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Waters APGC Operator's Manual Supplement

Atmospheric pressure gas chromatography
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Atmospheric Pressure
GC
Operator's Guide Supplement
Revision F
Copyright © Waters Corporation 2010–2012
All rights reserved

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Summary of Contents for Waters APGC

  • Page 1 Atmospheric Pressure Operator’s Guide Supplement Revision F Copyright © Waters Corporation 2010–2012 All rights reserved...

  • Page 2: Copyright Notice

    Corporation assumes no responsibility for any errors that may appear in this document. This document is believed to be complete and accurate at the time of publication. In no event shall Waters Corporation be liable for incidental or consequential damages in connection with, or arising from, its use. For the most recent revision of this document, consult the Waters Web site (waters.com).

  • Page 3: Customer Comments

    Contacting Waters ® Contact Waters with enhancement requests or technical questions regarding the use, transportation, removal, or disposal of any Waters product. You can reach us via the Internet, telephone, or conventional mail. Waters contact information Contacting medium Information...

  • Page 4: Safety Considerations

    Safety considerations Some reagents and samples used with Waters instruments and devices can pose chemical, biological, or radiological hazards (or any combination thereof). You must know the potentially hazardous effects of all substances you work with. Always follow Good Laboratory Practice, and consult your organization’s safety representative for guidance.

  • Page 5: Safety Advisories

    APGC ion chamber • GC components Do not dispose of the instrument or return it to Waters for repair until the authority responsible for approving its removal from the premises specifies the extent of decontamination required, and the level of residual contamination permissible.

  • Page 6: Operating This Device

    The APGC allows coupling of a GC (gas chromatography) instrument to the atmospheric pressure ionization (API) source on compatible LCMS instruments. The APGC is for research use only. It is not intended for use in diagnostic applications. It is intended for use only by qualified laboratory...

  • Page 7: Calibrating

    Calibrating To calibrate GC systems, follow acceptable calibration methods using at least five standards to generate a standard curve. The concentration range for standards should include the entire range of QC samples, typical specimens, and atypical specimens. When calibrating mass spectrometers, consult the calibration section of the operator’s guide for the instrument you are calibrating.

  • Page 8: Ec Authorized Representative

    EC authorized representative Waters Corporation (Micromass UK Ltd.) Floats Road Wythenshawe Manchester M23 9LZ United Kingdom Telephone: +44-161-946-2400 Fax: +44-161-946-2480 Contact: Quality manager viii...

  • Page 9: Table Of Contents

    Safety advisories ....................v Operating this device ..................vi Applicable symbols ..................... vi Audience and purpose..................vi Intended use of the APGC .................. vi Calibrating ......................vii Quality control ....................vii ISM classification ....................vii ISM Classification: ISM Group 1 Class A ............vii EC authorized representative ................
  • Page 10 Removing the LC source enclosure from the mass spectrometer....2-3 Preparing the source ion block for GC operation ........... 2-5 Installing the APGC ion chamber on the mass spectrometer’s ion block ..2-9 Installing the APGC source enclosure in the mass spectrometer ....2-12 Installing the APGC vial carriers in the mass spectrometer’s source ..
  • Page 11 Specific warnings ..................... A-3 Caution advisory ....................A-5 Warnings that apply to all Waters instruments ......... A-6 Electrical and handling symbols ..............A-11 Electrical symbols ..................A-11 Handling symbols ..................A-12 B Installing the GC Column ..............B-1 C Preparing Sample Vials ..............C-1 Preparing vials ....................
  • Page 12 Table of Contents...

  • Page 13: Instrument Description

    ® The Waters Atmospheric Pressure GC (APGC) couples an Agilent GC with a compatible Waters LCMS instrument. Doing so makes possible performing LC and GC analyses in the same system, without compromising performance. It also avoids the need for separate, dedicated GCMS and LCMS instrumentation.

  • Page 14: Waters Apgc

    Waters APGC The APGC provides complementary information to the LCMS instrument, enabling analysis of compounds of low molecular weight or low-to- intermediate polarity. The APGC is compatible with these Waters LCMS instruments: ® • Xevo TQ MS • Xevo TQ-S •...
  • Page 15 Agilent GC and autosampler mounted on the APGC platform: Agilent 7890 GC Autosampler APGC platform Waters APGC...

  • Page 16: Apgc Components

    The platform carries the heated transfer line and the GC instrument, which the mass spectrometer connects to via the APGC source enclosure and ion chamber. A locking handle locks the sliding platform, preventing its unintentional movement when you disconnect the locking ring from the APGC source enclosure.

  • Page 17: Apgc Trolley (Synapt G2 Only)

    Trolley cabinet Locking lever Locking plate Stabilizers The APGC trolley is a mobile steel cabinet on top of which the APGC is fixed in place. A locking lever and locking plate engage or disengage the trolley and mass spectrometer. APGC components...
  • Page 18 Locking plate Supporting pillars (instrument) (trolley) To engage the APGC trolley: Slide the locking plate forward so that the two indentations meet the supporting pillars under the instrument. Push the trolley toward the locking plate so that the two indentations meet the supporting pillars under the trolley.
  • Page 19 Supporting pillars Locking plate Supporting pillars (instrument) (trolley) To disengage the APGC trolley: Before performing this procedure, ensure that you have first Requirement: loosened the stabilizers under the trolley. Lift the locking lever. Pull the locking tab outward as far as it will go.

  • Page 20: Heated Transfer Line

    Warning: heated transfer line. The line heats during normal use, and hot gas can escape from the capillary column’s tip. Use the APGC protection cap to cover the tip when you withdraw the tube from the source enclosure for extended periods.

  • Page 21: Apgc Source Enclosure

    The heated transfer line positions the capillary column tip in the correct location relative to the APGC ion chamber within the mass spectrometer’s source enclosure. Turning the locking ring through 180° locks the transfer line to the APGC source housing. APGC source enclosure...

  • Page 22: Heated And Unheated Vial Carriers

    Warning: heated vial carrier and vials. The mass spectrometer’s source ion block becomes hot during normal use. The APGC source enclosure incorporates two removable vial carriers (heated and unheated). Each carrier can contain up to three vials: • The heated vial carrier is located on top of the mass spectrometer’s source ion block.

  • Page 23: Apgc Ion Chamber

    APGC ion chamber For APGC operation, the APGC ion chamber mounts on the ion block, in place of the cone gas nozzle. The APGC ion chamber positions the corona pin relative to the mass spectrometer’s sample cone. Although the layout differs, the corona pin is functionally identical to the corona pin used in LC operation.
  • Page 24 1-12 Instrument Description...

  • Page 25: Setting Up The Apgc

    Setting up the APGC You must set up the APGC and otherwise prepare it for operation with compatible instruments. Refer to the online Help for information about operating the APGC. Contents: Topic Page Preparing the mass spectrometer for operation with the APGC 2-2...

  • Page 26: Preparing The Mass Spectrometer For Operation With The Apgc

    Set the source temperature to 30 °C. Wait 30 minutes, to allow the source to cool. The API gas flow stops automatically when you click Source Note: Standby. The relevant instrument’s operator’s overview and See also: maintenance guide. Setting up the APGC...

  • Page 27: Removing The Lc Source Enclosure From The Mass Spectrometer

    To avoid puncture wounds, take great care when the Warning: corona pin is in place and you are working with the source enclosure open. The tip of the corona pin is sharp. Preparing the mass spectrometer for operation with the APGC...
  • Page 28 Removing the source enclosure: Cable storage positions Supporting studs Source enclosure release Store the cables neatly by plugging them into the cable storage positions on the rear of the source enclosure. Setting up the APGC...

  • Page 29: Preparing The Source Ion Block For Gc Operation

    90°. Rotating the sampling cone assembly: Combined, 2.5-mm Allen wrench and cone extraction tool Sampling cone assembly Corona pin mounting socket Source isolation valve Cone gas nozzle handle Preparing the mass spectrometer for operation with the APGC...
  • Page 30 Sampling cone assembly Retrieve the combined, 2.5-mm Allen wrench and cone extraction tool from its storage location on the source adaptor housing. Slide the collar to the end of the tool. Preparing the cone extraction tool: Collar Setting up the APGC...
  • Page 31 Rotate and lift the tool and collar to remove the sample cone from the cone gas nozzle. Store the cone gas nozzle in a safe location. Tip: Removing the sample cone: Sample cone Cone gas nozzle Preparing the mass spectrometer for operation with the APGC...
  • Page 32 10. Repeat step 9 for the lower, gas-cone position block. 11. Return the tool to its storage location on the source adaptor housing. Store the gas-cone position blocks, securing screws, and washers in Tip: a safe location. Setting up the APGC...

  • Page 33: Installing The Apgc Ion Chamber On The Mass Spectrometer's Ion Block

    To avoid burn injuries, take great care while Warning: working with the source components, which can be hot. During APGC operation with the Xevo TQD or SQ Detector 2 Requirement: mass spectrometer, you must use the reduced-aperture, 0.36-mm, sample cone supplied with the APGC, to avoid problems associated with unstable signal intensity.
  • Page 34 Slide the sample cone into the left-hand end of the APGC ion chamber. Inserting the sample cone: Sample cone APGC ion chamber O-ring Locking plate Corona pin adjuster nut Looking into the right-hand end of the APGC ion chamber, use the corona pin adjuster nut to position the corona pin tip to the edge of the small hole at the opposite end of the assembly.
  • Page 35 Connect the APGC corona pin extension cable to the corona pin mounting socket. Pull out the locking plate on the APGC ion chamber to expose the 2 captive securing screws. Locate the APGC ion chamber on the ion block and use the combined, 2.5-mm Allen wrench and cone extraction tool to tighten the 2 captive...

  • Page 36: Installing The Apgc Source Enclosure In The Mass Spectrometer

    11. Connect the free end of the APGC corona pin extension cable to the APGC ion chamber cable connector. 12. Use the dentist’s mirror to look into the open end of the APGC ion chamber. If necessary, use the corona pin adjuster nut to reposition the...

  • Page 37: Installing The Apgc Vial Carriers In The Mass Spectrometer's Source

    Fit the heated vial carrier on top of the mass spectrometer’s source ion block. Fit the unheated vial carrier into the bottom of the APGC source enclosure; push it fully to the front of the enclosure. Open the source isolation valve.

  • Page 38: Installing Vials In The Vial Carriers

    Installing vials in the vial carriers You must install the vials in the vial carriers before connecting the APGC to the mass spectrometer (see page 2-16). Required materials • Chemical-resistant, powder-free gloves • Tweezers To avoid personal contamination with biologically...
  • Page 39 Use tweezers to insert the vials into the holes in the vial carriers. You must use only closed vials when placing samples in Requirement: the heated vial carrier. Tips: • Use the unheated vial carrier for more volatile samples, the heated vial carrier for less volatile samples.

  • Page 40: Connecting The Apgc To The Mass Spectrometer

    Pull the locking handle toward you to release the sliding table, then carefully move the sliding table towards the mass spectrometer (see the figure on page 1-4). Engage the screw threads on the APGC locking ring and source enclosure heated transfer line connector (see the figures on page 1-8 page 1-9).

  • Page 41: Disconnecting The Apgc From The Mass Spectrometer

    Carefully move the sliding table fully away from the mass spectrometer. Release the locking handle to secure the sliding table. Fit and tighten the APGC protection cap over the capillary column tip. Disconnecting the APGC from the mass spectrometer 2-17...

  • Page 42: Removing Vials From The Vial Carriers

    Removing vials from the vial carriers You must disconnect the APGC from the mass spectrometer before removing vials from the vial carriers (see page 2-17). Required materials • Chemical-resistant, powder-free gloves • Tweezers To avoid personal contamination with biologically Warning:...

  • Page 43: Preparing The Mass Spectrometer For Lc Operation

    To avoid burn injuries, take great care while working Warning: with the source and heated vial carrier; they can be hot. Pull the APGC source enclosure release (located at the bottom, right-hand side) outward, and then swing open the enclosure. Close the source isolation valve.

  • Page 44: Removing The Apgc Source Enclosure From The Mass Spectrometer

    Removing the APGC source enclosure from the mass spectrometer Required materials Chemical-resistant, powder-free gloves To avoid personal contamination with biologically Warning: hazardous, toxic, or corrosive materials, and to avoid spreading contamination to uncontaminated surfaces, wear clean, chemical-resistant, powder-free gloves when handling source components.

  • Page 45: Removing The Apgc Ion Chamber From The Mass Spectrometer's Ion Block

    Disconnect the APGC corona pin extension cable from the APGC ion chamber cable connector (see page 2-11). Pull out the locking plate on the APGC ion chamber to expose the 2 captive screws (see page 2-10). Use the combined, 2.5-mm Allen wrench and cone extraction tool to loosen the 2 captive screws that secure the APGC ion chamber to the ion block.

  • Page 46: Preparing The Source Ion Block For Lc Operation

    For all other instruments, retain the sample cone for use in the next procedure. Store all other APGC components in a safe location. Preparing the source ion block for LC operation Required materials • Chemical-resistant, powder-free gloves • Combined, 2.5-mm Allen wrench and cone extraction tool...
  • Page 47 Select the correct sample cone for your instrument: • For the Xevo TQD or SQ Detector 2 instruments, use the 0.50-mm sample cone, supplied with the instrument, which you stored when preparing the source ion block for GC operation (see page 2-8, step...

  • Page 48: Installing The Lc Source Enclosure On The Instrument

    Connect the source enclosure cables to the instrument’s connectors. The cables and connectors are color-coded; the blue-sleeved cable Tip: connects to the blue connector and the yellow-sleeved cable to the yellow connector. Slide the instrument’s source interface door closed. 2-24 Setting up the APGC...

  • Page 49: Maintenance Procedures

    Maintenance Procedures This chapter provides the maintenance guidelines and procedures necessary to maintain the APGC’s performance. Keep to a maintenance schedule, and perform maintenance as required and described in this chapter. Contents: Topic Page Maintenance schedule Spare parts Safety and handling...

  • Page 50: Maintenance Schedule

    When sensitivity page 3-7. decreases to unacceptable levels. Spare parts Waters recommends that you replace only the parts mentioned in this document. For spare parts details, see the Waters Quality Parts Locator on the Waters Web site’s Services/Support page. Maintenance Procedures...

  • Page 51: Safety And Handling

    (API gas) is turned off (see page 2-2). • The APGC is disconnected from the instrument (see page 2-17). • The APGC protection cap is fitted to the capillary column tip (see page 1-8). Appendix A for safety advisory information.

  • Page 52: Cleaning The Mass Spectrometer Sample Cone

    Cleaning the mass spectrometer sample cone For details about how to clean the sample cone, refer to the mass spectrometer’s operator’s overview and maintenance guide. Cleaning or replacing the corona pin APGC ion chamber assembly: APGC ion chamber body Insulator Spring...
  • Page 53 Disconnect the APGC corona pin extension cable from the cable connector of the APGC ion chamber. Do not lose any of the internal components of the APGC ion Important: chamber when removing the corona pin adjuster nut from the assembly.
  • Page 54 Fit the ceramic washer, spring, and insulator to the corona pin (see the figure on page 3-4). 10. Fit the corona pin assembly in the APGC ion chamber, and fit and tighten the corona pin adjuster nut. 11. Reposition the corona pin (see the figure on page 2-10).

  • Page 55: Cleaning The Apgc Ion Chamber

    To avoid damaging the instrument by sudden Caution: venting, do not open the source isolation valve at any time while the APGC ion chamber is removed from the ion block assembly. To clean the APGC ion chamber: Prepare the instrument for working on its source (see page 2-2).
  • Page 56 Maintenance Procedures...
  • Page 57 Safety Advisories Waters instruments display hazard symbols designed to alert you to the hidden dangers of operating and maintaining the instruments. Their corresponding user guides also include the hazard symbols, with accompanying text statements describing the hazards and telling you how to avoid them.

  • Page 58: A Safety Advisories

    Heed all warnings when you install, repair, and operate Waters instruments. Waters assumes no liability for the failure of those who install, repair, or operate its instruments to comply with any safety precaution.

  • Page 59: Specific Warnings

    The following warnings can appear in the user manuals of particular instruments and on labels affixed to them or their component parts. Burst warning This warning applies to Waters instruments fitted with nonmetallic tubing. Pressurized nonmetallic, or polymer, tubing can burst. Warning: Observe these precautions when working around such tubing: •...
  • Page 60 Biohazard warning This warning applies to Waters instruments that can be used to process material that might contain biohazards: substances that contain biological agents capable of producing harmful effects in humans.

  • Page 61: Caution Advisory

    Chemical hazard warning This warning applies to Waters instruments that can process corrosive, toxic, flammable, or other types of hazardous material. To avoid injury from handling biologically Warning: hazardous, toxic, or corrosive materials, you must know the hazards associated with them. Observe Good Laboratory Practice (GLP), and consult your organization’s safety...

  • Page 62: Warnings That Apply To All Waters Instruments

    Warnings that apply to all Waters instruments When operating this device, follow standard quality control procedures and the equipment guidelines in this section. Attention: Changes or modifications to this unit not expressly approved by the party responsible for compliance could void the user’s authority to operate the equipment.
  • Page 63 • Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind. • Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder konzentrierte Salpeter- oder Schwefelsäure verwenden. • Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich reduziert. Warnings that apply to all Waters instruments...
  • Page 64 Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico sotto pressione: • Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero pressurizzati. • Spegnere tutte le fiamme vive nell'ambiente circostante. • Non utilizzare tubi eccessivamente logorati o piegati. •...
  • Page 65 농축 질산 또는 황산과 함께 사용하지 마십시오. • 염화 메틸렌(Methylene chloride) 및 디메틸술폭시드(Dimethyl sulfoxide)는 비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오. 警告：圧力のかかったポリマーチューブを扱うときは、注意してください。 • 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。 • 近くにある火を消してください。 • 著しく変形した、または折れ曲がったチューブは使用しないでください。 • 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流 さないでください。 • 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が あり、その場合、チューブは極めて低い圧力で破裂します。 Warnings that apply to all Waters instruments...
  • Page 66 Warning: The user shall be made aware that if the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired. Attention: L’utilisateur doit être informé que si le matériel est utilisé d’une façon non spécifiée par le fabricant, la protection assurée par le matériel risque d’être défectueuses.

  • Page 67: Electrical And Handling Symbols

    These can appear in instrument user manuals and on the instrument’s front or rear panels. Electrical power on Electrical power off Standby Direct current Alternating current Protective conductor terminal Frame, or chassis, terminal Fuse Contact Waters for correct disposal and recycling instructions. Electrical and handling symbols A-11...

  • Page 68: Handling Symbols

    Handling symbols These handling symbols and their associated text can appear on labels affixed to the outer packaging of Waters instrument and component shipments. Keep upright! Keep dry! Fragile! Use no hooks! A-12 Safety Advisories...

  • Page 69: B Installing The Gc Column

    GC column that operates in constant-flow mode. The length of the make-up gas tube within the oven is critical, and only a Waters engineer should install it.
  • Page 70 To avoid eye injury, wear safety glasses when handling the Warning: capillary column, the ends of which are sharp. To install the APGC column: Referring to the Agilent GC user documentation, fit the capillary column to the GC oven frame.
  • Page 71 Inspect the column end using an eyeglass. Ensure that the cut end is perpendicular to the column, Requirement: even, and has no chips or rough edges, for a rough, ragged, or skewed end can reduce performance. Otherwise, repeat step Incorrect Incorrect Correct Retract the capillary column so that no more than 1 mm of the column...
  • Page 72 Installing the GC Column...
  • Page 73 Preparing Sample Vials If you need to use reference or modifier samples, you must prepare vials for use with the APGC. Contents: Topic Page Preparing vials...

  • Page 74: C Preparing Sample Vials

    Preparing vials For both reference and modifier samples, you must use only closed vials when placing samples in the heated vial carrier. Preparing closed vials Required materials • Chemical-resistant, powder-free gloves • Ceramic wafer • 1.5-mL crimp-top autosampler vials • Septum caps •...

  • Page 75: Preparing Open Vials

    Preparing open vials Required materials • Chemical-resistant, powder-free gloves • 1.5-mL crimp-top autosampler vials To prepare open vials: Place approximately 0.5 mL of modifier sample in a crimp-top autosampler vial. Preparing vials...
  • Page 76 Preparing Sample Vials...
  • Page 77 1-11 installing removing 2-21 handling symbols A-12 source enclosure installing 2-12 installing removing 2-20 APGC source enclosure 2-12 vial carriers APGC vial carriers 2-13 installing 2-13 LC source enclosure 2-24 removing 2-19 intended use applicable symbols ISM classification...
  • Page 78 APGC ion chamber 2-21 APGC source enclosure 2-20 LC source enclosure replacement parts replacing, corona pin safety advisories safety procedures, maintenance sample cone, cleaning source enclosure APGC, installing 2-12 LC, installing 2-24 source ion block preparing for GC operation...

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