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Operation

4000 MiD® Instructions, V6695

6. Operation

6.1 Preparing to analyse

This section describes the steps you need to follow in order to prepare

the MiD for analysing chemical samples.

Note:

Follow each subsection in order.

6.1.1 MiD system pump-down

The MiD has to be pumped down before it can be used for analysis. To

pump the system down the user should follow the steps detailed below.

Click the“pump down“ button in the software. This will initiate the

pump down cycle. Nitrogen gas purges the interface before the va-

cuum pumps are activated.

Allow 30 minutes to ensure pump down is complete and all electro-

nics are warmed-up and functioning within their correct environmen-

tal parameters.
The base pressures in the ion guide (IG) chamber and analytical (AQ)

chamber must be below ~2.0 E-3 Torr and 5.0 E-4 Torr, respectively.

Pressure readouts for these chambers are displayed in the software.

Check these pressures are achieved before proceeding further.

To vent the system, click the vent button in the software. This will ini-

tiate the vent cycle. The user will be prompted to confirm before the

vent cycle starts.

6.2 Shutting down the MiD

The following section details the basic procedures for putting the MiD

into ‘standby’, venting the system, and powering down the system.

6.2.1 Entering ‘Standby’ mode

If using an LC system, flush the system using a mobile phase solution

containing 95% of the organic solvent. Follow the procedure descri-

bed in the corresponding software instructions.

Monitor the spray current in the software. The spray current value

turns grey when the microspray has stopped.

Click the Operate/Standby button to set the instrument to standby

mode. All high voltages and the nebuliser gas are switched off.

6.2.2 Venting the MiD

The MiD can be left in standby mode. If, however, you need to vent the

MiD to atmosphere, to change the vac-chip for example, please follow

the instructions below.

Click the vent button in the software.

A dialog appears to confirm that you wish to vent the instrument.

Click <Yes>. The MiD vents to atmosphere, and the pressures in the

analytical and ion guide chambers increase to 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.

Procedure

Содержание 4000 MiD

Страница 1: ...Mass spectrometer Instructions Document No V6695 HPLC 4000 MiD...

Страница 2: ...14163 Berlin Phone 49 30 809727 0 Fax 49 30 8015010 Internet www knauer net E Mail info knauer net Version information Article number V6695 Version number 1 0 Last update 2018 08 21 Copyright This doc...

Страница 3: ...anel 12 4 Scope of delivery 13 5 Unpacking and setup 14 5 1 Site requirements and storage conditions 14 5 2 Power supply 14 5 3 Power cords 14 5 4 The MiD and associated parts 15 5 5 Setting up the Mi...

Страница 4: ...Removing and replacing the spraychip 33 9 3 Cleaning the spraychip 34 9 3 1 Cleaning the Spraychip with DFI 34 9 3 2 Cleaning the Spraychip with SFI 34 9 4 Liquid flow rate measurement 35 9 5 Spraychi...

Страница 5: ...ng operation and maintenance of the 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 liabilit...

Страница 6: ...emical This symbol with the Warning notice denotes corrosive chemicals A corrosive chemical may be present Exposure may result in serious injury Use appropriate skin protection Note A Note indicates i...

Страница 7: ...s notices d avertissement sont aussi associ es avec des pictogrammes repr sentant des dangers sp cifiques Attention possibilit de choc electriqu Ce pictogramme d note la possibilit de choc lec trique...

Страница 8: ...quipement est utilis d une mani re non sp cifi e par le fabricant la protection fournie par l quipement peut tre alt r e Caution The MiD should only be used with accessories that meet the manufacture...

Страница 9: ...n analysing hazardous chemicals Avertissement Les gaz d chappement de la pompe du MiD doit tre connect un syst me d extraction appropri Une extraction ad quate doit galement tre fournie la zone micros...

Страница 10: ...ges voltage fluctuations and flicker in public low voltage supply systems for equipment with rated current 16 A per phase and not subject to conditional connection ICES 003 2004 Spectrum Management an...

Страница 11: ...ifies the original product or installs additional compo nents Avertissement La d claration du fabricant est annul e si l uti lisateur modifie l origine du produit ou installe des composants suppl ment...

Страница 12: ...ribed in these Instructions Avertissement NE PAS essayer de faire fonctionner l appareil avec les couvercles enlev s Des hautes tensions sont pr sentes lorsque l appareil est en fonctionnement NE PAS...

Страница 13: ...mall sample volumes for example nanolitres over long periods of time Very low solvent consumption and minimum waste when coupled to a nano LC Lower voltages are required to provide efficient electrosp...

Страница 14: ...asses through an emitter or capillary tip at a flow rate of 300 1000 nL min The voltages and flow rates used in microspray are lower than for convention al electrospray ionisation This means that lowe...

Страница 15: ...1 They are used to indicate the current operational status of the instrument the LEDs are shown in detail in Fig 2 Fig 2 LED status indicators The LEDs indicate the following statuses Red Indicates t...

Страница 16: ...panel of the MiD These ports include terminals and connectors for the gas supply vacuum exhaust system and computer peripherals Refer to the labels listed in the table below when connecting the MiD an...

Страница 17: ...Only use original parts and accessories made by KNAUER or a com pany authorized by KNAUER 4000 MiD MiDas Starter kit Mains leads 2 in total PTFE tubing form Nitrogen input Exhaust Silencer Split flow...

Страница 18: ...behind the instrument to un plug the power cord Attention Lors de l installation ou l utilisation de l instrument vous devez vous assurer qu il ya suffisamment d espace derri re l appa reil pour d bra...

Страница 19: ...o change Caution All items listed must only be supplied by the manufac turer or an agent thereof Use of alternative parts may lead to improper operation of the MiD or failure to comply with safety or...

Страница 20: ...ate and dust cap 5 5 Setting up the MiD Fig 4 shows a typical configuration of the 4000 MiD Fig 4 The 4000 MiD Caution Allow sufficient spacing around the MiD for proper cooling and for the connection...

Страница 21: ...s les r gles de sant et les r gles de s curit du pays Caution The maximum weight that can be supported by the MiD is 60 kg Attention Le poids maximum qui peut tre pris en charge par le MiD est de 60 k...

Страница 22: ...itable length of clean PTFE tubing from the gas supply to the Nebuliser Gas Port A 6 mm tubing can be used Note If replacing or refitting the gas supply tubing it is recommended that the end of the li...

Страница 23: ...r and the ion guide chamber housing the ion guide Fig 6 The SFD assembly 5 6 The spraychip flange The spraychip flange is used to connect the MiD s microspray source to the SFD and provides the nebuli...

Страница 24: ...vac chip needs to be cleaned or replaced see 8 7 Removing and replacing the vac chip on page 42 for further details To fit or remove the vac chip assembly follow the subsequent steps The vac chip ass...

Страница 25: ...Fig 9 The vac chip assembly being installed on the MiD 3 If excessive resistance is felt when fitting the assembly to the SFD stop immediately remove the assembly and retry step 2 4 Once positioned on...

Страница 26: ...ntained within the spraychip assembly 5 8 The spraychip assembly The spraychip assembly consists of the spraychip and a mounting inter face there are three available components The spraychip 200 Split...

Страница 27: ...rt Fig 11 The Split Flow Interface SFI To assemble the spraychip to the main body of the SFI use the following procedure 1 Place the PEEK screw over the metal collar as shown in Fig 11 2 Unscrew the g...

Страница 28: ...ut flow rate and liquid composition changes during a gradient Flow rates can be measured using the flow meter assembly see sec tion 8 4 Liquid flow rate measurement on page 35 For a fixed length decre...

Страница 29: ...itting a spraychip assembly to the MiD a nitrogen flush of the interface must be initialised Open the software and click the nitro gen flush button after a few seconds a flow of nitrogen gas should be...

Страница 30: ...e door in the front cover The door has two positions as shown in Fig 16 When the door is shut the safety interlock is off and high voltages can be applied his is indicated in the Status bar When the d...

Страница 31: ...from the rear of the instrument of 70dB Attention Une fois install et en fonctionnement normal ce produit a une mission de pression acoustique la position de l op rateur et de 1 m de l arri re de l in...

Страница 32: ...firm before the vent cycle starts 6 2 Shutting down the MiD The following section details the basic procedures for putting the MiD into standby venting the system and powering down the system 6 2 1 En...

Страница 33: ...nctionality of the device 7 2 Operation Qualification OQ The Operation Qualification includes an extensive functionality test accor ding to KNAUER standard OQ documents The Operation Qualification is...

Страница 34: ...using the appropriate calibration solution directly from a syringe pump 1 If the MiD is turned off switch it on and pump the instrument down as described in the section MiD system pump down 2 Fill the...

Страница 35: ...maintenance procedures the door has to be ope ned with the safety interlock engaged If in any doubt power down the instrument see the section 6 2 3 Shutting down the MiD on page 28 and perform the ma...

Страница 36: ...dures detailed in this chapter Warning Handling toxic flammable and hazardous chemicals can lead to health and safety risks Avertissement La manipulation de produits chimiques toxiques inflammables et...

Страница 37: ...assembly see Fig 32 for reference Fig 18 The Split Flow Interface SFI 7 Carefully unscrew and remove the spraychip from the DFI SFI 8 Carefully screw a new or cleaned spraychip into the assembly Note...

Страница 38: ...for use Note If an increased delay is observed on the split flow inter face SFI when using the cleaned spraychip then attempt to clean again In the event that this delay continues to be unac ceptable...

Страница 39: ...chip assembly is measured This can be performed on both the DFI and SFI To measure the liquid flow rate the flow meter assembly Fig 33 will be required Fig 19 Flow meter assembly 1 Remove the spraychi...

Страница 40: ...w when a custom split ratio is created for an SFI see 5 8 1 The Split Flow Interface SFI on page 23 If the measured flow is incorrect the user can simply change the length or diameter of the waste lin...

Страница 41: ...replace the low flow tubing located inside the DFI see 8 6 Spraychip assembly maintenance on page 38 9 5 2 Cleaning the Split Flow Interface The following procedure should be used to clean the SFI 1 F...

Страница 42: ...flow tubing should be replaced The following sections detail the procedures for replacing the tubing in both the DFI and SFI assemblies The SFI DFI tubing kit A66919 will be re quired for the followin...

Страница 43: ...removed 7 Unscrew the fingertight nuts from the input and reducing unions and remove the low flow tube 8 To fit a new low flow tube first slide the tube through one of the fingertight nuts 9 Fit the n...

Страница 44: ...e initial problem persists and or you have any queries please contact KNAUER 9 6 2 Replacing the Split Flow Interface tubing The following procedure should be used to replace the tubing inside the SFI...

Страница 45: ...e the screw retaining the tee Fig 42 Fig 28 SFI splitting tee and retaining screw 8 Remove the tee reducing union and tubing from the SFI using the plastic tweezers A66911 Fig 43 Fig 29 SFI with split...

Страница 46: ...ig 41 18 Refit the metal collar and PEEK screw by reversing steps 3 6 The SFI low flow tube has been successfully changed Fit either a spray chip 200 or measure the flow rate Liquid flow rate measurem...

Страница 47: ...he vac chip flange with five vacuum screws The vac chip is located under this assembly Fig 30 The vac chip and tube lens assembly 12 Using the Phillips head screwdriver partially unscrew the five vacu...

Страница 48: ...e Do not over tighten the vacuum screws and do not continue to tighten screws if any resistance is felt in this case remove the assembly and retry Caution The vacuum screws have been specially made fo...

Страница 49: ...th of the tube 5 Slowly turn the test tube until vertical allowing the vac chip to slide slowly to the bottom of the tube 6 Pour enough HPLC grade water into the test tube to cover the vac chip 7 Plac...

Страница 50: ...auf qu elles ont t fournies par le fabricant Caution The vac chip is fragile Always handle it with extreme caution Attention Le vac chip est fragile Toujours manipuler avec une extr me prudence 1 Clea...

Страница 51: ...owing 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 to the spraychip assembl...

Страница 52: ...flow from the syringe pump LC to the spraychip assembly Capillary tip may be clogged Change the spraychip 200 see chapter 8 2 on page 33 A voltage cannot be applied to the spraychip assembly because t...

Страница 53: ...uations increase under fixed condi tions Capillary tip may be dull or clogged Replace the spraychip 200 see chapter 8 2 on page 33 A leak in the tubing Check all fluidic connec tions Ions are in the w...

Страница 54: ...to 2000 m Temperature Operation 15 30 C Storage 10 50 C Relative humidity Operation 40 80 Pollution Degree 2 Normally only non conductive pollution occurs Occasionally however a temporary conductivit...

Страница 55: ...aste line increases the spraychip flow rate For a fixed diameter increasing the length of the waste line increases the spraychip flow rate Changing the diameter of the waste line has a greater effect...

Страница 56: ...tion 1 If the inner diameter of your desired waste tube is 254 m then Note It is always better to start with a longer piece of tubing at least 10 cm longer so that if the low flow rate is too high the...

Страница 57: ...ay D type male socket and is shown in more detail in Fig 49 Fig 35 Auxiliary I O port The port contains two optically isolated digital inputs and two optically isolated digital outputs The digital inp...

Страница 58: ...h an open ended cable for development purposes Wires will either be coloured or numbered as appropriate identifiers Auxiliary I O port pin assignments Pin Number Signal Name Description Comments 1 5 V...

Страница 59: ...n supplied with an open ended cable examples include triggering from active and passive sources All terminations not made to the MiD should be made in accordance with the relevant manufacturer s instr...

Страница 60: ...MiD The manufacturer is not responsible for any damage to external instrumentation Attention Lors de la fixation du MiD la source de d clenche ment passif l utilisateur doit s assurer que l instrument...

Страница 61: ...57 Appendices 4000 MiD Instructions V6695...

Страница 62: ...tions online https www knauer net en Support User manuals KNAUER Wissenschaftliche Ger te GmbH Hegauer Weg 38 14163 Berlin Phone Fax E Mail Internet 49 30 809727 0 49 30 8015010 info knauer net www kn...

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