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Pickering Laboratories Pinnacle PCX Operator's Manual

Post-column derivatization instrument
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O
M
peratOr
anual
Post-Column
Derivatization
Instrument
1280 Space Park Way
Mountain View
CA 94043
USA
800-654-3330 • 650-694-6700
650-968-0749
fax
www.pickeringlabs.com
support@pickeringlabs.com
http://pickeringlabs.blogspot.com
Cat. No. 0101-0008
Version 10, April 2016
Copyright © 2005 by Pickering Laboratories, Inc. All rights reserved. No Portion of this manual or
any artwork contained herein may be reproduced in any shape or form without the
express written consent of Pickering Laboratories, Inc.

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Summary of Contents for Pickering Laboratories Pinnacle PCX

  • Page 1 Cat. No. 0101-0008 Version 10, April 2016 Copyright © 2005 by Pickering Laboratories, Inc. All rights reserved. No Portion of this manual or any artwork contained herein may be reproduced in any shape or form without the express written consent of Pickering Laboratories, Inc.

  • Page 3: Table Of Contents

    Reservoir Tray / Bottles Fluidics Panel Quick Change Reactor Detector Connections Pump Compartment Gas Manifold Display Module 2.10 Electronics Compartment 2.11 Back Panel 2.11 Safety Features in the Pinnacle PCX 2.13 Standard Configurations of Pinnacle PCX 2.14 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 4 Installation Section 3 Site Requirements Instrument Unpacking and Preparation Unpacking Gas Connections to Back Panel of Pinnacle PCX Computer Connections Software Installation Pump and Autosampler Connections Eluant Priming 3.10 Column and Guard Installation 3.10 Detector Connections 3.11 Reservoir Connections 3.12 Reagent Pump Preparation 3.13...
  • Page 5 Procedure 6.2-5 Sample Chromatograms and Gradient Programs 6.2-6 Precautions 6.2-18 Carbamates Introduction Background Basic Sample Preparation 6.3-2 Reagent Preparation 6.3-3 Post-Column Conditions 6.3-5 Analytical Procedure 6.3-5 Sample Chromatograms and Gradient Programs 6.3-5 Precautions 6.3-12 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 6 6.4-4 Analytical Procedure 6.4-4 Sample Chromatograms 6.4-5 Precautions 6.4-6 Troubleshooting Section 7 Contact Pickering Laboratories For Support Instrument Parameter Log General Troubleshooting Advice Common System Problems Common Chromatography Problems Common Column Problems Application Specific Troubleshooting • Amino Acids • Carbamates •...
  • Page 7 Appendices Installation/Operational Qualitication of the Pinnacle PCX Installation/Operational Qualitication of the Pinnacle PCX Data Sheet Performance Qualifications of the Pinnacle PCX Data Sheet Sample Instrument Parameter Log 8.15 Flow Diagram – Simplex 8.16 Flow Diagram – Duplex 8.17 Parts List for Pinnacle PCX 8.18...
  • Page 8 Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 9: Read This

    The Pinnacle PCX manual is designed to contain all of the information necessary for the installation, operation, maintenance and troubleshooting of the Pinnacle PCX. It is designed to contain any and all information that you may require during the lifetime of your Pinnacle PCX.
  • Page 10 Read this First! Before attempting to install the Pinnacle PCX post-column derivatization instrument, it is vitally important that you read this manual first, and attend to site, HPLC, and accessories requirements: HPLC – Page 5 Gas Supply Requirements – Page 5 Reagent Reservoir bottles –...
  • Page 11 120 VAC +/- 10%, 240 VAC +/- 10% 5 A maximum at 108 VAC 47 – 63 Hz Installation over voltage category: Pinnacle PCX complies with Class B Emission Test Specifications. Fuses 2 ea, 5mm x 20 mm, 6 A, time lag Backlit, positive mode, high contrast, viewing area –...
  • Page 12 Minimum 3 inches clearance at back of instrument for venting. Note: Space quoted above is for Pinnacle PCX. The total space requirement depends on the brand and model of HPLC. Electrical Outlet One grounded outlet must be provided for the Pinnacle PCX. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 13 Outlet of regulator must connect to 1/8” OD tubing Reagent Reservoir Bottles The Pinnacle PCX includes one pressurized reagent reservoir for the one reagent system and two for the two reagent system. Note: For your safety, the bottles are coated with a tough plastic film and rated to a maximum of 15 psig (1 bar).
  • Page 14 Pressure rating of flow cell must be > 110 psi Inlet capillary must be > 0.17 mm ID MISCELLANEOUS SUPPLIES For Amino Acid analysis, a Dead-Head kit is required. This can be purchased from Pickering Laboratories. Chemistry The user must check the chemistry requirements for the specific application.
  • Page 15 (see application section for cat. nos.) B: UV – Visible detection • DI Water • TRIONE Ninhydrin reagent (cat. no. T1OOC or T200) ® • Pickering sodium or lithium elution buffers (see application section for cat. nos.) Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 16 Notes Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 17: What Is Post-Column Derivatization?

    The Pinnacle PCX post-column derivatization instrument automatically mixes the stream of effluent flowing from the HPLC column with a stream of reagent solution. The mixture flows through a reactor to allow enough time for the chemical reactions to complete.

  • Page 18: Design Of A Hplc System

    Design of a HPLC system This next section is a simplified view of a HPLC, followed by the ideas behind a post-column system. This section is intended to help novice HPLC operators. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 19 Actually, the column does more than separation; it creates a back- pressure. It is the combination of the pulse dampener and the column that creates a smooth baseline. (Figure 1-3) Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 20: Designing A Post-Column System

    The same principals that are used in HPLC can be applied to the post-column system. What happens if we simply add a post-column pump, a mixing tee, and a reactor? The periodic noise returns to the baseline (created by the post-column pump; Figure 1-4). Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 21 However we do not need to invent anything new; we just need a pulse dampener and a column. In the generation of Post-column systems prior to the Pinnacle PCX, the restriction performed by the column was achieved using a Restrictor, which is packed with very inert material. With this “flow conditioner” in place, the baseline is now acceptable.

  • Page 22: Design Of The Pinnacle Pcx

    Design of the Pinnacle PCX The Pinnacle PCX has taken the post-column system to a new level. The introduction of a syringe pump has eliminated the need for a pulse-dampener and restrictor by: • The Pickering syringe pumps complete a filling cycle prior to the injection of a run, and deliver reagent during the run at a constant rate.

  • Page 23: Background 6

    Reservoir Tray / Bottles Fluidics Panel Quick Change Reactor Detector Connections Pump Compartment Gas Manifold Display Module 2.10 Electronics Compartment 2.11 Back Panel 2.11 Safety Features in the Pinnacle PCX 2.13 Standard Configurations of Pinnacle PCX 2.14 Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 24: Introduction

    TO DETECTOR HPLC Flow Path – Dual Pump Figure 2-2 The flow path of the Pinnacle PCX is extremely inert, FILTER COLUMN rendering it very versatile. The same instrument can be used for many different applications, and will tolerate a...

  • Page 25: Check Valve

    Fast column cooling is assisted by the introduction of fresh air flow into the chamber by means of two fans that are controlled by the Pinnacle PCX control software. The temperature range holds within ± 1˚C resolution from 5˚C above ambient to 75˚C. A temperature gradient...

  • Page 26: Reagent Pump

    The pump contains a piston wash for extended seal life. The piston wash is automatically performed with the movement of the piston. For purposes of fast refill and flushing, the pump can refill or dispense (to waste) at 55 ml/min. Syringe pump cylider Figure 2-4 Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 27: Reagent Valves

    Change Wash and Flush solutions at least once a week to prevent contamination. The pressurized reagent reservoir serves two purposes: It protects air-sensitive reagents from oxidation. Figure 2-6 It helps the syringe pump fill consistently and quickly by providing a source of pressure. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 28 10 psig (0.7 bar). No utilice botellas sin recubrimiento. Avvertimento. Per la sua protezione, le bottiglie sono construite forti con un percentuale du plastica, e sono usabili per un massimo di 0.7 Bar (10 psi). Non usare bottiglie normali. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 29: Fluidics Panel

    Section 2 verview There are three types of Reservoir/Cap assemblies used on the Pinnacle PCX: 1) Reagent Reservoir is 1L, 45-430, safety-coated. These are shipped with blue caps with white valve assembly. These can be pressurized. 2) The wash Reservoir is 1L, 38-430, clear glass. These are shipped with caps with 1ea 1/4” opening and 2ea 1/8”...

  • Page 30: Quick Change Reactor

    The reactor can be easily switched if it becomes blocked or if a different volume is required. The electronics of the reactor are contained within the Pinnacle PCX, making Figure 2-9 replacement affordable and easy. Volumes ranging from 0.15 ml to 3 ml are available. The most commonly used volumes are available off the shelf, but if you require a volume that is not in our price list, we can make it for you.

  • Page 31: Pump Compartment

    Gas Manifold The “Gas Inlet” fitting is a 1/4-28 fitting located on the back panel of the Pinnacle PCX (reference fig 2-15). The inert gas source is connected via a 1/8” OD Air Barrier tubing, and the pressure is regulated to 5psi before pressurizing the reagent reservoirs.

  • Page 32: Display Module

    The STOP LED will illuminate when the Pinnacle PCX has been stopped manually by the user. When STOP is pressed, the LED will glow red, indicating that there has been an emergency manual stoppage. To reset the instrument after emergency stop, turn instrument OFF and then turn it back ON.

  • Page 33: Electronics Compartment

    Fuses Power Switch and Main Fuse Vents and other openings COMMUNICATION PORTS Figure 2-15 USB Port The USB port on the Pinnacle PCX connects directly to one of the USB ports on the computer. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 34 The relays will be explained in the operations chapter under Site Requirements. Ethernet Port This port is used for connecting the Pinnacle PCX to a network. POWER SWITCH AND MAIN FUSE The power connector is a standard IEC 320 type connector. Use the appropriate power cord for your local wall outlet and electrical code.

  • Page 35: Safety Features In The Pinnacle Pcx

    2.13 Section 2 verview Safety Features in the Pinnacle PCX The Pinnacle PCX system has features designed into the instrument and operation that will prevent reagent back-flow onto the column and bursting of reactor tubing due to Over-pressure relief valve a blockage.

  • Page 36: Standard Configurations Of Pinnacle Pcx

    , reagent reservoirs, gas manifold, Air Barrier gas tubing, and other accessories. The Pinnacle PCX includes one pressurized reagent reservoir for the one-reagent system and two for the two- reagent system. The instrument also includes a 1L wash bottle and a 1L flush bottle for the piston wash and flush feature.
  • Page 37 Installation Checklists (see Appendix) The Pinnacle PCX instrument is shipped in one carton. Application Kits may be shipped in one or more cartons each. Report any carton damage to the carrier. Unpack all cartons and review the contents using the Packing List to ensure that your order is complete.

  • Page 38: Site Requirements

    The minimum bench space does not include the HPLC system. The total space requirement depends on the brand and model of HPLC. For most cases, it is best to place the LC pump and injector system on the left side of the Pinnacle PCX, and the detector on the right.
  • Page 39 Reagent 1, Nitrogen must be used to prevent out-gassing. ® A waste container should be provided for the waste lines from the Pinnacle PCX and the HPLC detector. HPLC SYSTEM REQUIREMENTS Since every HPLC is different, the following procedure has been generalized. Before attempting to connect any tubing, examine the HPLC setup, and determine the best possible means of making the connections.

  • Page 40: Instrument Unpacking And Preparation

    For HPLC systems other than Agilent 1100, or 1200, the Software and system must be capable of sending a relay signal to an external piece of equipment to achieve synchronization. Chemstation version 9.0 or higher is needed for Agilent 1100 or Agilent 1200. Pinnacle PCX software will communicate with Chemstation directly – no relay connection is needed.

  • Page 41: Gas Connections To Back Panel Of Pinnacle Pcx

    Ensure that there is enough room to open the column oven door and the fluidics door. Ensure that there is at least 3 inches clearance between the outlet vent at the back of the Pinnacle PCX and any walls or other instruments. This is very important for proper cooling of the column oven.

  • Page 42: Computer Connections

    Check for leaks at the Gas Inlet connection, and check that there is gas flowing out of the 1/8" tubes. Switch the toggle valve OFF. Slide the Pinnacle PCX into place on the bench. Allow a minimum of 3 inches of space for venting at the back of the instrument. Computer Connections RELAY CONNECTIONS Relay Input Connector can be used to trigger Pinnacle PCX operations.
  • Page 43 Connecting the Pinnacle PCX to the network It is at the user’s discretion if they would like their Pinnacle PCX placed on their company network. This will involve working closely with the Company’s IT personnel, to determine proper address and their network security procedures.

  • Page 44: Pump And Autosampler Connections

    Open the prime-purge valve on the HPLC. Purge each line in the system with a water/methanol mixture to flush the system. Set the flow rate to the maximum and purge at least 25 ml through each line. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 45 Connect the outlet of the injector to the Check Valve assembly. Use 0.011" ID tubing and a PEEK nut and ferrule. (PNs 1452-0118, 1452-0117, 2104-0210, 1452-0226) Place the open end of the check valve tubing into a beaker. Flush line from injector for 5 minutes at 1 ml/min with 80/20 Water/Methanol. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 46: Eluant Priming

    When liquid exits the guard column, connect the from HPLC Column “column connector/coupler” provided in the packing Blue Peek Tubing kit. When liquid exits the connector, connect the PEEK Nut PEEK Nut Check Valve (3101-0011) (1452-0226) (3106-1007) Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 47: Detector Connections

    Set the time constant on the detector to 2–4 seconds. The pressure rating of the detector flowcell must be >110 psi (7.5 bar). If your detector flowcell is rated lower, consult Pickering Laboratories. Special Note to Hewlett-Packard 1046A end-users: Replace the 0.12 mm ID inlet tubing (red) and heat- exchanger from the left side of the detector to the flowcell (behind the front panel of the detector) with a 0.25...

  • Page 48: Reservoir Connections

    REAGENT RESERVOIR CONNECTIONS Connect 1/8" Air Barrier lines from “Gas Supply OUT” port on the back of the Pinnacle PCX to the CHECK VALVE on the top of the reagent cap. Use a 1/4-28 Nut and ferrule (PN 3101-0005 and 3101-0006). Don’t over tighten! Connect 1/8"...

  • Page 49: Reagent Pump Preparation

    Ensure that the Flush and Piston Wash lines are immersed in liquid. The Pinnacle PCX has a maximum of two waste lines that must be fed into a waste container. They can either be fed into a separate container, or into the waste stream of the HPLC. These are the 1/8" OD clear FEP tubes that are connected to the Waste port (No.

  • Page 50: Running A Chromatogram

    Equilibration time should be at least 5 min long to give Pinnacle PCX enough time to refill between the runs. If using relays to synchronize with Pinnacle PCX set up relay signal at time 0.0 in the HPLC method.

  • Page 51: Shutdown

    The Pinnacle PCX must be flushed out at the end of a series of injections, and the reactors must be cooled down. If the instrument is simply stopped, with reagent inside the reactor in a hot state, with no movement, then the heated reactor will become blocked.
  • Page 52 Time (min) % Storage Eluant Flow (ml/min) Analytical flow rate* Analytical flow rate* 30.1 0.0 or 0.02mL/min *Follow instructions that come with the column. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 53: Software Overview

    4.17 Software Overview Pinnacle PCX can be controlled only with PC using Pinnacle PCX software. The system can be connected to PC through USB or Ethernet cable. Pinnacle PCX software controls column and reactor heaters, electronic valves and pumps. It allows to create, store and run post-column methods and sequences.

  • Page 54: Status Window

    Status Window The Status window is the main screen of the Pinnacle PCX software (Figure 4-1). The Status window can be moved, or minimized into an icon at the bottom of the PC screen. It has a menu bar on the top, status bar at the bottom and icons for the Pinnacle PCX components.
  • Page 55 Stop: This will stop the instrument. It does not matter what task the instrument is performing when this is pressed. The Pinnacle PCX will stop whatever it is doing and will not resume until the user has Reset the system.

  • Page 56: Menu Options/Functions

    PeratiOn Menu Options/Functions FILE Import/Export exports existing methods and sequences into a file. The file then can be imported to another instance of the Pinnacle PCX software. Exit closes Pinnacle PCX software. CONTROL Enable selecting Enable will cause the reactor and column heaters to begin heating. This will not start the pumps.
  • Page 57 Pinnacle PCX finishes current run then stops the pump(s) and turns the heaters OFF. Pause sequence this option allows the Pinnacle PCX to finish current run and then stops the pump(s). It leaves the heaters ON. The sequence will continue after Resume Sequence is selected.

  • Page 58: Configuring Your Pinnacle Pcx

    More Tab: HPLC type: Select the brand of HPLC that you will be using with Pinnacle PCX. This will determine the type of synchronization between Pinnacle PCX and HPLC system.

  • Page 59: Log Files

    HPLC are all stored for 3 days before being overwritten. Log files are necessary to troubleshoot Pinnacle PCX system and software and should always be collected after a problem is detected. To collect Log files go to Help, select Send Log to Support and select file from the day the problem happened.
  • Page 60 Pinnacle will use this information for analysis. The items marked with * indicate required parameters. *Run Time, min In this window, enter the total run time for the Pinnacle PCX method. This must be a whole number, greater than 1 *Equilibration Time, min Enter the time between runs.
  • Page 61 This tab allows you to designate currently open method as a Flush Method (figure 4-4). This method can be set as a last method in the Pinnacle PCX sequence in order to flush the reagent pumps and the Pinnacle PCX reagent lines and reactor.

  • Page 62: Creating And Editing Sequences

    Match analysis time to Run time of the Pinnacle PCX and match time of the equilibration step to Equilibration time of the Pinnacle PCX. Creating and Editing Sequences To create or edit a post-column sequence select Sequence then Edit/Delete.

  • Page 63: Tutorials

    CREATE A METHOD The following is a tutorial on how to create a method and start a run on the Pinnacle PCX. It is not intended to be used for a real run because the flow rates and temperatures are not representative. If you like, you may use this tutorial as a guide to create your own methods.
  • Page 64 Type a Name for your method. For this example, type “Tutorial”, and click OK. The Pinnacle PCX software has now added the method “Tutorial” to the list of available methods. Highlight this method if it is not already done so.
  • Page 65 Type a Name for your Sequence. For this example, type “Tutorial 1” and click OK. The Pinnacle PCX software has now added the Sequence “Tutorial 1” to the list of available sequences. Highlight this sequence if it is not already done so.

  • Page 66: Running Post-Column Analysis Using Pinnacle Pcx

    The number of Runs should match the number of runs you plan to make on the HPLC using that method. In this example, your system will perform 3 injections using the Pinnacle PCX method “Tutorial”. The sequence table on your HPLC system should also have 3 injections programmed.
  • Page 67 PcX O innacle PeratiOn Create sequence for Pinnacle PCX using your post-column method(s). Set up the same number of runs as in the HPLC sequence. Select Save to save Pinnacle PCX sequence. Select Load to load Pinnacle PCX sequence. Sequence name and the first method name will appear in the status bar at the bottom of the Pinnacle PCX software.
  • Page 68 5 min before the end of the Equilibration time. Once next injection signal is received Pinnacle PCX starts the second method in the sequence. The number of the current run and total number of runs in the Sequence are shown on the bottom of the Pinnacle PCX software.

  • Page 69: Stop/Reset Pinnacle Pcx

    In a case of an emergency there are two ways of stopping Pinnacle PCX: On the front of the instrument press STOP button. To reset turn the instrument OFF and ON again. In the Pinnacle PCX software select STOP. Once selected this option changes to RESET. Select RESET once the emergency is cleared.
  • Page 70 4.18 Section 4 PcX O innacle PeratiOn AUTOMATIC SHUTDOWN Create a Shutdown Method for Pinnacle PCX using the following settings as an example: Run time: 30 min Equilibration time: 5 min Reactor temperature: 35 C Column temperature: 35 C Pump(s) flow rate: 0 mL/min Set it up as the last method in the Pinnacle PCX sequence.

  • Page 71: Maintenance Suggestions

    Create a maintenance schedule for your laboratory to ensure that the instrument is kept in good working order. Always use PEEK nuts and ferrules in the Pinnacle PCX fluidics lines. Use of stainless steel nuts and ferrules in the PEEK ports will void the warranty. Stainless steel nuts and ferrules will cut the threads at the bottom of the ports, causing them to leak.

  • Page 72: Operating Suggestions

    1) Always wear safety glasses or goggles, laboratory coat, gloves, and other appropriate safety-clothing. 2) Read and understand the instructions in the MSDS’s shipped with the chemicals. If the MSDS’s are missing, please contact Pickering Laboratories and we can fax you a copy, or you can download them from our website at www.pickeringlabs.com.

  • Page 73: Proper Shutdown Procedures

    The Pinnacle PCX must be flushed out at the end of a series of injections, and the reactors must be cooled down. If the instrument is simply stopped, with reagent inside the reactor in a hot state, with no movement, then the heated reactor will become blocked.
  • Page 74 LONG-TERM SHUTDOWN The above methods are used if the Pinnacle PCX will be used again within 3 days of the last run. If you plan to not use the Pinnacle PCX for more than 3 days, we recommend that you use the Long-term Shutdown.
  • Page 75 Select Instrument – Maintenance- Flush Instrument. Follow directions on the screen to complete this procedure. After Flush Instrument is completed select Disable function in the Control menu of the Pinnacle PCX software to turn OFF heaters and pumps. Allow the HPLC to pump at least 30 minutes to allow for the reactor to cool.

  • Page 76: Basic Maintenance Procedures

    Section 5 aintenance Select Refill Pump(s) from Control menu of the Pinnacle PCX software. This will flush the reagent lines from the bottles from the remaining reagent. Select in the Pinnacle PCX software Instrument – Maintenance – Prepare for Storage/Shipping. Follow directions on the screen to complete the procedure.

  • Page 77: Reagent Filter(S) Replacement

    Simplex system. They are located in the reagent manifolds; Items 6 and 8. Reagent Filter 1. Be sure that the Pinnacle PCX is shut down and depressurized before changing a filter. 2. Remove the 1/16" fitting from the inlet of the reagent filter.

  • Page 78: Ambient Reactor Replacement

    Do not overtighten. The inlet tubing of the heated reactor is marked with a piece of black shrink tube and connects to mixing manifold I (Item 8). Start the LC pump and inspect for leaks. Figure 5-4 Retaining Screw Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 79: Valve Maintenance

    When the flush is complete, pull the Flush tubing out of the liquid to prevent siphoning of the liquid back into the flush line. Power down the Pinnacle PCX and turn the power back on again. This will move the valve to the blocked position. This is important for alignment of the new or repaired valve face.
  • Page 80 Push the 5 new Size 4 O-rings into the ports of the PEEK ring. Port 6 (Waste port) does not have an O-ring. Figure 5-9 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 81 Ensure that the V is between ports 2-3 (that is, ensure that the spool is in the home blocked position) refer to figure 5-10. Push the valve face firmly against the Pinnacle PCX. Ensure that the Valve Spool is firmly pushed against the motor mount.

  • Page 82: Pump Seal Replacement

    Pump Seal Replacement The Pinnacle PCX uses Pickering’s own pulse-free syringe pump with piston wash. The pump is specially designed for extended seal life, however the piston seals will require periodic replacement. The length of service to be expected from the seal depends on a wide variety of factors, including whether proper shutdown procedures were followed, how often the system was turned on and off, and whether the piston-wash system was wetted.
  • Page 83 Loosen and remove the third top screw. Use caution as this will cause the pump to lean toward you. Brace the pump toward the wall of the Pinnacle PCX to prevent damage. Carefully remove the pump from the chassis. If it is Pump 1, tilt the back end up and remove the pump in a vertical position.
  • Page 84 Note: Do not over tighten cap screws. Over tightening will strip the threads on the PEEK piston head. Rinse with DI water and reassemble the Piston Head using the new O-ring and cap screws. Set the reassembled Piston Head Unit aside until Pump Reassembly. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 85 Once it is centered, tighten the set screw. Tighten the set screw so that the syringe is tight against the base of the pump. Figure 5-18 Finally, tighten the cap screws using the 3/16" alan wrench. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 86: Fuse Replacement

    REPLACE THE PUMP IN THE PINNACLE PCX Replace the pumps in the Pinnacle PCX by following the reverse of the directions in section titled “To Remove the Pump From Pinnacle PCX” on page 5.12. Be sure that the body of the pump rests on the support brackets, and that the front of the pump is protruding through the front of the chassis.
  • Page 87 5.17 Section 5 aintenance 1100-0500 Tubing Kit, Pinnacle, Dual Pump TRANSDUCER 2 COLUMN PUMP 2 VALVE 2 FILTER AMBIENT HEATED REACTOR REACTOR TRANSDUCER 1 FILTER PUMP 1 VALVE 1 WASTE TO DETECTOR FROM HPLC Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 88 5.18 Section 5 aintenance 1100-0501 Tubing Kit, Pinnacle, Single Pump COLUMN FILTER HEATED REACTOR VALVE 1 PUMP WASTE TO DETECTOR FROM HPLC Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 89 Section 6 pplicAtions Section 6 ppliCatiOns AMINO ACIDS CARBAMATES GLYPHOSATE Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 90: Reagent Preparation 6

    (reduction of interference) leading to lower detection limits. The Pickering Laboratories Pinnacle PCX was developed to facilitate the determination of amino acids in using sodium ion-exchange or in native samples using lithium ion-exchange columns. There are two options for post-column detection of amino acids.
  • Page 91 440nm. The ninhydrin reaction is carried out at 130°C with a reactor volume of 500 µl. The elevated temperature is required because at room temperature, the ninhydrin reaction is very slow and takes hours to go to completion. Figure 6.2-A Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 92 OPA. This technique has some disadvantages, and is not often used. Contact Pickering for details. The Pickering Pinnacle PCX derivatization instrument for fluorescent detection of amino acids is similarly designed to the ninhydrin instrument, except that it contains a 150 µl reactor and the reacton is carried out at 45°C.

  • Page 93: Reagent Preparation 6

    T200: To prepare two-part TRIONE (Cat. No. T200), pour Bottle 1 into the reservoir, add Bottle 2 to the ® reservoir, and cap tightly under Nitrogen. Swirl until homogeneous. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 94: Post-Column Conditions 6

    7. Replace the cap and close the vent valve. Gently swirl the reagent to complete the mixing. Turn on the inert gas. Note: OPA reagent is sensitive to air oxidation and will degrade over time. The Pinnacle PCX system is designed to minimize this oxidation.

  • Page 95: Procedure 6

    Ambient Procedure Pickering Laboratories recommends different gradient conditions depending on the column and type of sample. Use the program recommended on the column data sheet for the initial testing. Do not change this program until you are sure that the other aspects of the system are functioning properly.

  • Page 96: Sample Chromatograms And Gradient Programs 6

    11 Glutamine 23 Cystathionine 35 Hydroxylysines 12 Sarcosine 24 Isoleucine 36 Ornitine *Internal Standard NOTE: This method utilizes column temperature gradient. Use Pinnacle PCX column oven or HPLC column oven with temperature gradient capabilities. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 97 20. Cystine 32. Tryptophan 44. α-Amino-β 9. Aspargine 21. Methionine 33. Ethanolamine guanidinopropionic acid 10. Glutamic acid 22. Cystathionine 34. Hydroxylysines 45. Arginie 11. Glutamine 23. Isoleucine 35. Ammonia 12. Sarcosine 24. Leucine 36. Creatinine Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 98 21 Methionine 32 Ethanolamine 43 Glucosaminic Acid* 11 Glutamine 22 Cystathionine 33 Ammonia *Internal Standard NOTE: This method utilizes column temperature gradient. Use Pinnacle PCX column oven or HPLC column oven with temperature gradient capabilities. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 99 20. Cystine 32. Tryptophan 44. α-Amino-β- 9. Aspargine 21. Methionine 33. Ethanolamine guanidinopropionic acid 10. Glutamic acid 22. Cystathionine 34. Hydroxylysines 45. Arginie 11. Glutamine 23. Isoleucine 35. Ammonia 12. Sarcosine 24. Leucine 36. Creatinine Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 100 GUARD COLUMN: GARD COLUMN TEMP: 38°C HPLC FLOW RATE: 0.35ml/min REAGENT FLOW RATE: 0.3ml/min INJECTION VOLUME: 10ul Time (min) %Li275 %Li750 %RG003 Comment Inject Linear gradient 25.1 Step gradient Isocratic 30.1 Step gradient Re-equilibration Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 101 24 Trans-4-Hydroxy-L-Proline Alanine 16 Lysine 25 D,L & allo-Hydroxylysine Cystine 17 Histidine Valine 18 Ammonia NOTE: This method utilizes column temperature gradient. Use Pinnacle PCX column oven or HPLC column oven with temperature gradient capabilities. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 102 HPLC FLOW RATE: 0.6ml/min REAGENT FLOW RATE: 0.3ml/min INJECTION VOLUME: 10ul HPLC PROGRAM COLUMN OVEN PROGRAM Time % Na315 % Na425 % Na640 % RG011 Time Temp ºC 15.0 16.0 31.0 31.1 33.0 33.1 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 103 HPLC FLOW RATE: 0.6ml/min REAGENT FLOW RATE: 0.3ml/min INJECTION VOLUME: 10ul HPLC PROGRAM COLUMN OVEN PROGRAM Time % Na315 % Na425 % Na640 % RG011 Time Temp ºC 15.0 16.0 31.0 31.1 33.0 33.1 1 2 3 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 104 Time (Min) Na270 % Na740 % RG011 % 32.1 56.1 58.1 PEAK IDENTIFICATION Aspartic Acid Leucine Threonine Phenylalanine Serine Lysine Glutamic Acid Ammonia Proline Histidine Glycine Arginine Alanine Cysteic Acid Valine Methionine Sulfone Isoleucine Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 105 13 14 *Collagen 15 16 Hydrolysate PEAK IDENTIFICATION Methionine-D,L,-Sulfoxide Isoleucine trans-4-Hydroxy-L-Proline Leucine Aspartic Acid Tyrosine Threonine Phenylalanine Serine D,L & allo-Hydroxylysine Glutamic Acid Lysine Proline Ammonia Glycine Histidine Alanine Tryptophan Cystine Arginine Valine Methionine Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 106 Time(min) %1700-0112* %Na740 %RG011 Comment inject isocratic linear gradient isocratic 53.1 step gradient isocratic 55.1 isocratic re-equilibration Collagen Hydrolysate 12 13 Protein Hydrolysate MINUTES * For use with columns with serial numbers after 1314 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 107 10. Cystine 17. Hydroxylysines 24. Methionine Sulfone 4. Threonine 11. Valine 18. Lysine 25. Norleucine 5. Serine 12. Methionine 19. Ammonia 6. Glutamic acid 13. Isoleucine 20. Histidine 7. Proline 14. Leucine 21. Tryptophan Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 108: Precautions 6

    Precautions for Amino Acid Analysis Use Pickering Laboratories reagents and eluants. The quality of the chemicals is excellent, and the cost is low relative to the worth of your analytical results. Use the Pickering column and eluants. They are designed to work together.
  • Page 109 After you make a change, get at least two chromatograms showing the same effect of the change. This is especially true when you are trying to optimize gradient conditions. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 110 Every model of HPLC forms gradients differently. The programs suggested in this manual or in the information sheets are typical of the more popular HPLC pumps. Consult Pickering Laboratories if you need advice. If you need only the early part of the chromatogram, you can save time by truncating the gradient. Go to the final concentration of regenerant and hold it until the most basic component (arginine) elutes, then re-equilibrate with the initial buffer.
  • Page 111 6.2-21 Section 6 pplicAtions Notes Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 112 6.2-22 Section 6 pplicAtions Notes Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 113: Analytical Procedure 6

    Post-column derivatization can give improved sensitivity or better selectivity (reduction of interference) leading to lower detection limits. The Pickering Laboratories Pinnacle PCX was developed to facilitate the determination of carbamate insecticides, meeting or exceeding performance requirements of U.S. Environmental Protection Agency (USEPA) Method 531.1/531.2, and the AOAC International Protocol 29.A05:...
  • Page 114 The general structure of the carbamate insecticides is an N-methyl substituted urethane with the variation in the ester moiety. The structural formulas are shown in Figure 6.3-A. Aldicarb Sulfoxide Aldicarb Sulfone Carbaryl Aldicarb 3-Hydroxy Carbofuran Methomyl Carbofuran Oxamyl Propoxur 1-Naphthol Methiocarb BDMC Figure 6.3-A Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 115 1-naphthol, but at a different retention time. This observation is useful for troubleshooting. Basic Sample Preparation The following is a general sample preparation for Water samples containing carbamate. For details, consult the EPA 531.2 method for drinking water and the AOAC method for Vegetables. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 116 The two derivatization reagents required for carbamate analysis are a hydrolysis reagent (NaOH) and o-phthalaldehyde reagent. Note: During initial installation, the reagent bottles, lines, and pump should first be cleaned and primed with methanol to reduce possible fluorescence background. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 117 Note: The preparation of the OPA Diluent by the user is not recommended because sodium borate (any grades) contains excessive amounts of heavy metal contaminants and insoluble matter. These impurities will eventually precipitate in the reactor and flowcell. The one year warranty does not cover damage caused by these contaminants. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 118 1. Aldicarb sulfoxide (Standak) 7. Propoxur (Baygon) 2. Aldicarb sulfone 8. Carbofuran (Furadan) 3. Oxamyl (Vydate) 9. Carbaryl (Sevin) 4. Methomyl (Lannate) 10. 1-Naphthol 5. 3-Hydroxy carbofuran 11. Methiocarb (Mesurol) 6. Aldicarb (Temik) 12. BDMC internal standard Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 119 CONDITIONS FOR WATER/METHANOL GRADIENT Time (Min) Water % MeOH % 46.1 51.1 Carbamate Test Mix, 2.5ppm, 10ul injection, 25cm, Carbamate C column (0840250) Carbamate Test Mix, 0.25ppb, 100ul injection, 25cm, Carbamate C column (0840250) Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 120 40 pg of Carbamates in 400 µL 1. Aldicarb sulfoxide 5. 3-Hydroxycarbofuran 9. Carbaryl 2. Aldicarb sulfone 6. Aldicarb 10. 1-Naphthol 3. Oxamyl 7. Propoxur 11. Methiocarb 4. Methomyl 8. Carbofuran 12. BDMC (internal standard) Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 121 COLUMN TEMPERATURE: 42˚ C REAGENT FLOW RATE: 0.3 ML/MIN CONDITIONS FOR METHANOLIC SAMPLES Time (Min) Water % MeOH % 28.5 28.6 33.5 33.6 Carbamate Test Mix, 2.5ppm, 10µl injection, 15 cm, Carbamate C column(1846150) Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 122 COLUMN (4.6X150 MM) WITH AQUEOUS SAMPLES COLUMN TEMP: 42 ºC HPLC FLOW RATE: 1.0ML/MIN REAGENT FLOW RATE: 0.3ML/MIN CONDITIONS FOR AQUEOUS SAMPLES Time (Min) Water % MeOH % 26.1 28.1 4 ng of Carbamates in 150 µL Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 123 HPLC FLOW RATE: 1.0ML/MIN COLUMN TEMPERATURE: 42˚ C REAGENT FLOW RATE: 0.3 ML/MIN CONDITIONS FOR METHANOLIC SAMPLES Time (Min) Water % MeOH % 44.1 49.1 Carbamate Test Mix, 2.5ppm, 10μl injection, 25cm, Carbamate C Column (0846250) Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 124 METHOD 6: 0846250 C COLUMN (4.6X250MM) WITH AQUEOUS SAMPLES HPLC FLOW RATE: 1.0ML/MIN COLUMN TEMPERATURE: 42˚ C REAGENT FLOW RATE: 0.3 ML/MIN CONDITIONS FOR AQUEOUS SAMPLES Time (Min) Water % MeOH % 39.1 41.1 Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 125: Precautions 6

    70% acetonitrile if it will be used as the mobile phase. Do not store the column in water. Use the Pickering Laboratories carbamate analysis column, which is specifically designed and tested for the separation of carbamates in the EPA Methods.
  • Page 126 6.3-13 Section 6 pplicAtions Notes Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 127: Analytical And Post-Column Conditions 6

    (reduction of interference) leading to lower detection limits. The Pickering Laboratories Pinnacle PCX was developed to facilitate the determination of the herbicide glyphosate (and its metabolite AMPA), meeting or exceeding performance requirements of USEPA Method 547.
  • Page 128 125 ml. Blend at high speed for 3-5 min. and centrifuge for 10 min. Transfer 20 mL of the aqueous extract into a centrifuge tube and add 15 mL of methylene chloride (to remove nonpolar Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 129 AMPA. Figure 6.4-B µL of 5% NaOCl per L of GA116 shows a typical response curve. Figure 6.4-B Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 130 Note: The OPA reagent is sensitive to air oxidation and degrades over time. When the OPA reagent reservoir is maintained under inert gas pressure, the OPA reagent maintains its activity for up to one week without significant loss of activity. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 131 Reactor 2 Temp: Ambient Analytical Procedure Allow the column to equilibrate for about 20 minutes under initial conditions. Inject 10µl of Glyphosate Text Mixture (or the appropriate volume of your standard), and collect the first chromatogram. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 132: Sample Chromatograms 6

    The peak heights are influenced by the amount of hypochlorite in Reagent 1. Sample Chromatograms Glyphosate Test Mix, 2.5ppm, 10μl injection Glyphosate AMPA Figure 6.4-C Glyphosate and AMPA, 13ppb in K200, 100μl injection Glyphosate AMPA Figure 6.4-D Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 133: Precautions 6

    These impurities will eventually precipitate in the reactor and flowcell. The one year warranty does not cover damage caused by these contaminants. Use Restore if Iron contamination of the column is suspected. ™ Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 134 Filter all samples through a 0.45µm membrane filter. Some samples may require even more stringent filtration, especially if colloids are present. Aqueous samples must always be properly buffered. Consult EPA Method 547 for details. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 135 6.4-8 Section 6 pplicAtions Notes Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 136 6.4-9 Section 6 pplicAtions Notes Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 137: Contact Pickering Laboratories For Support

    • To Remove Iron Contamination From Column • To Pump RESTORE Through The Glyphosate Column CONTACT PICKERING LABORATORIES FOR SUPPORT There are several easy ways to contact Pickering Laboratories for Technical Support: Email: support@pickeringlabs.com Telephone: 800-654-3330 or 650-694-6700 Fax: 650-968-0749 Web Site: www.pickeringlabs.com...

  • Page 138: Instrument Parameter Log

    Please email the Log files INSTRUMENT PARAMETER LOG If you should have any problems with your Pinnacle PCX, the Instrument Log file is a key resource to finding the cause of, and solving any problems. Pinnacle PCX records detailed information about the instrument parameters in the Log files.

  • Page 139: Common System Problems

    Defective back-pressure regulator pressure regulator end, until the pressure drops Reagent pump stops or delivers wrong Check pump setting flow rate Check reagent pressurization Check pump seal for leakage Test or clean valves continued Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 140: Common Chromatography Problems

    Hydrindantin deposits from Expired TRIONE COMMON CHROMATOGRAPHY PROBLEMS When having chromatography problems collect 2-3 chromatograms that show the problem. Fax these and most recent normal one to Pickering Laboratories at (650) 968-0749. OBSERVED PROBLEM COMMON CAUSE ACTION TO TAKE NOTES...

  • Page 141: Amino Acids

    Remove any reagents used in amine synthesis, or cigarette smoke laden clothing Retention times drift over a long time Buildup of contaminants Flush the column Room temperature changes greatly Air condition the room with the seasons Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 142: Carbamates

    Disconnect the dichloromethane. Wash again with outlet of the column during the back methanol before use column flush operation. If organic solvent is on the cation- exchange column, follow the procedure on Page 7.8 Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 143: Glyphosate

    Glyphosate peak too small or gone, but Oxidizing reagent too weak, too old, AMPA present NaOCl stock solution too old Reactor at wrong temperature AMPA peak disappears, but Oxidizing reagent too strong Make fresh Oxidizing reagent Glyphosate present Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 144: Software Troubleshooting

    Minimum Equilibration time for steps are. Match analysis time to Pinnacle PCX is 5 min Run time of the Pinnacle PCX and match time of the equilibration step to Equilibration time of the Pinnacle PCX.
  • Page 145 More runs set up in HPLC sequence HPLC software usually displays only Pinnacle PCX software but not all Sequence and HPLC sequence do than in Pinnacle PCX. Make sure you number of unknown samples and your samples were completed not match...
  • Page 146 SOFTWARE TROUBLESHOOTING continued Reactor temp sensor error Heated reactor is not connected to the Open the Pinnacle PCX right side Contact Pickering Laboratories before main board panel and check that heated reactor changing any major components Heated reactor or main board are...

  • Page 147: Procedures

    IF REAGENT BACKFLOWS ONTO COLUMN This procedure usually works but may not work every time. 1. Shut down the Pinnacle PCX. 2. Flush both columns with regenerant. Use a very slow flow rate so that the back pressure does not exceed 2000 psi.
  • Page 148 4) Reconnect the column and guard in the normal directions and restart the HPLC and post-column systems. If analytical column is also contaminated, reverse the column and flush with Restore for 2 hrs. Equilibrate with K200 for 1 hour before use. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 149 Installation/Operational Qualitication of the Pinnacle PCX Installation/Operational Qualitication of the Pinnacle PCX Data Sheet Performance Qualifications of the Pinnacle PCX Data Sheet Sample Instrument Parameter Log 8.15 Flow Diagrams 8.16 • Simplex • Duplex Consumables and Spare Parts 8.18...

  • Page 150: Installation/Operational Qualitication Of The Pinnacle Pcx

    To qualify the installation and operation of the Pinnacle PCX 2.0 REFERENCES: 2.1 Operators Manual for the Pinnacle PCX 2.2 Installation / Operational Qualification of the Pinnacle PCX Data Sheet. Section 8.3 of the Operators Manual for the Pinnacle PCX. 3.0 EQUIPMENT:...
  • Page 151 Valve 2 when testing Pump 2. 5.1.5 Disconnect the analytical column to the Pinnacle PCX. This is the blue PEEK tubing that goes into the first mixing tee. Replace the blue peek tubing with a plug into the mixing tee. This will prevent any leaking out of the mixing tee.
  • Page 152 Installation / Operational Qualification of the Pinnacle PCX Data Sheet, Section 8.8 of the Operators Manual for the Pinnacle PCX. 5.1.12 Repeat steps 5.1.7 through 5.1.11 for Pump 2. Make sure to program the flowrate of Pump 2 to 1.0ml/min and change the flowrate of Pump 1 to 0ml/min.
  • Page 153 Create a method with the following parameters: 5.2.4 Create a sequence with one run of the method created in Step 5.2.3 5.2.5 Save and then Load the sequence that was created in Step 5.2.4. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 154 Allow enough time for the temperature to stabilize, and then record the temperature of the column heater. The specifications for the column heater accuracy are in the Installation / Operational Qualification of the Pinnacle PCX Data Sheet, Section 8.3 of the Operators Manual for the Pinnacle PCX.

  • Page 155: Installation/Operational Qualitication Of The Pinnacle Pcx Data Sheet

    Does the display turn on when the Pinnacle PCX is powered on? Yes / No Do the valves find home position when the Pinnacle PCX is turned on? The home position is when Yes / No the “V” on the valve is between 2 and 3.

  • Page 156: Performance Qualifications Of The Pinnacle Pcx Data Sheet

    Serial Number: Customer: 120V or 240V Asset: Performance Qualifications of the Pinnacle PCX Data Sheet Flow Rate Accuracy Pump 1 Flowrate Setpoint in mL/min Record Flowrate in ml/min Specifications Pass / Fail +/- 0.030 ml/min Pump 2 Flowrate Setpoint in mL/min...
  • Page 157 Run 4 Run 5 Run 6 Average Peak Standard Glyphosate Peak Area % CV Specification Pass / Fail Area Deviation Run 1 Run 2 ≤ 1.5% Run 3 Run 4 Run 5 Run 6 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 158 Run 4 Run 5 Run 6 Average Standard Aldicarb Peak Area % CV Specification Pass / Fail Peak Area Deviation Run 1 Run 2 ≤ 1.5% Run 3 Run 4 Run 5 Run 6 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 159 Run 5 Run 6 Retention Time Average Standard Cysteic Acid % CV Specification Pass / Fail in min Retention Time Deviation Run 1 Run 2 ≤ 0.5% Run 3 Run 4 Run 5 Run 6 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 160 20.1 24.1 Stop Time 24 min Post Time 12 min * Use the A Buffer corresponding to the column you have. The column insert will have the correct initial buffer listed in the method. Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 161 Run 5 Run 6 Retention Time Average Standard Cysteic Acid % CV Specification Pass / Fail in min Retention Time Deviation Run 1 Run 2 ≤ 0.5% Run 3 Run 4 Run 5 Run 6 Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 162 Reagent Flow Rate: 0.3mL/min 24.1 Stop Time 24 min Post Time 12 min * Use the A Buffer corresponding to the column you have. The column insert will have the correct initial buffer listed in the method. Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 163: Sample Instrument Parameter Log

    Sample Instrument Parameter Log NORMAL PRESSURES AND FLOWS AT INITIAL CONDITIONS Flow Rate Pressure Analytical Pump (Column) Reagent Pump 1 Reagent Pump 2 TEMPERATURE Set Temperature Actual Temperature Analytical Column Heated Reactor Room Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 164: Flow Diagram – Simplex

    Nut: 1452-0118 Ferrule: 1452-0117 Nut: 1452-0118 Nut: 3101-0011 Ferrule: 1452-0117 WASTE Ferrule: 1452-0112 Union: 3102-3063 1452-0185 Back Pressure Check Valve: 3106-1007 TO DETECTOR Regulator: 3102-9025 Nut: 1452-0226 Ferrule: 1452-0112 FROM HPLC bold = kit Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 165: Flow Diagram – Duplex

    Nut: 1452-0118 Nut: 3101-0011 Ferrule: 1452-0117 1452-0185 WASTE Ferrule: 1452-0112 Union: 3102-3063 Back Pressure TO DETECTOR Check Valve: 3106-1007 Regulator: 3102-9025 Nut: 1452-0226 Ferrule: 1452-0112 FROM HPLC bold = kit Nut: 1452-0116 Ferrule: 1452-0115 Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 166: Parts List For Pinnacle Pcx

    Tubing Assembly, Valve-Manifold, Dual Pump System 1452-0190 Tubing Assembly, Transducer-Valve, Single Pump 1100-0450 Tubing Assembly, Pinnacle PCX to HPLC 1100-0460 Dead Head Plumbing Kit, Pinnacle PCX to HPLC 1100-0500 Tubing Kit, Dual Pump Pinnacle 1100-0501 Tubing Kit, Single Pump Pinnacle Pinnacle Operators Manual...
  • Page 167 1452-0097 Reactor Cartridge Knitted Assembly - 2.0mL 130°C 1452-0098 Reactor Cartridge Knitted Assembly - 2.8mL 80°C 1452-0099 Reactor Cartridge Knitted Assembly - 3.0mL 80°C 1452-0100 Reactor Cartridge Knitted Assembly - 1.2mL & 1.6mL 130°C Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 168 Back Pressure Regulator, 100 psi 3102-9161 Tubing Cutter for 1/8-1/16” tubing 3106-1007 Inline Check Valve 3551-0073 Fuse, 5A Time lag high break ceramic 3560-2000 Cable, RS232 1452-0126 Relay Cable Assembly 3102-9040 Frit Replacement PEEK, 10µm 1452-0327 USB Cable Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 169: Recommended Consumables And Spare Parts

    Sodium eluant, pH 7.50, case of 4 ( 950mL per bottle) RG011 Sodium column regenerant (950mL) Na220 Sodium sample diluent, pH 2.20 case of 4 ( 250mL per bottle) 1700-0155 Calibration standard, oxidized feed hydrolysate, 0.25 µmole/mL, (5mL) Continued on next page Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 170 Native Sample Standard without Norleucine & Alpha-Amino-Beta- guanidinopropionic acid, in 0.2 N Lithium citrate buffer pH 2.36, 5 mL Sample Preparation SP 100 SERAPREP™, for sample preparation of serum, (250mL) UP 100 URIPREP™, for sample preparation of urine (250mL) Pinnacle Operators Manual Pickering Laboratories Inc.
  • Page 171 Glyphosate column, 4.0 mm ID x 150 mm (with Glyphosate test mixture1700-00??) 1700-3100 GARD Holder 1700-3101 Cation GARD (2 ea) 1700-3101 Kit, GARD Holder and two Cation GARDs 1705-0001 Sample clean up cartridge, SPE column caution exchange (10pkg) Pinnacle Operators Manual Pickering Laboratories Inc.

  • Page 172: Limited Warranty

    Limited Warranty INSTRUMENTS Pickering Laboratories, Inc., (Pickering) Instruments are warranted to be free of defects in material and workmanship under normal installation, use, and maintenance, for a period of one year from the date of delivery to the Customer. Pickering will replace or repair, without cost, any defective items.

  • Page 173: References

    • M.V. Pickering, “Modifying HPLC equipment to tolerate corrosive solutions,” LC•GC, 6, 9 (1988) 800–809.* • J.W. Dolan and L.R. Snyder, “Troubleshooting LC Systems,” Humana Press, Clifton, NJ (1989). * Reprints available from Pickering Laboratories AMINO ACID ANALYSIS • D.H. Spackman, W.H. Stein and S. Moore, Anal. Chem., 30 (1958) 1190.
  • Page 174 ndex Air Barrier tubing 2.6, 2.9, 2.14, 3.2, 3.5, 3.6, 3.12, 8.18 Ambient Reactor 2.7, 3.11, 5.7, 5.8, 8.3 Amino Acid 6, 7, 3.1, 3.3, 3.9, 3.14, 3.15, 6.2-5, 6.2-18, 8.11, 8.13, 8.21, 8.25 AMPA 6.4, 6.4-1, 6.4-2, 6.4-3, 6.4-5, 6.4-6, 8.23 Analytical Method 4.14 AOAC 6.2-2, 6.3, 6.3-1, 6.3-2, 6.4-1 Aqueous Sample 6.3-6, 6.3-7, 6.3-9, 6.3-11, 6.3-12, 6.4-7...
  • Page 175 ndex Dead-Head 6, 3.9 Deposits in Reactor 7.7 Designing a Post-column System 4 Detector Connections 2.8, 3.11 Detector Settings 4.14 Display Module 2.10 Electronics Compartment 2.11 Eluant 6, 2, 2.3, 3.1, 3.2, 3.10, 3.14, 3.15, 3.16, 4.18, 5.2, 5.3, 5.4, 5.5, 5.6, 6.2, 6.2-18, 6.2-19, 6.4-1, 6.4-7, 7.3, 7.4, 7.5, 7.6, 7.12, 8.9, 8.11, 8.13, 8.14, 8.21, 8.22 Empty Pump 3.13, 4.4, 4.15, 5.9 Enable 3.14, 4.3, 4.4, 4.5, 4.15, 5.5, 8.4, 8.6...
  • Page 176 ndex Heated Reactor 2, 2.7, 2.9, 2.13, 2.14, 3.11, 3.15, 4.2, 4.17, 5.2, 5.3, 5.5, 5.6, 5.8, 6.2-19, 7.4, 7.7, 7.10, 8.3, 8.15 Help 2, 4, 6, 2.5, 4.5, 4.7, 4.9, 4.11, 5.2, 7.2, 7.4, 7.8 High Pressure 5.3, 6.2-18, 7.6, 7.9, 8.19 HPLC Slowdown method 3.16, 4.18, 5.4 HPLC Synchronization 4.1 HPLC System Requirements 3.3...
  • Page 177 ndex OPA 6, 7, 3.2, 4.12, 5.3, 6.2, 6.2-2, 6.2-4, 6.2-5, 6.2-19, 6.3, 6.3-2, 6.3-4, 6.3-5, 6.3-12, 6.4-1, 6.4-3, 6.4-6, 7.5, 8.9, 8.10, 8.21, 8.23, 8.25 Operational Qualification 8.2, 8.4, 8.6 Organic Solvents 3.10, 6.2-18, 6.3-12, 6.4-7, 7.11 O-ring 2.4, 5.10, 5.14, 5.15, 7.10 Over-Pressure Relief 2.7, 2.13, 5.6, 7.4 Oxidized Feed Hydrolysate 8.21 Oxidizing Reagent 6.4-2, 6.4-3, 7.7...
  • Page 178 ndex Regenerant 3.3, 3.16, 4.18, 5.4, 6.2-18, 6.2-20, 7.5, 7.7, 7.11, 7.12, 8.9, 8.21, 8.22, 8.23 Relay 3, 5, 2.11, 2.12, 3.4, 3.6, 3.14, 4.1, 4.2, 4.3, 4.6, 4.14, 4.15, 7.8, 8.20 Rotor Seal 6, 3.3, 7.5, 7.6 Running a Chromatogram 3.14 Safety Features 2.13 Sample Chromatogram 6.2, 6.2-4, 6.2-6, 6.3, 6.3-5, 6.4, 6.4-5 Sample Preparation 6.2, 6.2-2, 6.3, 6.3-2, 6.3-3, 6.4, 6.4-1, 7.5, 8.22...
  • Page 179 ndex Technical Support 7.1, 7.6 Tefzel 6, 3.3, 6.2, 8.19 Thiofluor 6, 5.3, 6.2-2, 6.2-4, 6.2-5, 6.2-19, 6.3-2, 6.3-4, 6.3-5, 6.3-12, 6.4-1, 6.4-3, 6.4-4, 6.4-6, 8.9, 8.10, 8.21, 8.23 Trione 7, 3.2, 3.3, 3.14, 6.2, 6.2-3, 6.2-4, 6.2-19, 7.4, 7.5, 7.7, 8.11, 8.13, 8.21 Troubleshooting 1, 6.3-2, 7.2, 7.3, 7.7, 7.8, 7.9, 7.10, 8.25 Tutorials 4.11 URIPREP 6.2-3, 8.22...

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