Knauer 4000 MiD Instructions Manual
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Knauer 4000 MiD Instructions Manual

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4000 MiD®
Mass spectrometer
Instructions
HPLC
Document No. V6695

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  • Page 1 4000 MiD® Mass spectrometer Instructions HPLC Document No. V6695...
  • Page 2 For latest version of the instructions, check our website: https://www.knauer.net/en/Support/User-manuals Copyright: This document contains confidential information and may not be reproduced without written content of KNAUER Wissenschaftliche Geräte GmbH. © KNAUER Wissenschaftliche Geräte GmbH 2018 All rights reserved. 4000 MiD® Instructions, V6695...

  • Page 3: Table Of Contents

    6.1.1 MiD system pump-down ......... . . 28 4000 MiD® Instructions, V6695...
  • Page 4 Appendices ................51 4000 MiD® Instructions, V6695...

  • Page 5: Symbols And Signs

    MiD. Failure to comply with the warning instructions violates safety standards associated with the proper use of the system and its design. KNAUER assumes no liability for the failure to comply with these requirements.

  • Page 6: Pictogrammes De Sécurité (Fra)

    êtres suivit en tout temps lors de l’entretien, l’installation, la réparation et l’opération du MiD. Tous default d’application de ces règles de sécurité serait considéré comme une violation des normes de sécurité. KNAUER ne saurait voir sa responsabilité engagée en cas de manquement de l’uti- lisateur à...
  • Page 7 à des substan- ces corrosives. Utilisez des protections corporelles adéquates. Note: Une Note indique des informations importantes pour l’utilisation du software et/ou de l’équipement. Veuillez lire les informations avec attention et suivez les instructions. 4000 MiD® Instructions, V6695...

  • Page 8: Important Safety Information

    Sauf mention contraire, NE PAS retirer les cou- vercles de protection. Le produit est scellé à l’usine. Les dom- mages ou levée des scellés de garantie entraîne la perte de la responsabilité et droits de garantie. 4000 MiD® Instructions, V6695...

  • Page 9: Chemical Hazards

    In case of oxygen reduction, all personnel need to leave the room and alert the proper health and safety represent- ative. 4000 MiD® Instructions, V6695...

  • Page 10: Safety And Regulatory Standards

    Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at their expense. 4000 MiD® Instructions, V6695...

  • Page 11: Electromagnetic Compatibility

    WEEE Directive are identified with a crossed over “wheelie” bin symbol on the product label. An authorized waste disposal service must be used to dispose of the product for recycling or disposal, or alternatively return the product to KNAUER. Warning The manufacturer’s declaration becomes invalid if the user modifies the original product or installs additional compo- nents.
  • Page 12 Avertissement L’instrument n’est pas conçu pour être utilisé dans une atmosphère explosible. Il est de la responsabilité du client de vérifier que l’environnement de fonctionnement répond aux exigences d’un secteur non-dangereux quant à l’atmosphère explosible. 4000 MiD® Instructions, V6695...

  • Page 13: Product Information

    The vacuum system consists of a vacuum chamber coupled to two tur- bo-molecular pumps, which are backed by a small diaphragm pump. All vacuum pumps are integrated within the MiD. Unlike conventional mass spectrometers there are no external, floor-standing rotary pumps. This 4000 MiD® Instructions, V6695...

  • Page 14: Theory Of Microspray

    Fig. 1 shows the connections and ports on the front panel of the MiD. Refer to the labels listed in the table below during operation. Connection Description USB Port On/Off Power switch LED Status Indicators Spraychip assembly high voltage connection 4000 MiD® Instructions, V6695...

  • Page 15: Led Status Indicators

    Fig. 2 LED status indicators The LEDs indicate the following statuses: Red: Indicates that a serious error has occurred. User intervention will be required to rectify the fault. Fault details will be displayed on via error 4000 MiD® Instructions, V6695...

  • Page 16: The Rear Panel

    Avertissement Le 4000 MiD offre une double isolation renfor- cée pour l’alimentation secteur. Tout équipement externe connec- té aux 4000 MiD par le panneau arrière doit lui aussi fournir une double isolation renforcée à l’alimentation secteur. Connection Description...

  • Page 17: Scope Of Delivery

    Product information Fig. 3 Diagram of rear panel 4. Scope of delivery Note: Only use original parts and accessories made by KNAUER or a com pany authorized by KNAUER. ƒ 4000 MiD ƒ MiDas ƒ Starter kit: - Mains leads (2 in total)

  • Page 18: Unpacking And Setup

    The use of an inadequately rated power cord can lead to electric shock or short circuit. Avertissement N’utilisez jamais un cordon d’alimentation autre que celui fourni par le fabricant. L’utilisation d’un cordon d’ali- mentation non-adéquat peut provoquer un choc électrique ou un court-circuit. 4000 MiD® Instructions, V6695...

  • Page 19: The Mid And Associated Parts

    Syringe pump power supply New Era (NE-1000) syringe pump 250 µL luer lock syringe Syringe pump communication cable Optional Part number Description of part accessories A66907 vac-chip O-ring kit A66908 vac-chip screw kit A66919 SFI/DFI tubing & ferrule kit 4000 MiD® Instructions, V6695...

  • Page 20: Setting Up The Mid

    4 mm allen key – ‘T’ Handle Size PH1 Phillips screwdriver Delrin tweezers – flat, round SFD cover plate and dust cap Setting up the MiD Fig. 4 shows a typical configuration of the 4000 MiD. 253 mm 449 mm 354 mm 109 mm Fig.

  • Page 21: Operational Configuration

    Avertissement Le 4000 MiD offre une double isolation renfor- cée pour l’alimentation secteur. Tout équipement externe connec- té aux 4000 MiD par le panneau arrière doit lui aussi fournir une double isolation renforcée à l’alimentation secteur. 4000 MiD® Instructions, V6695...

  • Page 22: Switching On The System

    Product information Warning The 4000 MiD is used to analyse liquid samples, liquid contact with external equipment may lead to the risk of electric shock or short circuit. The user must ensure that fluidic connec- tions are not close to ancillary equipment and are checked for leaks prior to use.

  • Page 23: The Source, Filter, Detector (Sfd) Assembly

    1. Ensure the O-ring is present and then lower the spraychip flange Procedure down onto the front face of the vac-chip flange. Align the three mounting holes with the threaded sections on the vac-chip flange, as shown in Fig. 7. 4000 MiD® Instructions, V6695...

  • Page 24: The Vac-Chip Assembly

    Procedure 1. The MiD without the vac-chip assembly should look like in Fig. 8. Note: When no vac-chip assembly is fitted an SFD cover plate (not shown) must be fitted. 4000 MiD® Instructions, V6695...
  • Page 25 6. If excessive force is required stop immediately and repeat steps 2-5. 7. Once the vac-chip assembly is fitted the MiD should look as shown in Fig. 10. 4000 MiD® Instructions, V6695...

  • Page 26: The Spraychip Assembly

    Une mauvaise ins- tallation de l’assemblage pourrait le rendre électriquement dan- gereux. Pour éviter tout risque de blessure, s’il vous plaît suivez attentivement les instructions fournies pour installer l’assemblage spraychip. 4000 MiD® Instructions, V6695...

  • Page 27: The Split Flow Interface (Sfi)

    HPLC or MiDas™ compact interface module, to the MiD. KNAUER recommends to use a flow rate range of 10 µL – 2 mL/ min. The SFI is also used for calibrating the MiD (see „7.1 Calibrating the MiD“...
  • Page 28 SFI orientations When creating a split with the SFI, it is important to note the following: ƒ KNAUER recommends a flow rate of 0.3 - 2 µL/min to the spraychip 200. ƒ The split ratio can be changed by changing both the inner diameter and the length of the waste line (high flow tube).

  • Page 29: The Direct Flow Interface (Dfi) - Optional

    5.8.2 The Direct Flow Interface (DFI) – optional The DFI can be used to directly infuse samples from a syringe pump and couple the MiD to a nano-flow LC system. KNAUER recommends a flow rate range of 200 – 2000 nL/min to the spraychip 200.

  • Page 30: Operating The Front Cover Safety Interlock

    Status bar. The door will click into position when the door reaches 90° and will remain fixed in this orientation until pushed shut. Door shut Door open Fig. 16 Front cover door positions 4000 MiD® Instructions, V6695...

  • Page 31: Installing A Syringe Pump

    17) ou alors d’êtres équipé d’un silencieux (disponible auprès d’KNAUER). Warning Removal of the top cover of the 4000 MiD can lead to the risk of personal injury and exposure to hazardous voltages. Never remove the cover of the 4000 MiD, only certified persons are authorised to carry out repairs internally.

  • Page 32: Operation

    9.0E2 Torr. 6.2.3 Shutting down the MiD At times, the MiD has to be powered down, for example, when service or maintenance work has to be performed. Follow the procedure in the corresponding software instructions. 4000 MiD® Instructions, V6695...

  • Page 33: Functional Tests

    7.1 Installation Qualification (IQ) The customer may request the Installation Qualification, which is free of charge. In case of a request, the Technical Support of KNAUER or from a provider authorized by KNAUER performs this functionality test during the installation.

  • Page 34: Calibration

    8. Calibration The MiD has to be calibrated before any sample analyses can be per- formed. Sodium Formate (NaOOCH) is used to calibrate the 4000 MiD. The required solution is 1 mg/mL in 1:1 2-propanol:water. It is recom- mended that the MiD is recalibrated if known m/z or resolution values have shifted, an ion guide or ionchip is replaced or the MiD is moved to a new environment.

  • Page 35: Flushing The System After Calibrating

    The external surfaces of the 4000 MiD can be cleaned by wiping the sur- faces down with 10% aqueous isopropyl alcohol. It is recommended to perform periodic inspections and maintenance of the 4000 MiD components to ensure its operational performance.
  • Page 36 The items used with the 4000 MiD that can be maintained by the user are the spraychip 200 vac-chip™, DFI and SFI. All items can be cleaned and/ ®,...

  • Page 37: Removing And Replacing The Spraychip

    If there is any excessive resistance when tightening the screw, stop and repeat steps 6–12. 13. Connect the high-voltage connector from the DFI/SFI to the high-voltage output located at the front of the MID (see Fig. 15). 14. Close the door. 4000 MiD® Instructions, V6695...

  • Page 38: Cleaning The Spraychip

    In the event that this delay continues to be unac- ceptable then the spraychip must be replaced. If the spraychip looks visually degraded or you have any queries please contact KNAUER before using the device. 9.3.2 Cleaning the Spraychip with SFI Procedure 1.

  • Page 39: Liquid Flow Rate Measurement

    If the spraychip looks visually degraded or you have any queries please contact KNAUER before using the device. Liquid flow rate measurement In the case that sensitivity or spray stability remains poor after cleaning or replacement of the spraychip 200.

  • Page 40: Spraychip Assembly Cleaning

    3. Screw the flow meter adaptor into the DFI (Fig. 35) using the same procedure as when fitting a spraychip (see „8.2 Removing and replac- ing the spraychip“ on page 33 flow meter adapter Fig. 21 DFI with flow meter adapter 4000 MiD® Instructions, V6695...

  • Page 41: Cleaning The Split Flow Interface

    5. Using the syringe pump flush the SFI. 6. Infuse at least 200 µL of the methanol/water solution through the SFI. The solution will drip from the end of the waste and input lines of the SFI. 4000 MiD® Instructions, V6695...

  • Page 42: Spraychip Assembly Maintenance

    In the event the SFI appears blocked and/or the measured flow rate is incorrect, then replace the low flow tubing located inside the SFI (see „8.6 Spraychip assembly maintenance“ on page 38). If the problem persists and/or you have any queries please contact KNAUER before using the SFI. Spraychip assembly maintenance When the spraychip assemblies appear blocked and/or the measured flow rates are incorrect, then the low flow tubing should be replaced.
  • Page 43 9. Fit the nut to the input union, the larger of the two; push the tube into the union whilst tightening the nut. 10. Slide the opposite end of the low flow tube into the second finger- tight nut. 4000 MiD® Instructions, V6695...

  • Page 44: Replacing The Split Flow Interface Tubing

    5. Unscrew the input line nut (Fig. 40 and Fig. 41) and associated tubing. 6. Using the PH1 Phillips screwdriver, loosen the three screws in the main body of the SFI. Once the screws are loose remove the top cover of the SFI (Fig. 41). 4000 MiD® Instructions, V6695...
  • Page 45 8. Remove the tee, reducing union and tubing from the SFI using the plastic tweezers (A66911) (Fig. 43). Fingertight nuts Reducing union Splitting tee SFI base Fig. 29 SFI with splitting tee and reducing union removed 4000 MiD® Instructions, V6695...

  • Page 46: Removing And Replacing The Vac-Chip

    200 or measure the flow rate ( ). If the initi- Liquid flow rate measurement al problem persists and/or you have any queries please contact KNAUER. Removing and replacing the vac-chip Please follow the procedure below in the event that the vac-chip has to be replaced or removed.
  • Page 47 Fig. 31 Tube lens assembly and vacuum screws 13. Gently lift the tube lens assembly away from the vac-chip flange. 14. Using a pair of tweezers, remove the vac-chip from the flange (Fig. 46). 4000 MiD® Instructions, V6695...
  • Page 48 20. Once positioned on the SFD fit the four M4 screws provided. 21. Use the 4mm “T” Allen key and tighten the four M4 screws in an alter- nating criss-cross pattern until the screws are tight. 4000 MiD® Instructions, V6695...

  • Page 49: Cleaning The Vac-Chip

    (Fig. 61). 13. Gently blow dry the vac-chip with compressed air/nitrogen. Remove as much excess liquid as possible. 14. Place the vac-chip in an oven at 75 °C for 30 min to completely dry it. 4000 MiD® Instructions, V6695...

  • Page 50: Cleaning The Vac-Chip Flange

    15. The vac-chip is now clean and ready for use. If the device looks visually degraded or you have any queries please con- tact KNAUER before using the device. Cleaning the vac-chip flange The following procedure is the recommended cleaning procedure for your vac-chip flange.

  • Page 51: Troubleshooting

    Toujours porter une protection oculaire et utiliser des outils appropriés lors de la manipulation des capillaires. The following table details some basic symptoms, possible causes and potential solutions for some basic issues with the 4000 MiD. Symptom Possible Cause Remedy Cannot apply any voltages Interlock is engaged.
  • Page 52 200 (see chapter 8.2 on page 33). Severe drop in TIC back- The vac-chip is clogged. Replace the vac-chip ground accompanied with (see chapter 8.2 on page no signal for late eluting 33).. peaks in an HPLC reverse gradient chromatograph. 4000 MiD® Instructions, V6695...
  • Page 53 Vacuum pump exhaust Ensure that the tubing cuum in the Ion Guide and tubing is restricted or is free from any restricti- Analytical chambers blocked. ons. Vacuum pumps may re- Contact KNAUER. quire replacement. 4000 MiD® Instructions, V6695...

  • Page 54: Technical Data

    Technical data 11. Technical data Requirement Description Indoor use The 4000 MiD can only be used in an indoor environ- ment Bench space Required: 56cm x 35.5cm x 25.5cm (L x W x H) MiD weight: 32 kg Power Line voltage: 100–240V AC ±10 %...

  • Page 55: Appendices

    DHF – Inner diameter of the high flow tube in microns LHF – Length of the high flow tube in centimetres DLF – Inner diameter of the low flow tube in microns LLF – Length of the low flow tube in centimetres 4000 MiD® Instructions, V6695...
  • Page 56 ID for tubing ID length/cm 0.005“ (127 µm) 0.007“ (178 µm) 0.01” (254 µm) 167.8 647.6 2685.2 83.9 323.8 1342.6 55.9 215.9 895.1 42.0 161.9 671.3 28.0 107.9 447.5 21.0 81.0 335.6 16.8 64.8 268.5 4000 MiD® Instructions, V6695...
  • Page 57 0.3–2 µL/min. Appendix B: Auxiliary I/O The auxiliary I/O port (Aux I/O) is located at the rear of the 4000 MiD (see Fig. 3 on page 13). The port can be used to supply and receive analog voltages and also to send/receive triggers.
  • Page 58 Designated as Analog output tage channel 3 Analog In 0 Analog input voltage Designated as Analog input channel 1 Analog In 2 Analog input voltage Designated as Analog input channel 3 Ground Isolated Ground Isolated from main system ground 4000 MiD® Instructions, V6695...
  • Page 59 To & From Exter- Comments Connect to MiD Signal Name nal Instrument Aux I/O Pin Number Volt-free contact First side of volt-free Isolated 5V supply contact Volt-free contact Second side of volt-free First input trigger contact 4000 MiD® Instructions, V6695...
  • Page 60 Lors de la fixation du MiD à la source de déclenche- ment passif, l’utilisateur doit s’assurer que l’instrument externe est évalué pour la sortie à partir du MiD. Le fabricant n’est pas respon- sable de tout dommage à l’instrumentation externe. 4000 MiD® Instructions, V6695...
  • Page 61 Appendices 4000 MiD® Instructions, V6695...
  • Page 62 Latest KNAUER instructions online: https://www.knauer.net/en/Support/User-manuals KNAUER Phone: +49 30 809727-0 Wissenschaftliche Geräte GmbH Fax: +49 30 8015010 Hegauer Weg 38 E-Mail: info@knauer.net 14163 Berlin Internet: www.knauer.net © KNAUER 2018...

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