Teledyne Everywhereyoulook ACCQPrep SFC Operation Manual
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Teledyne Everywhereyoulook ACCQPrep SFC Operation Manual

Teledyne Everywhereyoulook ACCQPrep SFC Operation Manual

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ACCQPrep
SFC
®
Operation Guide
Part #69-5263-074
Rev. A October 2023
© 2022 Teledyne Instruments Incorporated. All rights reserved.
Use and Disclosure of Data: Information contained herein is classified as EAR99 under the
U.S. Export Administration Regulations. Export, reexport or diversion contrary to U.S. law is prohibited.
Diversion contrary to U.S. law is prohibited.

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  • Page 1 Part #69-5263-074 Rev. A October 2023 © 2022 Teledyne Instruments Incorporated. All rights reserved. Use and Disclosure of Data: Information contained herein is classified as EAR99 under the U.S. Export Administration Regulations. Export, reexport or diversion contrary to U.S. law is prohibited.

  • Page 3: Safety Overview

    ACCQPrep HP150 Installation and Operation Guide Safety Overview ® Refer to the document ACCQPrep SFC Important Information, (PN 69-5263-088) for the most current safety information. This document is included with your ACCQPrep system, and the latest version is available at www.teledyneisco.com. Hazard Severity Levels This manual applies Hazard Severity Levels to the safety alerts.
  • Page 4 Safety Warnings Hazard Symbols (Continued) Ce symbole signale l’existence d’instructions importantes relatives au produit dans ce manuel. Ce symbole signale la présence d’un danger d’électocution. Ce symbole signale la présence d’une surface chaude à l’intérieur du produit. Warnungen und Vorsichtshinweise Das Ausrufezeichen in Dreieck ist ein Warnze- ichen, das Sie darauf aufmerksam macht, daß...
  • Page 5 CAUTION Installation Installation should be performed by Teledyne ISCO qualified personnel. Do not carry multiple modules at the same time. WARNING WARNING Safe Lifting Practice Keep the unit upright when moving.
  • Page 6 In all cases, use good laboratory practices, appropriate personal protective equipment, and standard safety procedures. Should these chemicals be used, Teledyne ISCO highly recommends that these applications be performed in an isolated environment and/or a laboratory fume hood designed to reduce exposure to a safe level for these types of materials in accordance with federal, state, and local regulatory laws, and in compliance with your company’s...

  • Page 7: Hot Surface

    Safety Warnings CAUTION Unintended Use of this Equipment Use of this instrument in any way not specified in the manual or the user not following on-screen prompts and messages may impair the protection provided by the instrument. Operators and maintainers of the system must be provided with all applicable health and safety regulations for use of the system, its accessories, and consumables.
  • Page 8 Safety Warnings The ACCQPrep SFC system is designed to perform supercritical Hazards Unique to SFC: fluid chromatography using carbon dioxide (CO ) as the super- Using Carbon Dioxide critical fluid. The use of other supercritical fluids is prohibited. Your CO gas supplier should be consulted for proper design, installation, and safety guidance regarding CO supply infra-...
  • Page 9 Safety Warnings WARNING WARNING Pressurized Gas It is the customer’s responsibility to ensure that the ACCQPrep SFC and any CO supply and/or connections are placed in an appropriately sized room and well-ventilated space. is denser than air and can accumulate in higher concentrations in low spaces.
  • Page 10 Safety Warnings WARNING WARNING Aerosolization Depressurization of CO from the eluate during fraction collection may result in aerosolization of compounds/sample or solvent found in the eluate. Do not inhale aerosolized particles and observe safety data sheets for all substances being used. The ACCQPrep SFC system should be properly exhausted to a suitable exhaust source and the AutoSampler or fraction collection bottles should be used in an...
  • Page 11 Safety Warnings Static electricity can also be generated during system operation, Preventing Static such as when non-polar liquids flow through it. To prevent static Electrostatic Discharge During System Operation buildup as the system operates, observe the following precau- tions: 1. Do not exceed the flow rate specified in the documentation for the preparative chromatography column.
  • Page 12 If the breaker trips again, follow your company’s guidance on lock out/tag out to prevent operation until the instrument can be repaired by a qualified service technician. Technical assistance for the Teledyne ISCO ACCQPrep SFC can For Additional Information be obtained from: Teledyne ISCO 4700 Superior St.

  • Page 13: Table Of Contents

    ACCQPrep® SFC Table of Contents Section 1 Introduction 1.1 Overview ............1-1 1.2 Product Overview .
  • Page 14 ACCQPrep® SFC Table of Contents 4.1.1 PeakTrak Window Elements ........4-1 4.1.2 Method File .
  • Page 15 ACCQPrep® SFC Table of Contents 2-10 Define Methods options ..........2-14 2-11 The Idle Configuration tab .
  • Page 16 ACCQPrep® SFC Table of Contents 5-21 Disconnecting the clear tubing ........5-15 5-22 Removing the tubing .

  • Page 17: Section 1 Introduction

    • An overview of the PeakTrak interface. ® • Maintenance instructions. The Teledyne ISCO ACCQPrep SFC chromatography system 1.2 Product Overview combines high resolution and productivity in a small footprint. It features easy-to-use software, programmable gradients, UV detection and peak collection, and automatic detection of col- lection tube racks.

  • Page 18: Operating Overview

    ACCQPrep® SFC Section 1 Introduction Figure 1-1 ACCQPrep SFC ACCQPrep SFC – This Prep SFC system has flow rates from 50-200 mL/min, with up to 6000 psi (413 Bar) capability. A two component gradient can be formed between CO and 4 different cosolvents.

  • Page 19: Multiple Control Possibilities

    Teledyne ISCO recommends that you obtain assistance from your Information Technology department before attempting direct or network connections. See Technical Note 28 Net- working Guidelines on the Teledyne ISCO website for more information. The ACCQPrep SFC system can be accessed from the built-in 1.3.1 Multiple Control...

  • Page 20: System Pressure Management

    ACCQPrep® SFC Section 1 Introduction Figure 1-2 Location of power cord for the ACCQPrep SFC system The ACCQPrep SFC monitors the pressure at several different 1.4.2 System Pressure points within the system. In addition to predefined pressure Management limits within the system, the user may input a lower column pressure limit in order to use and prevent damage to columns with lower limits than system-defined limits.

  • Page 21: Specifications

    ACCQPrep® SFC Section 1 Introduction 1.5 Specifications Table 1-1 ACCQPrep SFC Dimensions of ACCQPrep SFC 41 x 56 x 73 cm (16.25 x 22.25 x 28.75 in) (W x D x H) (Footprint without column installed) Weight 83.3 kg (183.5 lbs) (Including AutoInjector, Column Selector Valve Module, Pump Module, Column Oven, and Control Module)

  • Page 22: Fcc Statement

    ACCQPrep® SFC Section 1 Introduction Table 1-3 Component Materials List Chromatographic Tubing 316 stainless steel tubing, PEEK, and Fluoropolymer Drain Tubing Vinyl with FEP liner Chromatographic Valves PEEK, PPS, perfluorelastomer (FFKM) Flow Cell PEEK, quartz, FEP Chromatography Pump 316 Stainless Steel, UHMWPE, ETFE, ruby, sapphire, and zirconia Pressure Transducer 316 and 17-4 PH stainless steels and perfluorelastomer (FFKM) AutoSampler Wash...

  • Page 23: Section 2 Configuration

    ACCQPrep® SFC Section 2 Configuration The system can be configured using PeakTrak. For more about 2.1 Configuration of the the user interface, See Section 4, PeakTrak. ACCQPrep SFC For power control, ACCQPrep SFC systems use a combination 2.2 Turning the System On power switch and circuit breaker located on the rear panel of the and Off control module and rear panel of the oven module.

  • Page 24: Instrument Configuration

    ACCQPrep® SFC Section 2 Configuration Instrument Configuration (Figure 2-1) can be found at 2.3 Instrument > T > C > I CREEN OOLS ONFIGURATION NSTRUMENT ONFIG Configuration URATION Figure 2-1 The Instrument Configuration tab EAR99 Technology Subject to Restrictions Contained on the Cover Page...
  • Page 25 If a solvent you intend to use is not on the current solvent list, please contact Teledyne ISCO for guidance. Solvent Levels – • M allows you to specify a...
  • Page 26 When the vapor level limit is exceeded, the system will stop the pumps to minimize a hazardous condition. Currently, Teledyne ISCO ships all systems with this vapor limit feature enabled to the default setting of H sensitivity.
  • Page 27 ACCQPrep® SFC Section 2 Configuration Figure 2-2 PeakTrak vapor limit alarm Once you have remedied the cause for the vapor sensor alarm, you may choose to change the default vapor sensitivity level or ignore the vapor alarm and continue operation without the vapor sensor disabled for 10 minutes.

  • Page 28: Network Configuration

    ACCQPrep® SFC Section 2 Configuration Queue Screen Custom Parameters – This sets extra param- eters for the Q tab (Section 3.3.4). These parameters change UEUE fraction collection options. • NONE = no additional parameters • UV THRESHOLD = level, as absorbance units (AU), to start peak collection Network Configuration –...

  • Page 29: User Preferences

    ACCQPrep® SFC Section 2 Configuration · DHCP: Indicates that the IP address, Netmask, and Gateway will be automatically retrieved from the DHCP server. • IP A – Enter the static IP Address for the DDRESS system. This applies only when the N ETWORK Static IP.

  • Page 30: Prep Sfc

    ACCQPrep® SFC Section 2 Configuration Figure 2-4 The User Preferences tab (detail) Language – Allows selection from several languages for the user interface. If the system is set up for multiple users, each user can select a preferred language. Pressure Units – Allows you to choose between PSI and Bar. Other User Preferences –...

  • Page 31: The Prep Sfc Tab

    ACCQPrep® SFC Section 2 Configuration Figure 2-5 The Prep SFC tab Loop Volume – The ACCQPrep SFC system ships with a preinstalled 5 mL sample loop and a 1 mL loop (found in the accessory fittings package case). The 1 mL loop provides better injection accuracy and reproducibly when doing injections below 0.5 mL.

  • Page 32: Installing A Loop

    ACCQPrep® SFC Section 2 Configuration Installing a loop is similar to installing a column (Section 2.6.4); 2.6.1 Installing a Loop however, you will need a 1/4" wrench to connect the loop directly to the injection valve in the back of the oven box drawer. Figure 2-6 The sample injection valve Ensure that the column is under appropriate solvent storage con- 2.6.2 Removing a Column...

  • Page 33: Priming The Cosolvent Pump

    ACCQPrep® SFC Section 2 Configuration Ensure that the cosolvent pump is properly primed before use, 2.6.3 Priming the Cosolvent after changing or refilling solvents, and when directed. Oth- Pump erwise, CO can accumulate in the cosolvent fluid path and enter the sample injection flow path, which could lead to sample loss.

  • Page 34: Loading A Column Onto The System

    ACCQPrep® SFC Section 2 Configuration · A window appears for each solvent’s priming cycle that reports the expected completion time of the priming run in seconds. · A “priming complete” window announces the completion of the priming process . 5. Turn the manual prime valve control to 2.6.4 Loading a Column onto the System Note...

  • Page 35: Defining A Column

    ACCQPrep® SFC Section 2 Configuration 6. While the oven drawer is open, set the flow rate to 30 mL/min, choose 5% cosolvent and select 5% C . Monitor the oven box and column OSOLVENT fittings for any leaks. Once no leaks have been confirmed, the oven drawer may be closed and the column may be used.

  • Page 36: Resetting Column History

    ACCQPrep® SFC Section 2 Configuration If you are replacing a column in a position with an identical 2.6.6 Resetting Column column, you needn’t create a new column definition, Instead, you History can reuse the existing one by choosing its C OLUMN pressing R .

  • Page 37: Idle Configuration

    ACCQPrep® SFC Section 2 Configuration 3. Press N 4. Enter the name you have chosen. 5. Once named, press E NTER 6. The newly created method uses the default method parameters. To modify the new method: a. Select E b. Make changes as desired in the method editing screen. c.
  • Page 38 ACCQPrep® SFC Section 2 Configuration to pressurize the system with CO and stabilize the flow. Pump Control allows the pumps to remain running after an operation is stopped. This provides for immediate use of the system, while reducing the use of solvent by limiting how long it is pumped.

  • Page 39: Section 3 Operation

    ACCQPrep® SFC Section 3 Operation The ACCQPrep SFC system is unique to the chromatography 3.1 Introduction market. It has several methods of operation that you can select to fit your needs. Methods contain all of the information used during a separation of a single sample, such as gradient profile, detection and peak cutting parameters, and fraction size.

  • Page 40: Starting A Separation

    ACCQPrep® SFC Section 3 Operation the M screen, or by selecting the M . Once ETHOD DITOR edited, the method can be used directly for the immediate sepa- ration(s) or saved with a name for future reuse. To separate a single sample, press S to start a separation.
  • Page 41 ACCQPrep® SFC Section 3 Operation · PeakTrak will divide S by the AMPLE OLUME injection volume to determine the number of injec- tions. · PeakTrak will perform exactly as programmed. It will also compensate for the volume of tubing used for the supplied sample probe.
  • Page 42 ACCQPrep® SFC Section 3 Operation Figure 3-3 Starting the equilibration from the Minimum Run Requirements window Figure 3-4 Sample probe prompt Figure 3-5 Sample probe prime prompt a. In most instances, you should prime the probe. b. Once the priming sequence is complete, the system will present the same two options and instruct you to lift the sample probe to insert a small air gap between the sample and priming solvent.
  • Page 43 • If the sample probe is ever lost or damaged, it should be replaced with the AutoInjector Needle Assembly. (Visit https://store.teledyneisco.com for parts for your ACCQPrep SFC system, or contact your local Teledyne ISCO representative.) 5. After the last injection is performed, a sample probe wash dialog is shown, prompting you to wash the probe with a strong solvent.

  • Page 44: Autoinjection Operating Steps

    ACCQPrep® SFC Section 3 Operation Figure 3-7 Viewing injections This section outlines the steps performed by the AutoInjector 3.3.2 AutoInjection during sample injection. Operating Steps 1. A prompt appears, allowing you to either prime the sample probe with solvent or to place the sample probe into the sample container before the separation begins.

  • Page 45: Separation Using An Autosampler Module

    ACCQPrep® SFC Section 3 Operation 7. After the first separation has completed, the next separa- tion begins with the equilibration as described above (from Step 3). During this process, the AutoInjector Module con- tinues to aspirate the programmed injection volume. 8.

  • Page 46: Creating Autosampler Queues

    ACCQPrep® SFC Section 3 Operation • Access the R tab. This will result in a screen and operation much like the standard ACCQPrep SFC system without an installed AutoSampler Module. • Select the Q button. This will allow you to set up UEUE a separation sequence for multiple samples.

  • Page 47: The Queue Screen

    ACCQPrep® SFC Section 3 Operation For example: • If you have a single injection run it can be named A01. • For multiple injections, the first injection will be named A01-I1, the second will be A01-I2, and the third will be named A01-I3.
  • Page 48 ACCQPrep® SFC Section 3 Operation change the injection volume or otherwise modify the method as needed and disable the pause for the remaining injections, or leave it enabled to allow a second condition scouting separation. Samples with pauses are easily found on the Q window: their UEUE rows are highlighted.

  • Page 49: Autosampler Injection Techniques

    ACCQPrep® SFC Section 3 Operation Figure 3-9 The Sample Options window • T — The volume of the sample, in milli- OTAL AMPLE liters, selected from a drop-down list. • I — The volume of each injection, NJECTION OLUME selected from a drop-down list. Below these settings will be listed the number of injections (i.e., T ÷...
  • Page 50 ACCQPrep® SFC Section 3 Operation 1. During column equilibrium, the sample loop is first placed into the run position. This position passes the cosolvent through the loop to clear out any air or CO that may have entered the loop. It also allows the wash solvent that is drawn up from the AutoSampler to be sent to waste instead of going into the loop.

  • Page 51: Fraction Collection With The Autosampler

    ACCQPrep® SFC Section 3 Operation 13. Air is drawn into the sample probe to draw the remaining sample into the loop without leaving any sample in the probe. 14. The sample is now loaded and the separation will begin. 15. The next injection of the sample is accomplished by repeat- ing the above process.
  • Page 52 ACCQPrep® SFC Section 3 Operation 3. Select a sample to open the S window AMPLE PTIONS (Figure 3-9). 4. Enter the T volume and I OTAL AMPLE NJECTION OLUME for each run. To initially fine-tune the method, enter a small injection volume such as 0.2 mL (see Figure 3-9), as you will be able to change it later.
  • Page 53 ACCQPrep® SFC Section 3 Operation - Allows the injection volume to be changed. In NJECTION our example, the injection volume was changed to 2.0 mL for the next injection, since the run suggested that there was sufficient resolution for a larger injection. is found on the P window ONTINUE...

  • Page 54: Stacked Injections Window In A

    ACCQPrep® SFC Section 3 Operation of the time window without entering values. The different colors (green and brown) represent a different stacked injection. The crosshatch patterns represent different time windows within an injection. Figure 3-13 Simulated stacked injections for the run in Figure 3-12 Depending on the complexity of the chromatogram, it may be easier to adjust the time windows within the context of a single...
  • Page 55 ACCQPrep® SFC Section 3 Operation If no fractions were collected during the previous steps, S also permits easier manual time window set- INGLE NJECTION tings. Figure 3-15 Adding a Third Time Window Deselecting S shows a simulation of three INGLE NJECTION injections with the third collection window.

  • Page 56: Fraction Collection With Fractionation Valve

    ACCQPrep® SFC Section 3 Operation Figure 3-17 Four Stacked Injections with Time Windows Adjusted T h e f r a c t io na t io n va lv e i s a n al t er n a te m et h od t o t h e 3.4 Fraction Collection AutoSampler fraction collector to collect peaks.

  • Page 57: Operation Troubleshooting

    ACCQPrep® SFC Section 3 Operation Then, on the C window, enter the OLLECTION EFINITION maximum fill volume for the containers used with the fraction- ation valve. "Max" is the value stored in the system configu- ration, but other values up to 5000 mL may be entered. Figure 3-19 Collection options Injection Valve Leak –...
  • Page 58 ACCQPrep® SFC Section 3 Operation No peaks on chromatogram – • No sample injected: · Sample vial empty. · Sample probe plugged, injection loop plugged, or probe or injection pump fitting loose. · Perform a dummy injection and watch injector pump to determine if fluid is being aspirated.
  • Page 59 ACCQPrep® SFC Section 3 Operation • Column not suitable for the compounds separated. • Incorrect method. Peaks elute too late – • Co-solvent not being delivered properly. Check solvent level, inspect or clean co-solvent pump check valves, confirm solvent lines in correct solvents, and look for leaks of air into the lines.
  • Page 60 In rare cases, the stator must also be replaced. Rotors and stators for ACCQPrep SFC systems are available online at https://store.teledyneisco.com. Or, contact your local Teledyne ISCO representative. 3-22 EAR99 Technology Subject to Restrictions Contained on the Cover Page...

  • Page 61: Section 4 Peaktrak

    ACCQPrep® SFC Section 4 PeakTrak PeakTrak is the software that controls the ACCQPrep SFC 4.1 Overview system. This section discusses the basic functionality of PeakTrak when operated via the touchscreen or a remote browser window. The M screen displays the current M .

  • Page 62: Method File

    ACCQPrep® SFC Section 4 PeakTrak Figure 4-1 Main screen Note The available commands and options will change according to the active window, the state of the system, and the current file. PeakTrak controls the separations performed by the system 4.1.2 Method File through a M .

  • Page 63: Run File

    Method files use a .pmtd filename extension. When PeakTrak is started, the system loads a Default Method. A Default Methods Default Method contains Teledyne ISCO’s recommended basic and advanced settings for the use of a default column (as selected on the C window).
  • Page 64 ACCQPrep® SFC Section 4 PeakTrak Figure 4-2 File Menu screen New – Opens a new method file. PeakTrak will open the window using the default program settings for the default configured column size. Open – Opens a M (.pmtd) or a R (.run) ETHOD stored on the system’s internal hard drive.

  • Page 65: Method Editor (Menu Item)

    ACCQPrep® SFC Section 4 PeakTrak Note are an exception and cannot be overwritten EFAULT ETHODS by the S command. If a D is open ETHOD EFAULT ETHOD and you attempt to save any modifications to that method, the window appears so you can rename the method file. ILES This preserves the default method.

  • Page 66: Tools Menu

    ACCQPrep® SFC Section 4 PeakTrak control your ACCQPrep SFC system: Figure 4-3 Tools menu Manual Control – Opens the M window. ANUAL ONTROL From this window, you can operate the system manually. Manual control can assist with priming or purging the internal plumbing, and aid system troubleshooting.

  • Page 67: Help

    ACCQPrep® SFC Section 4 PeakTrak • To add a user, click the A button and enter the user name in the window that appears. A Password window will appear; enter a password for the new user, or leave the text empty if no password is desired. When you add a user, a working folder for that user is automatically created.

  • Page 68: Peaktrak Windows

    ACCQPrep system software. Export Log Files – Writes operating data to a log file during system operation. Teledyne ISCO service personnel can interpret this data to optimize system performance or to troubleshoot difficulties. Teledyne ISCO recommends that you use this menu command only when advised by a qualified service technician.

  • Page 69: The Gradient Plot Area

    ACCQPrep® SFC Section 4 PeakTrak the left side of the window changes to show the collection rack map or the method parameters in a P OLLECTION pane. Figure 4-6 The Gradient Plot area Gradient Plot – Depicts the current gradient that will be used for the run.
  • Page 70 ACCQPrep® SFC Section 4 PeakTrak insert and delete points. For complete instructions on defining gradient curves, see Section 4.4.3 Defining a Gradient. The following controls appear in the Gradient Plot Area: • I — Enables the gradient point insert NSERT OINT mode.
  • Page 71 ACCQPrep® SFC Section 4 PeakTrak System Status Bar Figure 4-7 The System Status Bar The oven temperature is shown at far left beside the measured bpr presure. • In Figure 4-7 (a) it is 39.8 °C. The system pressure is the measured BPR pressure shown at the left end of the pressure gauge.
  • Page 72 ACCQPrep® SFC Section 4 PeakTrak The actual pressure at column is a derived figure. For example: 122.2 BAR (system pressure) - 100.2 (measured BPR pressure) = 22 BAR Using the measured limit to accurately calculate the maximum system pressure helps prevent damage to the column. For example, if the entry to BPR P is 100.2 BAR and the RESSURE...
  • Page 73 ACCQPrep® SFC Section 4 PeakTrak Figure 4-9 Main: Run Control buttons • S — Starts or resumes the run. After a TART ONTINUE run has started, this button is replaced by the P AUSE button. • I — Holds the %co-solvent at the current SOCRATIC value while the system continues to operate.
  • Page 74 ACCQPrep® SFC Section 4 PeakTrak Peak Collection Buttons – Three peak collection buttons are located at the bottom of the M screen. Figure 4-10 Main: Peak Collection buttons • A — Collects all eluant in the fraction collection tubes. Detected peaks will advance to the next tube automati- cally to maximise peak concentration and purity •...

  • Page 75: The Method Editor Window

    ACCQPrep® SFC Section 4 PeakTrak • Select where eluant will be collected. • View and edit the current gradient. • Set detector settings. • Save methods to Run Files for later retrieval. To open the window, select M from the P ETHOD DITOR menu at the top of the screen.
  • Page 76 ACCQPrep® SFC Section 4 PeakTrak • S — Opens the F window. From this window ILES you can rename the current method and save it on the system’s internal storage. • E — Closes the M and return to the ETHOD DITOR INDOW...
  • Page 77 ACCQPrep® SFC Section 4 PeakTrak · The BPR P limit, when combined with the RESSURE column P (Section 2.6.5), sets the RESSURE IMIT system pressure limit. Were the system to exceed its pressure limit, a hard stop would occur. · The entry to BPR P does not necessarily RESSURE dictate at-column pressure because, at any given...
  • Page 78 ACCQPrep® SFC Section 4 PeakTrak The gradient plot area also provides a convenient method to edit the gradient curve. You can click and drag any of the points to change the shape of the curve, or use the buttons at the bottom of the plot area to insert and delete points. To zoom into a portion of the graphic area, use “pinch zoom”...
  • Page 79 ACCQPrep® SFC Section 4 PeakTrak For complete instructions on defining gradient curves, see Section 4.4.3 Defining a Gradient. The gradient table depicts the points that define the gradient curve in a tabular format. From this table you can change the flow rate, the duration, and %co-solvent concentration of any point on the curve.
  • Page 80 ACCQPrep® SFC Section 4 PeakTrak Tube Volume – Allows you to specify the Tube Volume for col- lected fluids. This volume can be the default maximum volume for that tube size (Max option) as entered in the C ONFIGURATION window, or a method-specific volume less than the capacity defined by the C window.
  • Page 81 ACCQPrep® SFC Section 4 PeakTrak Figure 4-16 A Peak Detection settings window options and their settings: Peak Detection options ETECTION •  and  (wavelength 1 and 2) — Instruct the system to use and allow you to configure primary and secondary wavelength detection.
  • Page 82 ACCQPrep® SFC Section 4 PeakTrak · T — When selected, enables threshold HRESHOLD peak detection. Peaks will start when the detector signal exceeds the programmed value. The peak will end when the detector signal drops to .01 AU below the programmed value. This reduces the potential of multiple peaks if a noisy signal oscillates around the threshold value.
  • Page 83 ACCQPrep® SFC Section 4 PeakTrak differing times as a purity measurement. It also allows fractionation on the basis of spectral purity. · S — Allows fractionation PECTRAL URITY ETECTION on the basis of spectral purity. · T — Works similarly to the T HRESHOLD HRESHOLD setting for ...
  • Page 84 ACCQPrep® SFC Section 4 PeakTrak · F info scroll box — Lists the contents of OLDER the current folder. The contents can be sorted by clicking the column headings. · F — When shown, limits the display to certain types of files. Select the desired file type from the list.

  • Page 85: Manual Control Settings - Quick Cleaning

    ACCQPrep® SFC Section 4 PeakTrak Manual Control can assist with method development, mainte- 4.3.6 Manual Control nance of the system plumbing, and system troubleshooting. The window can be opened by selecting ANUAL ONTROL > M from the P menu. OOLS ANUAL ONTROL Figure 4-17...

  • Page 86: Examples Of Peaktrak Actions

    ACCQPrep® SFC Section 4 PeakTrak • P – The percentage of ERCENT XX SOLVENT co-solvent pumped with CO • S – Stops the pump. This button is only active while the pump is running. The raw lamp energy display can be used to verify flow cell clean- liness.
  • Page 87 ACCQPrep® SFC Section 4 PeakTrak Editing a method allows you to tailor the operation of the 4.4.1 Editing a Method ACCQPrep SFC system to best separate or purify the compounds of interest. PeakTrak has two types of method settings: basic and advanced. The basic settings allow you to control the %co-solvent gradient Basic Method Settings mix, flow rate, solvents, and run length.
  • Page 88 ACCQPrep® SFC Section 4 PeakTrak 4. Enter more time windows as needed. You can define up to six time windows. • P — There are three peak collection OLLECTION options: A , or N EAKS · The A option will collect peak and non-peak fluid in tubes.

  • Page 89: An Alternative Way To Create Method Files

    ACCQPrep® SFC Section 4 PeakTrak See Section 4.3.2, Peak Detection options for more information about peak detection settings. Some useful method options are described below: •  and  (wavelength 1 and 2) — Enable these options to use and configure primary and secondary wavelength detection.

  • Page 90: Real-Time Gradient Editing

    ACCQPrep® SFC Section 4 PeakTrak The above methods work in the M window and M ETHOD window. Alternatively, you can modify, add, insert, and DITOR delete points using a tabular view on the M ETHOD DITOR window. Click the E button to open this view, then RADIENT use the controls to modify the settings.

  • Page 91: Viewing Runs

    ACCQPrep® SFC Section 4 PeakTrak pounds, the changing ratio during the detected peak would reveal the impurity. Therefore, one can aassume that if the ratio is not constant for the entire duration of the peak, the compound that is eluting may not be pure. The following controls can be found on the P URITY EASURE...
  • Page 92 ACCQPrep® SFC Section 4 PeakTrak remote personal computer, you can save the summary to any connected storage device. If you are attempting to save a PDF file from the touch panel display, insert a USB Flash drive in the USB port below the display panel.

  • Page 93: Manual Control Of The Accqprep Sfc

    ACCQPrep® SFC Section 4 PeakTrak following: · The red absorbance trace produced by the system’s peak detector. Absorbance units (also shown in red) that correspond to this trace are shown on the left Y-axis. · Purple absorbance and green purity measurement traces.
  • Page 94 ACCQPrep® SFC Section 4 PeakTrak Depending on what you are doing with the M ANUAL ONTROL functions, low lamp energy could indicate normal operation. For example, a UV-absorbing compound could be present in the flow cell as you are pumping solvent, or the selected solvent absorbs UV light at 254 nm.

  • Page 95: Section 5 Maintenance

    ACCQPrep® SFC Section 5 Maintenance This section will cover some common maintenance routines for 5.1 Introduction the ACCQPrep SFC system. To clean the exterior surfaces, use a cleaning cloth dampened 5.1.1 Cleaning with a mixture of distilled water and a mild detergent. Use iso- propyl alcohol for tougher stains.

  • Page 96: Tubing Inspection

    ACCQPrep® SFC Section 5 Maintenance WARNING As long as the AC mains power cord is connected and rear circuit breakers are in the ON position, power is inside the unit. The mains power cord is the disconnect device. Position the ACCQPrep system so that the power cord can be unplugged, or use a power strip where the plug can quickly be removed from the outlet in the event of an emergency.

  • Page 97: Preventive Maintenance

    . A P r e v e n t i v e M a i n t e n a n c e K i t Maintenance (PN 60-5267-020) is available from Teledyne ISCO for this purpose.

  • Page 98: Flow Cell Cleaning

    ACCQPrep® SFC Section 5 Maintenance 5.4 Flow Cell Cleaning As a preventive measure, all default column methods finish the 5.4.1 Post Separation separation run with a high percentage of co-solvent (Figure 5-1). This brief time (one to six column volumes) of strong solvent flushes residual compounds from the column, flow cell, and internal tubing.

  • Page 99: Flow Cell Cleaning When Recommended

    ACCQPrep® SFC Section 5 Maintenance CAUTION Do not use polar, basic solvent systems with silica column media. These solvent systems may break down the silica structure, possibly causing obstructions in the flow path. Examples of such solvent systems include, but are not limited to, those containing more than 20% methanol with ammonium hydroxide.

  • Page 100: Manual Control Settings - Quick Cleaning

    ACCQPrep® SFC Section 5 Maintenance To perform a quick cleaning after clicking the C ANCEL button: 1. Install a union in one of the column positions. Correctly installed, this turn that position into a bypass. Note You can rename the column position using T >...

  • Page 101: Accqprep Sfc Maintenance

    ACCQPrep® SFC Section 5 Maintenance CAUTION Choosing the wrong column position in Step 4a could cause the solvent mixture to be pumped through a column. If the mix- ture is incompatible with the column, it could be damaged. 6. Set the P to 5% and press ERCENT OSOLVENT...

  • Page 102: The Injection Valve Rotor Assembly

    ACCQPrep SFC system and includes Valve Rotor the rotor for this procedure. Note For other parts for your ACCQPrep SFC system, visit https://store.teledyneisco.com, or contact your local Teledyne ISCO representative. 2. Do a system vent. Select T > M > OOLS ANUAL ONTROL ).

  • Page 103: Column Select Valve Rotor Replacement

    ACCQPrep® SFC Section 5 Maintenance Figure 5-5 Rotor thumbscrew removal 5. Locate the rotor inside and slip out by using a magnet. 6. Make note of marking on rotor, as it needs to go back in the same orientation. · Use a marker to mark the front face of the rotor or make note of the embossed letter on the rear edge of the rotor, as it needs to go back in the same orien- tation.

  • Page 104: Removing The Rotor Cap

    ACCQPrep® SFC Section 5 Maintenance 4. Access the column oven module. Using a 5/8" open-faced wrench (or adjustable open-faced wrench) to loosen the rotor cap. Figure 5-6 Loosening the rotor cap 5. Finish removing the rotor cap by hand. Figure 5-7 Removing the rotor cap 6.

  • Page 105: Fractionation Valve Rotor Replacement

    ACCQPrep® SFC Section 5 Maintenance Figure 5-9 Tightening the new rotor 8. Test new rotor by running the unit in Manual Control and verifying that there is flow to each column position without leaking or over-pressurization errors. Failure of the fractionation valve rotor requires its removal, 5.5.4 Fractionation Valve cleaning or, potentially, its replacement.

  • Page 106: The Fractionation Valve Mounted (Left) And Removed (Right)

    ACCQPrep® SFC Section 5 Maintenance Figure 5-11 Control modules case top 5. Remove fractionation valve bracket by removing the two nuts that secure its mounting bracket to the side of the chassis. Use a 5/16" nut driver or wrench. Be sure to unplug the USB and power connectors as well, noting their locations.

  • Page 107: Removal Of The Fractionation Valve Stator

    ACCQPrep® SFC Section 5 Maintenance Mounting clip Stator Valve Body Rotor Figure 5-14 Removal of the fractionation valve stator 8. Slip out the rotor from the valve. This may require the use of needle-nose pliers or another tool, but take care not to scratch any surfaces of the valve.

  • Page 108: Autosampler Maintenance

    ACCQPrep® SFC Section 5 Maintenance 10. Line up the stator face with the 1 port near the 12 o’clock position. The stator face will not go into position unless the offset mounting pins are aligned. Figure 5-17 Reinstallation of the fractionation valve stator 11.
  • Page 109 ACCQPrep® SFC Section 5 Maintenance Figure 5-19 The peristaltic pump at the back of the AutoSampler 1. At the pump: push the levers at the top and bottom of each tube retaining clip, then pull the clips out (Figure 5-20). Figure 5-20 Removing a retaining clip 2.
  • Page 110 ACCQPrep® SFC Section 5 Maintenance Figure 5-22 Removing the tubing 4. Install the new peristaltic tubing with the thicker tubing towards the AutoSampler. · Install the new peristaltic tubing with the 3.2 mm ID tubing (thicker) towards the AutoSampler (ports labeled 2 and 4).

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