired setting. 20. Pack the column by moving the toggle switch to the “DOWN” position. Depress the

switch firmly so that it locks in that position and the system is maintained under pressure after the sliding mechanism comes to a stop. If desired, the column may now be operated in the instrument. The bed may continue to settle for a few minutes. The column can be left under compression from the pneumatic cylinder during this time if desired.

21. Rotate the threaded flange with your hand to lower it. Bring it close to the column flange, leaving approximately 1/8-inch (4mm) gap. Make sure that the holes in the threaded flange and the column flange are lined up.

22. Thread the three bolts through the threaded flange and into the bolt holes in the column flange then and tighten using your hand or by applying minimal force using a wrench. Do not over torque the bolts!

23. Retract the sliding mechanism by moving the control lever into the “UP” position. 24. Remove the packed column from the MultiPacker instrument. It is now ready to use.

Unpacking a Spring Column

1. Place the spring column into the column mounting plate on the MultiPacker with the locking mechanism at the top.

2. Close the speed control valve. 3. Lower the sliding mechanism until it contacts the threaded spacer by moving the

control lever to the “DOWN” position and slowly opening the speed control valve. Take care to align the parts when they come in contact with each other.

4. Keep the control switch in the “DOWN” position and allow the cylinder to push down on the threaded spacer. This will slightly compress the spring and free the locking mechanism bolts, which can then be turned by hand or using a wrench.

5. Unscrew and remove the nuts or bolts holding the threaded flange of the locking mechanism to the column flange

6. Release the pressure by moving the toggle switch to the “UP” position until the sliding mechanism reaches its fully retracted position.

7. Remove the locking mechanism, the guide tube and the spring elements by inverting the entire column.

8. Remove all bolts on the endplate of the column 9. Remove the endplate, orings and frits (if possible) to expose the media bed 10. Insert the unpacking spacer into the column and return the column to the MultiPacker. 11. Place an unbreakable container below the column in position to receive the media 12. Close the speed control valve 13. Lower the sliding mechanism until it meets unpacking spacer by moving the toggle

switch to the “DOWN” position and slowly opening the speed control valve 14. Unpack the media by continuing to push the unpacking spacer. Control the speed

using the speed control valve. Collect the media in the pan positioned below the column. When the piston assembly emerges from the column take care not to let it drop into the pan or it may be damaged.

Note: Care must be taken to “Catch” the piston assembly as it is pushed out of the column. To catch the piston assembly, place one hand below the column ready to catch the assembly watch for its leading edge to begin to emerge from the end of the column. Advance the sl iding mechanism another 1-2 cm. As soon as the orings clear the end of the column, the parts wil l drop into the catching hand. At this point, the sl iding mechanism direction may be reversed and returned to its ful ly retracted posit ion by moving the control lever to the “UP” posit ion.

15. Discard the PTFE orings, which cannot be reused. Use discretion when choosing to reuse frits. Do not attempt to reuse a bent or chipped frit nor a frit that has been clogged by deposition of organic substances.

Cleaning the Unpacked Spring Column Parts

1. Cleaning of the piston assembly 1.1. Remove the orings from the head of the piston body assembly 1.2. Discard the Teflon–encapsulated orings if they are damaged (cut, abraded, etc.) 1.3. Wash the media from the piston body assembly using the following guidelines:

NOTE 1: any l iquid used to wash the fr it section of a piston assembly wil l enter the fr it. While detergents easi ly remove any remaining media, f lushing of the fr it to el iminate any detergent residue is advised.

NOTE 2: The piston assembly is designed to be reusable, however after several uses, the backpressure of the spring column may rise as small particles (e.g. f ines from the media) become lodged in the fr it. Sonication of the fr it in a suitable solvent for one hour may reduce the backpressure to normal levels. Replacement of the fr it can be accomplished using a Frit Replacement kit obtained from MODcol (see the l ist ing of replacement parts on page 38). Use of a heat gun is required for this purpose. An exchange of the used, assembled frit section of the piston body for a new unit (having a new frit) is also avai lable from MODcol as a service. Please consult MODcol’s technical support department for addit ional information.

1.4. The spacers are constructed from aluminum and may be washed with a mild detergent. Take care to dry any residual water thoroughly.

2. The column body and endplate are constructed from stainless steel. Washing may be done with an organic solvent or hot water and detergent. More aggressive conditions may be used to remove any deposited material. These parts are indefinitely reusable when care is taken not to scratch the surfaces that are wet by the mobile phase.

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Teflon

How to Replace Seals and Frits Seal Replacement

The main seal system is located on the piston assembly consists of a Teflon-Encapsulated-Viton oring that is compatible with all solvents used in chromatography. These orings should only be replaced if necessary, for example in cases where the Teflon coating has begun to show signs of wear or if sealing is no longer effective.

A secondary sealing system can be found on the piston body. This sealing system consists of a thin Teflon sheath that holds the frit to the piston body. Its main purpose is to prevent media from reaching the main Teflon-Encapsulated oring. This is replaced along with the frits in the procedure outlined in the next section. The entire sealing system in the piston assembly of the Spring Column has been designed for a high amount of reuse. It has been demonstrated at MODcol that, under normal operating conditions, ten or more packings may be done before replacement of the seals is warranted.

Before a new Teflon encapsulated oring can be installed, it may need to be stretched slightly before it can be slipped on to the piston assembly. Using both hands to pull outwards on the oring, stretch it using low to moderate force. Only stretch it the minimum amount necessary to allow it to slip on to the piston. Excessive stretching may impair the performance of the seal. Frit Replacement

When to Replace Frits

If the performance and appearance of the frits is acceptable (pressure drop is not excessive, no discoloration, etc.) then the frit section of the piston body may simply be cleaned with an organic solvent or mild soap and water to remove any remaining media. If soap and water are used, care should be taken to remove all of the soap from the pores of the frit before using the part. Blowing air through the back of the frit will cause the top of the frit to bubble if soap is still present. Cleaning of the entire frit section with a strong organic solvent in an ultrasonic bath is also recommended. Make sure to thoroughly rinse away any of the solvent that may remain in the pores of the frit before reusing the assembly. If there is excessive pressure drop or discoloration that cannot be removed using these methods then the frit should be replaced using one of the Frit Replacement Kits. Consult page 38 for a list of replacement parts for the Spring Columns.

STEP 1: Preparation

The Frit Replacement Kit includes a section of heat-shrink Teflon, a frit and installation instructions. A source of heat capable of high temperatures (e.g. 530ºF / 275ºC) is required such as a “heat gun” or an oven. A sharp razor blade, the MultiPacker instrument, the piston assembly, a clean spring column body and a lubricating organic solvent such as ethanol or isopropanol are needed for frit replacement.

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Teflon

STEP 2: Remove the Teflon sheath and Frit

Before the new frits can be installed, the old frits and Teflon sleeve must be removed. To remove the Teflon sleeve, cut it along its edge using a sharp razor or knife. Take care not to scribe or mark the raised ridges that run around the outer edge of the metal core underneath the Teflon sleeve. Once the Teflon has been removed, the frits are easily separated from the metal core. The metal core should be cleaned before installing the new frits. It is constructed entirely from type 316 stainless steel so that, if necessary, very aggressive cleaning conditions may be used.

STEP 3: Assembly

To install the frit, first place the piston with the radial slots (See Figure 6) oriented upwards on to a heat-resistant surface (if using a heat gun) or in the oven. Position the frit so that the side with a more coarse appearance lies on top of the radial slot pattern in the piston, e.g. is “facing down”. Center and align the frit and the piston and then place the section of heat-shrink Teflon around them. Best results are obtained when the frits and Teflon are centered about the core as shown in Figure 6.

Figure 6 – Positioning the core of the frit section (left), aligning the core, frit and heat-shrink Teflon (middle) and after shrinking the heat-shrink Teflon (right).

If using an oven, heat the part to and maintain at 300ºC for approximately 15 minutes to ensure full shrinkage. If using a heat gun, direct the hot air on to the heat-shrink Teflon from above using a circular motion so that heating is even. Once the shrinking has occurred, continue to heat the Teflon for approximately 2-3 minutes, directing full heat on to the sides of the part. Allow adequate time for the part to cool, remembering that the heated metal core will cool slowly and can burn.

STEP 4: Swaging the Teflon onto the Piston Core

Once the piston assembly has cooled, it must be pushed once through a spring column body using the MultiPacker instrument in order to force the Teflon material onto the sharp ridges of the piston. The ridges prevent the Teflon from slipping off during column packing.

NOTE: It is important not to remove the excess Teflon material before the assembly has been pushed through the column.

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Teflon

NOTE: In order to control the movement of the MultiPacker sl iding mechanism you wil l need to use the speed control. If you are not famil iar with the operation of the speed control, famil iarize yourself with its operation at this t ime by moving the sl iding mechanism of the MultiPacker up and down and turning the speed control knob clockwise to slow or stop the movement. The speed control works only in the “down” direction. To slow movement in the “up” direction, reduce the air pressure below 20psi.

Place a spring column in the mounting bracket of the MultiPacker with the coned opening upwards. Liberally wet the walls of the spring column with the lubricating organic solvent such as ethanol or propanol. Place the piston assembly into the coned opening so that the frits enter first. No orings are needed. Remove the threaded flange from the threaded spacer and place it on top of the piston assembly. Lower the sliding mechanism until it contacts the threaded spacer, repeating alignment if necessary. Slowly push the piston assembly through the spring column body. Use the speed control to keep the speed low (e.g. 0.5inch/sec or 1cm/sec). If the maximum travel of the sliding mechanism is reached before the parts exit from the bottom, add a packing or unpacking adapter below the threaded spacer. To prevent damage to the piston assembly it is important to “Catch” it as it exits from the column body. Do not let it fall to the floor. To facilitate catching the piston assembly, reduce the speed to a minimum just before the piston assembly exits the column.

STEP 5: Trimming the excess Teflon

In the final assembly step, the excess Teflon material is removed using a sharp razor blade. Use Figure 7 as a guide. Hold the frit section of the piston body in one hand with the frits oriented upwards and hold the razor blade in the other hand. Push the razor blade through the Teflon above the surface of the frits. Place the thumb of the hand holding the razor blade on to the side of the frit section of the piston body. Rotate the frit section of the piston body so that the razor blade begins to cut the Teflon material. The knife blade should be oriented so that it is almost parallel to the frit surface, tilted up and away from the frits slightly so that it cannot scratch them. Work the knife down through the Teflon to the edge of the frits in a spiral path and then continue cutting along the edge of the frits until the material has been cut down to the level of the frit. Remember to be careful not to scratch the surface of the frits with the blade. Using a similar technique, remove the Teflon that is covering the recess in which the main orings are installed. Once the Teflon has been removed, the frit section is now ready for use. See Figure 8 for pictures of a frit section of the piston body after the above steps have been performed.

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Teflon

Figure 7 – Completing the assembly of the frit section of the piston body by trimming away the excess Teflon.

Figure 8 – Three views of the completed frit section of piston body.

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Spring Column Chromatograms and Packing Methods

The following data has been presented to provide the user with a reference point from which slurry packing procedures may be developed. The examples presented in this section are representative of the chromatographic performance that can be achieved with good quality media.

MODcol does in no way guarantee that these results can be duplicated using types

of media other than those specified in each example. Some alteration of these conditions may be necessary to obtain optimum packing conditions for other types of media.

C18 bonded phase

Column: 25mm diameter, 100mm bed length Media: Kromasil C18, 10um, 100Å, 30 grams Solvent: 300 ml of ethanol Slurry Volume: 310 ml Packing pressure: 2000 psi

TEST MIXTURE:

Solute Concentration Uracil 0.2 milligrams per milliliter of mobile phase Phenol 3.6 milligrams per milliliter of mobile phase Toluene 28 microliters per milliliter of mobile phase Napthalene 1.0 milligram per milliliter of mobile phase

TEST CONDITIONS

Mobile Phase Composition: 70% Acetonitrile, 30% Water (v/v) Flowrate (mL/min): 15 Injection Volume (µL): 100 Detection Wavelength (nm): 254 Column Pressure Drop (psi): 162

TEST RESULTS

Solute Retention Time

plates per column*

Asymmetry (10%)

plates per meter

Uracil 1.73 1873 1.256 18733 Phenol 2.61 3308 1.200 33075 Toluene 6.35 5381 1.156 53812 Napthalene 7.64 5872 1.086 58715 * calculated using the USP tangent method

C18 bonded phase

Column: 50.8mm diameter, 250mm bed length Media: Kromasil C18, 10um, 100Å, 380 grams Solvent: 500 ml of fully denatured ethanol Slurry Volume: 800 ml Packing pressure: 2000 psi

TEST MIXTURE:

Solute Concentration Uracil 0.2 milligrams per milliliter of mobile phase Phenol 3.6 milligrams per milliliter of mobile phase Toluene 28 microliters per milliliter of mobile phase Napthalene 0.6 milligrams per milliliter of mobile phase

TEST CONDITIONS

Mobile Phase Composition: 70% Acetonitrile, 30% Water (v/v) Flowrate (mL/min): 60 Injection Volume (µL): 100 Detection Wavelength (nm): 254

Column Pressure Drop (psi): 420 TEST RESULTS


plates per column*

Asymmetry (10%)

plates per meter


C18 bonded phase

Column: 50.8mm diameter, 150mm bed length Media: Kromasil C18, 7um, 100Å, 200 grams Solvent: 500 ml of fully denatured ethanol Slurry Volume: 700 ml Packing pressure: 2000 psi

TEST MIXTURE:


TEST CONDITIONS




plates per column*

Asymmetry (10%)

plates per meter


C8 bonded phases

Column: 50.8mm diameter, 150mm bed length Media: Kromasil C8, 10um, 100Å, 195 grams Solvent: 600 ml of chloroform Slurry Volume: 700 ml Packing pressure: 2000 psi

TEST MIXTURE:


TEST CONDITIONS




plates per column*

Asymmetry (10%)

plates per meter


C8 bonded phase

Column: 50.8mm diameter, 250mm bed length Media: Kromasil C8, 10um, 100Å, 315 grams Solvent: 1100 ml of chloroform Slurry Volume: 1300 ml Packing pressure: 2000 psi

TEST MIXTURE:


TEST CONDITIONS




plates per column*

Asymmetry (10%)

plates per meter


C4 bonded phases

Column: 50.8mm diameter, 150mm bed length Media: Kromasil C4, 10um, 100Å, 200 grams Solvent: 800 ml of 50% chloroform, 50% 2-propanol (v/v) Slurry Volume: 900 ml Packing pressure: 2000 psi

TEST MIXTURE:


TEST CONDITIONS




Plates per Column*

Asymmetry (10%)

plates per meter


C4 bonded phase

Column: 50.8mm diameter, 250mm bed length Media: Kromasil C4, 10um, 100Å, 340 grams Solvent: 900 ml of 50% chloroform, 50% 2-propanol (v/v) Slurry Volume: 1100 ml Packing pressure: 2000 psi

TEST MIXTURE:


TEST CONDITIONS




plates per column*

Asymmetry (10%)

plates per meter


Chiralcel OD bonded phase

Column: 50.8mm diameter, 153mm bed length Media: Chiralcel OD, 20um, 185 grams Solvent: 600 ml 2-propanol Slurry Volume: 700 ml Packing pressure: 1000 psi

TEST MIXTURE:

Solute Concentration Stilbene Oxide 2.5 milligrams per milliliter of mobile phase

TEST CONDITIONS

Mobile Phase Composition: 90% hexane, 10% 2-propanol (v/v) Flowrate (mL/min): 60 Injection Volume (µL): 100 Detection Wavelength (nm): 254 Column Pressure Drop (psi): 60

TEST RESULTS


plates per column

Asymmetry (10%)

plates per meter

Peak 1 7.38 2100 1.02 13816 Peak 2 11.09 1832 1.06 12050

MultiPacker Installation This chapter explains the procedures to be followed to unpack, setup and prepare the Series 2002 MultiPacker instrument for first time use. To prepare the MultiPacker for shipping the pneumatic cylinder was removed from the instrument and the sliding mechanism was disassembled. When the MultiPacker is first unpacked there will be several labeled boxes and tubes containing the following: • The MultiPacker base assembly • The pneumatic cylinder • The aluminum air lines (in a tube) • Guide rods (in a tube) • The hose for the supply air to the instrument • Fittings to connect the air lines • The slider • The packing adapter • Assembly hardware for the guide rods, damping mechanism and pneumatic cylinder These parts must be reassembled before first time use. Follow the instructions below for first time installation. Initial Set-Up of the MultiPacker Instrument

Instructions for the 25mm MultiPacker: 1. Unpack the MultiPacker base assembly from the shipping carton and move it to the location

where it will be used. 2. (Important!) Take out plug located in the oil reservoir on the back leg of the MultiPacker

base by pushing down on the outside top of the instant fitting and pulling up on the plug 3. Unpack the guide rods and guide rod mounting hardware 4. Place the guide rods in the mounting recesses in the control deck of the MultiPacker base

assembly and loosely install the bolts and washers through control deck 5. Unpack the slider 6. Place the slider over the guide rods and slip it down to the bottom. 7. For the 50mm system, make sure the holes in the slider line up with the dowel pins on the

damping mechanism crossbar 8. Tighten the three guide rod mounting bolts installed in step 3 9. For 25mm MultiPacker: 10. Unpack the pneumatic cylinder 11. Position the pneumatic cylinder’s mounting plate above the guide rods and loosely install the

three bolts and washers 12. Raise the slider to the top of its travel 13. Tighten the three top guide rod bolts

14. Connect the aluminum air lines from the control deck to pneumatic cylinder inserting the aluminum tube with the straight instant union into the instant fitting closest to the front of the MultiPacker

15. Make sure all aluminum air lines are fully pressed into each instant fitting 16. Connect the hose to the air supply 17. Fully close the speed control knob (turn clockwise) 18. Adjust air pressure to 30psi 19. Depress the cylinder rod control switch to activate the cylinder in the down direction 20. Slowly turn the speed control knob in the counterclockwise direction to lower the cylinder

rod until it comes in contact with the slider, which should be resting on the damping mechanism crossbar

21. Insert 3” long threaded stud up through the damping mechanism crossbar and slider and thread into the adapter nut located at the end of the cylinder rod

22. Screw packing adapter onto the end of threaded stud protruding below the damping mechanism crossbar

23. (Optional) Tighten the packing adapter up to its highest point and then back it off counterclockwise so that the slot faces forward

24. Rotate the adapter nut located at the end of the pneumatic cylinder rod while holding the packing adapter so that the slot faces forwards when it has been fully tightened

25. Depress the cylinder rod control switch to activate the cylinder in the up direction until the cylinder stops

26. Close speed control 27. Depress the cylinder switch in the down position If more than one inch of downward movement of the slider is observed, perform the bleeding procedure on page 38. Instructions for the 50mm MultiPacker: 1. Unpack the MultiPacker base assembly from the shipping carton and move it to the location

where it will be used. 2. (Important) Take out plug located in the oil reservoir on the back leg of the MultiPacker base

by pushing down on the outside top of the instant fitting and pulling up on the plug 3. Unpack the guide rods and guide rod mounting hardware 4. Place the guide rods in the mounting recesses in the control deck of the MultiPacker base

assembly and loosely install the bolts and washers through control deck 5. Unpack the slider 6. Place the slider over the guide rods and slip it down to the bottom. 7. For the 50mm system, make sure the holes in the slider line up with the dowel pins on the

damping mechanism crossbar 8. Tighten the three guide rod mounting bolts installed in step 3Unpack the pneumatic cylinder 9. Position the pneumatic cylinder above the guide rods and insert them into the recesses in the

endcap so that the bottom air fitting in the endcap lines up closest with the air fitting located on the control deck

10. Loosely insert bolts and washers

11. Raise the slider to the top of its travel 12. Insert 2’ long thread rod through top and bottom endcap of pneumatic cylinder and screw

into guide rods 13. Insert washer and thread nut onto threaded rod in previous step 14. Connect the aluminum air lines from the control deck to pneumatic cylinder inserting the

tube with the straight union on the instant fitting closest to the rear of the MultiPacker 15. Make sure all aluminum are lines are fully pressed into each instant fitting 16. Connect the hose to the air supply 17. Fully close the speed control knob (turn clockwise) 18. Adjust air pressure to 30psi 19. Depress the cylinder rod control switch to activate the cylinder in the down direction 20. Slowly turn the speed control knob in the counterclockwise direction to lower the cylinder

rod until it comes in contact with the slider, which should be resting on the damping mechanism crossbar

21. Holding the slot in the packing adapter in the forward position, insert the 4” long round head slotted screw up through the packing adapter, damping mechanism crossbar, and slider and tightly thread into end of cylinder rod

22. Depress the cylinder rod control switch to activate the cylinder in the up direction until the cylinder stops

23. Close speed control 24. Depress the cylinder switch in the down position If more than one inch of downward movement of the slider is observed, perform the bleeding procedure on page 38.

Bleeding Trapped Air from the Damping Mechanism

The speed control will not function properly if air becomes trapped in the damping mechanism cylinders or tubing. The presence of air leads to a settling of the sliding mechanism when the rocker switch is moved to the “DOWN” position and the speed control valve is closed. This presents an unsafe situation to the operator. It is recommended that, if the sliding mechanism settles 1 inch or more, operation of the MultiPacker Instrument be suspended until the bleeding procedure has successfully been performed. Approximately 15 minutes time is required to complete the bleeding procedure. Use the following procedure to bleed air from the damping mechanism cylinders: 1. Open the speed control valve three turns 2. Move the sliding mechanism until it halfway between the top and bottom limits of its travel 3. Unscrew the damping crossbar from damping rods 4. Fully retract the air cylinder rod using the control rocker switch 5. Push the left damping rod to the bottom of its travel. Take care not to scratch the rod along the

edge of the opening at the top of the damping mechanism cylinder. 6. Pull the right damping rod out of the cylinder 7. Transfer approximately one-half of the remaining oil from the oil reservoir and fill the right

cylinder until the oil level is equal with the top of the cylinder 8. Reinstall damping rod by sliding it into the oil in the coned opening at the top of the cylinder.

Take care not to introduce air when performing this step. 9. Push down right damping rod to halfway position. Take care not to scratch the rod along the

edge of the opening at the top of the damping mechanism cylinder. 10. Pull up left damping rod to halfway position 11. Push down right damping rod to the bottom of its travel. Take care not to scratch the rod

along the edge of the opening at the top of the damping mechanism cylinder. 12. Pull left damping rod out of the cylinder 13. Completely fill the cylinder with oil from the reservoir 14. Reinstall left damping rod without letting air into cylinder 15. Return both damping rods to halfway position. Take care not to scratch the rods along the

edge of the opening at the top of the damping mechanism cylinders. 16. Reconnect damping rods to damping crossbar 17. Lower the cylinder rod until it is in contact with the sliding mechanism using the rocker

control switch 18. Re-connect the sliding mechanism and the cylinder rod 19. Move the sliding mechanism down to the bottom limit of its travel using the rocker control

switch 20. Move the sliding mechanism up to the upper limit of its travel using the rocker control switch 21. Close speed control 22. Depress the cylinder switch in the down position If more than one inch of downward movement of the slider is observed, repeat the bleeding procedure

List of Parts and Accessories The MultiPacker Series 2002 instruments are easy-to-use packing stations not designed to have user serviceable parts. For replacement parts, please contact MODcol or your local MODcol distributor.

MODcol Spring Column parts can be ordered using the part numbers from the following pages.

25mm ID Spring Column parts:

1. Base Spring Column Parts Kit - Choose an option 1.1. Plain Spring Column Parts Kit, 25mm ID, 40cm L. For bed lengths up to 15cm.

Part Number SA2002-025040

1.2. Water Jacketed Spring Column Parts Kit, 25mm ID, 40cm L. For bed lengths up to 15cm.

Part Number SA2002-W25040

1.3. Plain Spring Column Parts Kit, 25mm ID, 70cm L. For bed lengths up to 30cm. Part Number SA2002-025070


Part Number SA2002-W25070 1. Piston Assembly - Choose an option

1.5. Piston Assembly for 25mm ID Spring Column with 1um frit. Part Number AS2002-025A01


2. Outlet Frit - Choose an option 1.7. Outlet Frit with 1um porosity. Part Number AF0000-C02501 1.8. Outlet Frit with 5um porosity. Part Number AF0000-C02503

3. Spring Kit - Choose an option 1.9. Spring Kit for 25mm ID Spring Columns, 2000psi. Part Number AS2002-025A03 1.10. Spring Kit for 25mm ID Spring Columns, 900psi. Part Number AS2002-025A04 1.11. Spring Kit for 25mm ID Spring Columns, 400psi. Part Number AS2002-025A05

4. Tubing and Connectors - Choose an option 1.12. 1/16" OD, 0.020" ID connecting tube and fittings for use with 25mm ID Spring

Column. Part Number AS2002-025A06 1.13. 1/16" OD, 0.040" ID connecting tube and fittings for use with 25mm ID Spring

Column. Part Number AS2002-025A07

50mm ID Spring Column parts:

1. Base Spring Column Parts Kit - Choose an option 1.14. Plain Spring Column Parts Kit, 50mm ID, 40cm L. For bed lengths up to 15cm.

Part Number SA2002-050040


Part Number SA2002-W50040

1.16. Plain Spring Column Parts Kit, 50mm ID, 70cm L. For bed lengths up to 30cm. Part Number SA2002-050070


Part Number SA2002-W50070 2. Piston Assembly - Choose an option



3. Outlet Frit - Choose an option 3.1. Outlet Frit with 1um porosity. Part Number AF0000-B05001 3.2. Outlet Frit with 5um porosity. Part Number AF0000-B05003

4. Spring Kit - Choose an option 4.1. Spring Kit for 50mm ID Spring Columns, 2000psi. Part Number AS2002-050A03 4.2. Spring Kit for 50mm ID Spring Columns, 1500psi. Part Number AS2002-050A04 4.3. Spring Kit for 50mm ID Spring Columns, 900psi. Part Number AS2002-050A05 4.4. Spring Kit for 50mm ID Spring Columns, 400psi. Part Number AS2002-050A06

5. Tubing and Connectors - Choose an option 1.18. 1/16" OD, 0.040" ID connecting tube and fittings for use with 50mm ID Spring

Column. Part Number AS2002-050A07 1.19. 1/8" OD, 0.060" ID connecting tube and fitting for use with 50mm ID Spring Column.

Part Number AS2002-050A08

1.20. 1/8" OD, 0.085" ID connecting tube and fitting for use with 50mm ID Spring Column. Part Number AS2002-050A09

Replacement Parts:

Spring Columns are designed to be easily serviceable. Frit replacement is easily accomplished using the frit replacement kits. In addition to the parts that are listed above, a full array of replacement parts may be ordered from the list below. All of these parts can be re-ordered from MODcol at any time.

Part Number Description AF0000-C02501 1um Outlet Frit for 25mm ID Spring Columns AF0000-C02503 5um Outlet Frit for 25mm ID Spring Columns AH0000-R02503 Outlet Frit Seal Ring for 25mm ID Spring Columns AS2002-025A08 Replacement Hardware for plain jacketed 25mm ID Spring Columns AS2002-025A11 Replacement Hardware for water jacketed 25mm ID Spring Columns AS2002-025000 Threaded Spacer for 25mm ID, 40cm L Spring Columns AS2002-025001 Threaded Spacer for 25mm ID, 70cm L Spring Columns AS2002-025002 Threaded Flange for 25mm ID Spring Columns AS2002-025003 Packing Spacer for 25mm ID Spring Columns AS2002-025004 Unpacking Spacer for 25mm ID, 70cm L Spring Columns AS2002-025005 Unpacking Spacer for 25mm ID, 40cm L Spring Columns AS2002-025007 Piston for 25mm ID Spring Columns AS2002-025A12 1um Piston Frit replacement kit for 25mm ID Spring Columns AS2002-025A13 5um Piston Frit replacement kit for 25mm ID Spring Columns

Part Number Description AF0000-D05001 Outlet Disperser Frit for 50mm ID Spring Columns AF0000-B05001 1um Outlet Bed Support Frit for 50mm ID Spring Columns AF0000-B05003 5um Outlet Bed Support Frit for 50mm ID Spring Columns AH0000-R050A1 Oring Set for 50mm ID Spring Columns AS2002-050A10 Replacement Hardware for plain jacketed 50mm ID Spring Columns AS2002-050A13 Replacement Hardware for water jacketed 50mm ID Spring Columns AS2002-050000 Threaded Spacer for 50mm ID, 40cm L Spring Columns AS2002-050001 Threaded Spacer for 50mm ID, 70cm L Spring Columns AS2002-050002 Threaded Flange for 50mm ID Spring Columns AS2002-050003 Packing Spacer for 50mm ID Spring Columns AS2002-050004 Unpacking Spacer for 50mm ID, 70cm L Spring Columns AS2002-050005 Unpacking Spacer for 50mm ID, 40cm L Spring Columns AS2002-050007 Piston for 50mm ID Spring Columns AS2002-050A14 1um Piston Frit replacement kit for 50mm ID Spring Columns AS2002-050A15 5um Piston Frit replacement kit for 50mm ID Spring Columns

Warranty Information MODcol Corporation provides this limited warranty (the Warranty) to protect customers from non-conformity in the product workmanship or materials. The Warranty covers all new products manufactured by MODcol Corporation.

Conditions of Limited Warranty for the MultiPacker and Spring Column:

MODcol warrants that all products sold by MODcol will be of good quality and workmanship. The products will be fit for their intended purpose(s) when used strictly in accordance with MODcol’s instructions for use during the applicable warranty period.

This warranty is exclusive and in lieu of all other expressed and implied warranties, including but not limited to fitness for any other purpose(s). In no event will MODcol be liable for consequential, economic or incidental damages of any nature. MODcol reserves the right not to honor this warranty if it is determined that the customer has abused products. The Warranty will not be deemed to have failed of its essential purpose so long as MODcol is able and willing to repair or replace any non-conforming part or product.

Warranty Service Warranty service is performed at no charge and at MODcol's option in two ways: • The product is repaired at MODcol’s facility. The customer is responsible for the shipping

charges to transport the product to and from MODcol’s facility. • Replacement parts with the appropriate installation instructions are sent to the customer. Warranty service is not performed on: • Consumable parts such as frits, o-rings, etc. • Any product or part that is repaired by others, improperly installed, altered, or damaged

through misuse. • Products or parts that malfunction resulting from lack of routine maintenance, observation or

good operating procedures.

Warranty Period The warranty period begins when the product is installed, or in the case of a customer installation, fifteen days after shipment from MODcol. The warranty period for the MultiPacker and Spring Column is one year in duration. To reorder or for technical information, please call MODcol Corporation at (408) 782-5844 or toll free at (888) 349-9660.

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and spring column manual - duratec

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