Preparative, Pilot & Process Columns

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Preparative, Pilot & Process Columns 321 Preparative, Pilot & Process Columns Contents Prep Columns... 322-323 Dynamic Axial Compression Columns (DAC)... 324-325 Pilot Columns... 326-327 Chromatography columns for pilot- and process scale... 328-329 Introduction Columns for Preparative Chromatography YMC is one of the very few global suppliers in the market that meet all demands in preparative scale chromatography. Our ambition is to provide chromatographic solutions for any compound from its discovery through scaling-up into production and its quality control in the lab. We therefore offer one of the world s largest portfolios of selectivities, designed to handle even the most demanding separations, as well as providing support, chromatographic tools and technical assistance. Production Capacity The substantial investments into facilities and staff represent YMC s ongoing commitment towards high quality products and technical support: YMC s state-of-the-art silica production facilities allow large Lot sizes of more than 500 kg/lot. For many years Lots of even more than 200 kg of bonded silica have become routine operations. The annual capacity of YMC s production plants amounts to double digit tons of spherical silica.

322 Preparative, Pilot & Process Columns Preparative HPLC Columns 5-20 cm - direct scale up from analytical and semiprep YMC-Pack columns - standard column diameters: 50, 70, 100, 150 and 200 mm - standard column s: 250, 300, 500, 1,000 mm - pressure rated up to 2,000 psi - matching guard columns available Broad range of column dimensions YMC-Pack preparative columns, packed with YMC*Gels, are available in a broad variety of column sizes to accommodate virtually any preparative separation. YMC use a high-pressure slurry technique to pack all preparative columns in optional 1,000 or 2,000 psi pressure rated hardware. Standard column dimensions range from 50 to 200 mm inner diameter and 250 to 1000 mm in. Other column sizes will be available, please request a quotation. Guard columns for YMC-Pack preparative columns YMC strongly recommends the use of guard columns in order to extend column life. Matching YMC-Pack preparative guard columns are available for all the standard column sizes in either 50, 100 or 200 mm in, depending on the i.d.. mm i.d. 50 mm 100 mm 200 mm 250 mm 300 mm 500 mm 1000 mm 50 70 100 150 200 Guard columns are marked in red. Other dimensions are available. Please request a quotation.

Preparative, Pilot & Process Columns 323 Preparative HPLC Columns Distributor-frit assembly design The flanged stainless steel hardware of the YMC-Pack preparative columns contains a high efficient distributor-frit assembly that permits uniform distribution of sample across the entire diameter of the column bed. This allows maximum sample loading through optimised use packed bed. Similarly eluent flow is directed uniformly across the entire column diameter providing exceptional peak symmetry. Specification of empty flange-type column Quality assurance All YMC-Pack preparative columns are subject to an individual chromatographic test and have to meet stringent specifications which ensure excellent column performance and column-to-column reproducibility. A Column Test Report is included with each YMC-Pack preparative column specifying the theoretical plate number and asymmetry factor. All YMC-Pack columns are guaranteed to perform as shown in its Column Test Report. Convenient scale up Separations developed on YMC-Pack analytical or semi-preparative columns can be directly scaled up to preparative size YMC columns with pre-configured scale-up column kits. Each scale-up kit consists of one 4.6 mm i.d. scout column and one ore more preparative columns packed from the very same lot of bonded phase. By excluding any variation in the packing material, this method provides the opportunity to verify analytically obtained results in semi-preparative or preparative scale. Important parameters like loadability and yield can be easily determined using a 4.6 mm i.d. scout column. Being packed with the same gel lot and therefore showing exactly identical specifications, preparative columns included in the scale-up kit allow the reproducibility of the results in larger scale to be demonstrated. As a result, YMC scale-up kits provide the ultimate assurance that a chromatographic separation developed on YMC scout columns can be transferred to semi-preparative, pilot or production scale without method modification... Guaranteed.

324 Preparative, Pilot & Process Columns Dynamic axial compression Columns 5-60 cm For preparative liquid chromatography Nowadays preparative liquid chromatography is the method of choice for obtaining high value products in the pharmaceutical and biotechnological industries. By means of further developments and innovations in column technology, liquid chromatography has developed over recent years into an established and economically useful process technology. Working Principle In all dynamic axial compression (DAC) columns, a hydraulic jack operates a piston that moves inside the chromatographic column. The piston is used to maintain a controlled dynamic pressure on the chromatographic bed during column operation as well as being used for packing and unpacking operations. The DAC system allows fast column packing of virtually any kind of packing material and assures excellent bed stability, reproducibility and efficiency in pilot or production columns. YMC offers two types of column design to meet our customers specific process and site requirements: DAU-Columns: This type of DAC chromatographic column is mounted on top of the hydraulic jack; the column bed is compressed by dynamic axial compression in the upward (DAU) direction. This assembly allows convenient packing either automatically via the slurry inlet near the bottom of the column or manually by dismantling the column top. YMC DAU-Columns are available in two standard maximum bed s of 400 and 600 mm with inner diameters ranging from 50 to 600 mm and a pressure rating of 5 to 10 MPa (725 to 1450 psi). Versions with longer column beds are available on request. DAD-Columns: The hydraulic jack is mounted on top of this series of chromatographic columns and pressurizes the column bed by dynamic axial compression in the downward (DAD) direction. The DAD-column can be packed automatically via the slurry inlet near the top of the column and can be easily unpacked by pushing the column bed through the DAU 500 DAU 450 with slurry container lower column lid. Due to the compact design of this assembly the maximum chromatographic bed is limited to 300 mm. DAD-Columns are available with inner diameters ranging from 100 to 450 mm and with pressure ratings of 5 to 10 MPa (725 to 1450 psi). Options such as designed to meet specific user requirements as well as additional features slurry vessels, slurry inlets or double jackets for heating / cooling purposes are available on request.

Preparative, Pilot & Process Columns 325 Dynamic axial compression Columns Packing DAU columns loading slurry packing columns elution unpacking slurry outlet slurry column bed slurry sealing packing input sealed bring piston down Collected slurry transferring the slurry to the column compressing the slurry and removing the excess solvent the column is now ready for use bring piston down and wash packing out of the column using jets of water on 2 sides N/m 50000 40000 30000 20000 10000 0 N/m Tf 1 2 3 4 5 6 7 Packing number 1.5 1.25 Where: N/m = plate count Tf = tailing factor at 10% peak height 1 0.75 0.5 Tf Reproducibility of column efficiency Packing conditions Packing material: YMC ODS-A 15 µm, 12 nm Weight of packing material: 250 g Column: DAU 50-700 Column bed size: 50 mm i.d. x 200 mm Packing pressure: 6.4 MPa Slurry solvent: 100% methanol Concentration of slurry: 35% HPLC conditions for column inspection Sample: toluene + methyl benzoate Flow rate: 50 ml/min Temperature: ambient Detection: UV at 254 nm Eluent: methanol / water = 85/15 The specifications given here describe standard systems. To meet specific user needs, alternatives can be offered on demand. Column Column Max. bed Max. bed System Max. Model ID volume height pressure [mm] [mm] [mm] [L] [mm] [MPa] / [psi] DAU 50-700 50 700 400 0.8 2.200 10 / 1450 DAU 50-1000 50 1000 600 1.2 2.800 10 / 1450 DAU 100-700 100 700 400 3.1 2.300 7 / 1015 DAU 100-1000 100 1000 600 4.7 2.900 7 / 1015 DAU 150-700 150 700 400 7.1 2.400 7 / 1015 DAU 150-1000 150 1000 600 13.2 2.900 5 / 725 DAU 200-700 200 700 400 12.6 2.400 7 / 1015 DAU 200-1000 200 1000 600 18.8 3.000 5 / 725 DAU 300-700 300 700 400 28.3 2.700 7 / 1015 DAU 300-1000 300 1000 600 42.4 3.200 5 / 725 DAU 450-700 450 700 400 63.3 3.100 7 / 1015 DAU 450-1000 450 1000 600 95.4 3.500 5 / 725 DAU 500-700 500 700 400 78.5 3.100 7 / 1015 DAU 500-1000 500 1000 600 117.8 3.500 5 / 725 DAU 600-700 600 700 400 113 3.100 7 / 1015 DAU 600-1000 600 1000 600 169.6 3.500 5 / 725 Parts that make contact with the media are made of: 316 L stainless steel, PTFE, PFA Swagelok connections. Optional accessories (e.g. slurry container, heating/cooling casing) are available on demand.

326 Preparative, Pilot & Process Columns Pilot Columns biocompatible solvent resistant version available (optional) height adjustable plunger heating/cooling jackets available (optional) custom made for each application full stainless steel versions with extended pressure ratings available General Pilot columns are designed for use in pilot and production scale applications with organic solvents (version SR) or aqueous buffers (version AB), which makes them suitable for all common methods in chromatography including normal phase, reversed phase or biochromatography. High precision CNC manufacturing of plungers and distribution plates provides outstanding flow distribution which gives a linear flow distribution profile. Precise and reliable bed height adjustment is achieved by hand wheel adjusters on the plunger. A range of mounting options is available including fixed stands, wheeled trolley, or direct connections into plant. All materials are in compliance with FDA regulations. Certification and full documentation is available for validation purposes. The use of borosilicate glass and a completely metal-free construction guarantees maximum hygiene standards (no unrinsed areas, no dead volumes). Characteristics Column body: calibrated borosilicate glass, acrylic glass or stainless steel Pressure limit: depending on column body; 1-30 bar for glass columns, 50 bar for stainless steel columns Temperature range: aqueous buffer version (AB): up to 40 C solvent resistant version (SR): up to 70 C Wetted parts: borosilicate glass, stainless steel, PTFE or polyethylene EPDM, Viton or Kalrez seals, stainless steel or polyethylene frits Diameter: 100 mm, 140 mm, 200 mm, 300 mm (others on demand, e.g. 450 mm, 600 mm, 800 mm) Lengths: 400 mm, 750 mm (others on demand) Connections: stainless steel SR version or polyethylene AB version

Preparative, Pilot & Process Columns 327 Pilot Columns Applications gel permeation ion exchange hydrophobic interaction affinity reversed phase normal phase Areas of application: AB Series columns are suitable for use with salts and detergents, ethanol and methanol, 6M urea, 7M guanidinium chloride, 2M NaCl and 3M ammonium sulphate. The SR Series columns lend themselves to chromatography with silica gels and reversed phase materials as well as chiral stationary phases, which require the use of solvents such as methylene chloride, acetone, toluene, THF etc. Flow distributor for PILOT glass columns Specifications Model* i.d. Bed height Volume Cross section Max. pressure [mm] [mm] min [l] max [cm 2 ] [bar] PI100/400 100 100-400 0.78 3.1 78.5 10 PI100/750 100 450-750 3.5 5.9 78.5 10 PI140/400 140 100-400 1.5 6.1 154 7 PI140/750 140 450-750 6.9 11.5 154 7 PI200/400 200 100-400 3.1 12.5 314 4 PI200/750 200 450-750 14 23.5 314 4 PI300/400 300 100-400 7 28 706.5 1.5 PI300/750 300 450-750 32 52 706.5 1.5 *other models on demand, see characteristics on left page Components wetted by the media Series Capillary inlet Frits Seal Column body Temperature range SR Stainless steel 1/4" Stainless steel Kalrez KPG glass 2-70 C (Solvent Resistant) AB Polyethylene 1/4" Polyethylene EPDM KPG glass 2-40 C (Aqueous Buffer)

328 Preparative, Pilot & Process Columns Chromatography columns for pilot- and process scale Glass and steel columns for aqueous-based (Version AB; Aqueous Buffer) or organic solvent applications (Version SR; Solvent Resistant). Diameter 60 mm - 600 mm: column according to guidelines application. Custom made for each application and customer requirements. Pilot column 300 x 200 mm i.d. with cooling jacket, piroting mount, with slurry tray for column unpacking. Levelling guide to help you assemble the column correctly. Notched wheels to fix a rotating column body.

Preparative, Pilot & Process Columns 329 Chromatography columns for pilot- and process scale In addition to standard versions, PILOT columns can also be adapted to the individual wishes of the user. Adaptable options include: inner diameter up to 600 mm, bed s up to 150 mm, the materials used, height adjustment of the piston and the mechanism of supporting the column (the stand, trolley, etc.). Please see the questionnaire on page 197 for the questions to be answered before a custom built PILOT column can be manufactured. 600 mm i.d. column as a special reactor for coating processes. Integrated level indicators assist assembly / disassembly for maintenance purposes. Column head of a stainless steel 1000 x 100 mm i.d. column, 50 bar, with swivelling column body. 600 mm i.d. column, slurry outlet with separate tap, quadruple eluent outlet.