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Metrohm 930 Compact IC Flex, Manual

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Metrohm 930 Compact IC Flex Manual Download Page 15

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2 Overview of the instrument

930 Compact IC Flex SeS (2.930.1400)

￭￭￭￭￭￭￭￭

7

2  Overview of the instrument

2.1 

Front

Figure 1

Front

1

Bottle holder

Offers space for the eluent bottle and addi-
tional accessories.

2

Column holder

For hanging the separation column (iCol-
umn). With column recognition.

3

Column chamber

4

Metrohm Suppressor Module (MSM)

5

Inline filter

6

Injection valve

7

Pulsation absorber

8

Base tray

With leak sensor.

Summary of Contents for 930 Compact IC Flex

Page 1: ...930 Compact IC Flex 930 Compact IC Flex SeS Manual 8 930 8007EN 2017 07 31 ...

Page 2: ......

Page 3: ...etrohm AG CH 9100 Herisau Switzerland Phone 41 71 353 85 85 Fax 41 71 353 89 01 info metrohm com www metrohm com 930 Compact IC Flex 930 Compact IC Flex SeS 2 930 1400 Manual 8 930 8007EN 2017 07 31 zst ...

Page 4: ...techcom metrohm com This documentation is protected by copyright All rights reserved This documentation has been prepared with great care However errors can never be entirely ruled out Please send comments regarding possible errors to the address above ...

Page 5: ...ng up the instrument 13 3 1 1 Packaging 13 3 1 2 Checks 13 3 1 3 Location 13 3 2 Capillary connections in the IC system 13 3 3 Removing transport locking screws 16 3 4 Connecting the drainage tubing and leak sensor 17 3 4 1 Installing the drainage tubing 17 3 4 2 Connecting the leak sensor 19 3 5 Connecting the eluent bottle 19 3 6 Installing the high pressure pump 23 3 7 Installing an inline filt...

Page 6: ... 56 5 2 Capillary connections 57 5 3 Servicing the door 57 5 4 Handling the eluent 57 5 4 1 Manufacturing eluent 58 5 4 2 Changing the eluent 58 5 5 Notes on operating the high pressure pump 59 5 6 Servicing the high pressure pump 59 5 7 Servicing the inline filter 73 5 8 Servicing the pulsation absorber 76 5 9 Injection valve 76 5 10 Metrohm Suppressor Module MSM 76 5 10 1 Notes for operating the...

Page 7: ...rohm 89 6 Troubleshooting 90 6 1 90 7 Technical specifications 94 7 1 Reference conditions 94 7 2 Instrument 94 7 3 Ambient conditions 94 7 4 Housing 95 7 5 Weight 95 7 6 Leak sensor 95 7 7 High pressure pump 95 7 8 Injection valve 96 7 9 Metrohm Suppressor Module MSM 96 7 10 Metrohm CO2 Suppressor MCS 96 7 11 Detector 97 7 12 Power connection 97 7 13 Interfaces 97 8 Accessories 98 Index 99 ...

Page 8: ...mp with purge valve 24 Figure 10 Inline filter 25 Figure 11 Pulsation absorber 25 Figure 12 Exchanging the sample loop 27 Figure 13 Metrohm Suppressor Module MSM Connection capillaries 31 Figure 14 Connecting the MCS 37 Figure 15 High pressure pump Parts 60 Figure 16 High pressure pump Cross section 67 Figure 17 Tool for piston seal 6 2617 010 68 Figure 18 Removing the piston cartridge from the pu...

Page 9: ...oise emission The intelligent MagIC Net software The 930 Compact IC Flex is operated using the MagIC Net software A USB cable is used to connect the instrument to a computer with MagIC Net installed The intelligent software detects the instrument auto matically and checks its functionality The software controls and monitors the instrument evaluates the measured data and manages it in a data base T...

Page 10: ...uent Metrohm Suppressor Module MSM The chemical suppressor MSM consists of the suppressor drive a rotor and where applicable an adapter The suppressor drive gives you the flex ibility to use different rotors according to the principle one drive many rotors Suppression rotors with different capacities and construction or a rotor for sample preparation SPM Rotor are readily interchangeable with appr...

Page 11: ... the use of the 930 Compact IC Flex requires the user to have basic knowledge and experience in handling toxic and caustic sub stances Knowledge regarding the application of fire prevention measures prescribed for laboratories is also mandatory 1 3 Safety instructions 1 3 1 General notes on safety WARNING This instrument may only be operated in accordance with the specifica tions in this documenta...

Page 12: ... electrostatic charges WARNING Electronic components are sensitive to electrostatic charges and can be destroyed by discharges Do not fail to pull the power cord out of the power socket before you set up or disconnect electrical plug connections at the rear of the instrument 1 3 3 Tubing and capillary connections CAUTION Leaks in tubing and capillary connections are a safety risk Tighten all conne...

Page 13: ...quipment The correct disposal of your old instrument will help to prevent negative effects on the environment and public health More details about the disposal of your old instrument can be obtained from your local authorities from waste disposal companies or from your local dealer 1 4 Symbols and conventions The following symbols and formatting may appear in this documentation Cross reference to ...

Page 14: ... electrical current WARNING This symbol draws attention to a possible hazard due to heat or hot instrument parts WARNING This symbol draws attention to a possible biological hazard CAUTION This symbol draws attention to possible damage to instruments or instrument parts NOTE This symbol highlights additional information and tips ...

Page 15: ...igure 1 Front 1 Bottle holder Offers space for the eluent bottle and addi tional accessories 2 Column holder For hanging the separation column iCol umn With column recognition 3 Column chamber 4 Metrohm Suppressor Module MSM 5 Inline filter 6 Injection valve 7 Pulsation absorber 8 Base tray With leak sensor ...

Page 16: ...e sensor 10 High pressure pump Pumps the eluent through the IC system 11 Metrohm CO2 Suppressor MCS 12 Detector chamber Room for the detector and the adsorption cartridge for the MCS 2 2 Rear Figure 2 Rear 1 Bottle holder 2 Drainage tubing connection For connecting the drainage tubing which guides escaped fluids away from the bottle holder ...

Page 17: ...he high pressure pump when transporting the instrument 11 Drainage tubing connections For connecting two drainage tubings that guide the escaped fluid to the leak sensor and from there to the waste container 12 Base tray With leak sensor 13 Type plate 14 Serial number 15 Leak sensor connection socket Labeled Leak Sensor For connecting the leak sensor connection cable 16 Detector connection socket ...

Page 18: ...strument and the bottle holder see Figure 5 page 12 Openings on the door Figure 3 Feed throughs on the door 1 Luer connector For connecting a capillary from inside and for inserting a syringe 6 2816 020 from outside For manual sample injection 2 Opening for capillaries For up to 3 capillaries An opening for up to 3 capillaries is located on the door of the instru ment The two Luer connections abov...

Page 19: ...el is outfitted with openings through which capil laries and cables can be lead out of the detector chamber Ducts for capillaries There are ducts for capillaries between the instrument and base tray as well as between the instrument and the bottle holder The capillaries can be fed to the front of the instrument from both sides of the instrument and from the front of the instrument to the back of t...

Page 20: ...2 3 Feed throughs for capillaries and cables 12 930 Compact IC Flex SeS 2 930 1400 Figure 5 Ducts for capillaries ...

Page 21: ...n free of vibrations protected from corrosive atmosphere and contamination by chemicals The instrument should be protected against excessive temperature fluctua tions and direct sunlight 3 2 Capillary connections in the IC system Generally speaking capillary connections between two components of an IC system are made up of one connection capillary and two pressure screws used to connect the capill...

Page 22: ...hemically inert flexible and temperature resistant up to 80 C They can be readily cut down to the desired length with the capillary cutter 6 2621 080 Use PTFE capillaries 6 1803 0x0 are used for the low pressure section PTFE capillaries with an inner diameter of 0 5 mm for sample process ing and for the transfer of rinsing solutions they are not necessarily included in the scope of delivery of the...

Page 23: ...tone 2 Slide the pressure screw over the capillary Ensure that the capillary protrudes 1 to 2 mm from the tip of the pressure screw 3 Push the capillary into the connection or coupling as far as it will go and hold it there 4 Only then start turning the pressure screw Hold the capillary in the stop position while turning it shut Colored sleeves for PEEK capillaries The enclosed set of varicolored ...

Page 24: ... instrument and labeled with Transport security screws Remove these transport locking screws before the initial start up Accessories For this step you need 4 mm hex key 6 2621 030 Removing the transport locking screws Figure 6 Removing the transport locking screws 1 Transport locking screws For the vacuum pump Only present if the instrument has a degasser or a CO2 Suppres sor MCS 2 Transport locki...

Page 25: ...ff The software displays a warning The leak sensor functions properly only if the following preconditions are met The drainage tubing is connected The leak sensor connection cable is inserted into the leak sensor con nection socket The 930 Compact IC Flex is switched on The leak sensor is switched to active in the software 3 4 1 Installing the drainage tubing Liquid that leaks in the bottle holder...

Page 26: ...e bottle holder 3 Attach one end of the 20 cm long piece to the drainage tubing con nection on the detector chamber 4 Attach each of the loose ends of both pieces of silicone tubing to one end of the Y connector 5 Attach one end of the second 40 cm long piece to the third end of the Y connector Attach the loose end to the right side drainage tubing connection on the base tray 6 Attach one end of t...

Page 27: ...he leak sen sor connection socket labeled Leak Sensor 3 5 Connecting the eluent bottle The eluent is aspirated out of the eluent bottle via the eluent aspiration tubing The eluent aspiration tubing is installed on the entry to the high pressure pump The tubing must be be fed out of the instrument through a suitable open ing see Openings on the back panel page 11 before the loose end can be connect...

Page 28: ...e cap 6 1602 160 Start by pushing the M8 tubing nipple onto the loose end of the eluent aspiration tubing followed by the O ring Push the loose end of the eluent aspiration tubing through the M8 opening of the bottle cap and screw it on for the time being Figure 7 Installing the eluent bottle cap 2 Mounting the tubing adapter Install the parts of the tubing adapter for aspiration filter 6 2744 210...

Page 29: ...an also be found in the video Inserting a new aspi ration filter at the following link ic help metrohm com 4 Mounting aspiration filter NOTE Always wear gloves when handling the aspiration filter Place the loose end of the eluent aspiration tubing into the aspira tion filter The end of the tubing should reach approximately to the center of the aspiration filter Tighten the aspiration filter to the...

Page 30: ...t 6 Mounting the adsorber tube NOTE Depending on the eluent used the adsorber tube 6 1609 000 must be filled differently For alkaline eluents or eluents with a low buffer capacity first a little cotton then with CO2 adsorber material For all other eluents only with cotton Remove the plastic cover from the large opening of the adsorber tube Fill the adsorber tube and close it again using the plasti...

Page 31: ...ation high pressure pump pumps the eluent through the system It is equipped with a chip where its technical specifi cations and life history operating hours service data etc are saved The high pressure pump consists of The pump head which pumps the eluent through the system The purge valve used for bleeding the pump head ...

Page 32: ...llation work is required 3 7 Installing an inline filter Inline filters protect the separation column reliably from potential contami nation from the eluent The small filter pads with 2 µm pore size can be replaced quickly and easily They remove particles from the solutions An inline filter 6 2821 120 is installed between the purge valve and the pulsation absorber as protection against particles ...

Page 33: ...sorber The pulsation absorber is installed between the high pressure pump and the injection valve It protects the separation column from damage caused by pressure fluctuations e g when the injection valve is switched and reduces interfering pulsations during highly sensitive measurements Figure 11 Pulsation absorber 1 Connection capillary Connection to inline filter 2 PEEK pressure screws short 6 ...

Page 34: ...0 Dosino when the Metrohm intelligent Partial Loop Injection Technique MiPT is used The choice of sample loop depends on the application The following sample loops are normally used Table 1 Which sample loop do I need Application Sample loop Cation determination 20 µL Anion determination with suppression 20 µL Anion determination without suppression 100 µL MiPT 250 µL The injection valve is comple...

Page 35: ...e free installation of the sample loop see Creat ing dead volume free capillary connections page 15 1 Removing the existing sample loop Loosen the pressure screws 6 2744 010 at Port 3 and Port 6 Remove the sample loop 2 Installing a new sample loop Fasten one end of the sample loop to Port 3 using a PEEK pressure screw 6 2744 010 Use the second PEEK pressure screw 6 2744 010 to fasten the other en...

Page 36: ...using A connecting piece 6 2835 010 is used for all rotors for connecting the Metrohm Suppressor Module MSM to the IC system 6 2842 000 6 2842 020 6 2844 000 6 2842 020 6 2832 000 NOTE The instruments are supplied without rotor and without adapter The suitable rotor and the adapter if required must be ordered sepa rately 3 10 1 Inserting the rotors Accessories For this step you need the following ...

Page 37: ...0 6 2842 200 1 Removing the union nut Loosen the union nut and remove it 2 Inserting the rotor Clean the sealing surface of the rotor with ethanol using a lint free cloth Insert the rotor into the suppressor drive so that the tubing con nections on the rear of the rotor fit into the corresponding recesses inside the suppressor drive and one of the three holes of the rotor is visible from below in ...

Page 38: ...Inserting the connecting piece Clean the sealing surface of the connecting piece with ethanol using a lint free cloth Insert the connecting piece into the suppressor drive so that con nector 1 is on top and the three pins of the connecting piece fit into the corresponding recesses on the suppressor drive 4 Attaching the union nut Tighten the union nut on the thread of the suppressor drive by hand ...

Page 39: ... rotor is visible in the slot of the adapter 2 Inserting the adapter Insert the adapter into the suppressor drive just like a large rotor see Inserting large rotors page 29 3 10 2 Connecting the Metrohm Suppressor Module MSM The three entries and exits of the suppressor units numbered 1 2 and 3 on the connecting piece each have two permanently installed PTFE capil laries Figure 13 Metrohm Suppress...

Page 40: ...to the waste container 6 rinsing solution Inlet capillary for the rinsing solution Recommended installation Alternative installation 3 10 2 1 Installing the eluent path The eluent path is connected with the capillaries in and out 1 Connect the capillary labeled in to the outlet of the separation col umn using a short pressure screw 6 2744 070 2 Use a long pressure screw 6 2744 090 to connect the c...

Page 41: ...rom the accessory kit IC Vario Flex SeS 6 5000 020 Accessories from IC equipment Dosino Regeneration 6 5330 190 3 10 2 3 Connecting the regeneration solution The regeneration solution is connected to the regenerant capillary Connecting the regeneration solution to a Dosino For this step you need the following accessories Dosino 2 800 0010 Accessory kit Flex Vario SeS 6 5000 020 IC equipment Dosino...

Page 42: ... 080 to fasten the other end of the PTFE capillary to Port 1 of the Dosino 4 Connect the FEP tubing 6 1805 120 from the bottle with the regen eration solution to Port 2 of the Dosino 3 10 2 4 Connecting the rinsing solution Various possibilities exist for rinsing the Metrohm Suppressor Module Rinsing solution via STREAM recommended Use the eluent from the conductivity detector as rinsing solution ...

Page 43: ...ector outlet capillary must not be shortened Connecting the rinsing solution inlet to the Dosino The rinsing solution capillary can be connected to the Dosino to which the regenerant capillary is already connected For this step you need the following accessories not contained in its entirety in the standard accessories 3 short pressure screws 6 2744 070 Inline filter 6 2821 120 PTFE capillary 6 18...

Page 44: ... Suppressor MCS 3 11 1 General information on the MCS NOTE The Metrohm CO2 Suppressor MCS is used only in conjunction with conductivity detection with chemical suppression The Metrohm CO2 Suppressor MCS removes the CO2 from the eluent stream This lowers the background conductivity improves detection sen sitivity and minimizes the injection peak and carbonate peak CO2 can enter the eluent stream th...

Page 45: ...necting the MCS The MCS is connected between the Metrohm Suppressor Module MSM and the conductivity detector Connecting the MCS Figure 14 Connecting the MCS 1 Air aspiration capillary For drawing in air with low CO2 content via the CO2 adsorption cartridge 2 Pressure screw short 6 2744 070 Installed on the air aspiration capillary 3 Luer coupling 6 2744 120 Mounted on the air aspiration capillary ...

Page 46: ... order for the CO2 to be removed from the eluent efficiently In order to achieve this the air is aspirated through a CO2 adsorption cartridge CW 6 2837 100 Accessories For this step you need the following accessories Adsorption cartridge holder 6 2057 080 with two clips CO2 adsorption cartridge CW 6 2837 100 All of the parts are located in one accessory kit Vario Flex SeS 6 5000 020 Preparing the ...

Page 47: ...spirated The CO2 adsorption cartridge CW is now ready for installation NOTE The new CO2 adsorption cartridge CW 6 2837 100 works without attached H2O adsorption cartridge Installing the CO2 adsorption cartridge CW Accessories Adsorption cartridge holder 6 2057 080 Prepared CO2 adsorption cartridge CW 6 2837 100 CAUTION The following preparatory steps absolutely must be carried out for CO2 suppress...

Page 48: ...slots on the adsorption cartridge holder 2 Connecting the CO2 adsorption cartridge CW Attach the capillary connected to the Metrohm CO2 Suppressor s MCS Air in connection to the tip of the CO2 adsorption cartridge CW 3 Inserting the adsorption cartridges into the adsorption car tridge holder Clamp the CO2 adsorption cartridge CW in place using the clips on the adsorption cartridge holder ...

Page 49: ...The detector is available as separate device and is supplied with a separate manual Placing the detector in the instrument Follow the instructions in the chapter Inserting the detector in the manual for the detector Connecting the detector to the eluent path NOTE The separation column is not inserted into the instrument until it is being started up for the first time Until then the detector inlet ...

Page 50: ...ories in the detector chamber The detector is available as separate device and is supplied with a separate manual Placing the detector in the instrument Follow the instructions in the chapter Inserting the detector in the manual for the detector 3 14 Connecting the instrument to a computer NOTE If the instrument is connected to the computer then it must be switched off Accessories For this step yo...

Page 51: ...k from electrical potential Risk of injury by touching live components or through moisture on live parts Never open the housing of the instrument while the power cord is still connected Protect live parts e g power supply unit power cord connecting socket from moisture Unplug the power plug immediately if you suspect that moisture has gotten inside the instrument Only personnel who have been issue...

Page 52: ...e protective ground protection class I 3 16 Initial start up Even before the guard column and separation column are installed the entire system must be completely rinsed with eluent for the first time Rinsing the IC system CAUTION The separation column and the guard column are not permitted to be installed at the time of the initial start up Make sure that a coupling 6 2744 040 is being used inste...

Page 53: ... bottles are being used for rinsing and regeneration Ensure that the aspiration tubings for the aux iliary solutions regeneration solution and rinsing solution are immersed in the respective solutions and that there is enough solution in both bottles Check whether the detec tor outlet capillary is guided into the waste container or is connected with the waste collector Switch on the instrument Mag...

Page 54: ...inutes 3 17 Connecting and rinsing the guard column Guard columns protect separation columns and significantly increase their service life The guard columns available from Metrohm are either actual guard columns or guard column cartridges used together with a cartridge holder The process of installing a guard column cartridge into the corre sponding holder is described in the guard column leaflet ...

Page 55: ...trument has already been put into operation once see Chapter 3 16 page 44 The guard column and the separation column have to be replaced by a cou pling 6 2744 040 until then Accessories For this step you need the following accessories Guard column suitable for separation column Connecting the guard column 1 Removing the coupling Remove the coupling 6 2744 040 installed between the column inlet cap...

Page 56: ...ontrol Pump Flow in accordance with column leaflet On Rinse the guard column with eluent for approx 5 minutes Stop the high pressure pump in the manual control in MagIC Net again Off 3 18 Connecting the separation column The smart separation column iColumn is the heart of ion chromato graphic analysis It separates the different components according to their interactions with the column Metrohm sep...

Page 57: ...s area or request them from your responsible Metrohm representative free of charge CAUTION New separation columns are filled with a solution and sealed with stop pers on both sides Before inserting the column ensure that this solu tion can be mixed with the eluent being used follow the information provided by the manufacturer NOTE Connect the separation column only after the initial start up of th...

Page 58: ...3 18 Connecting the separation column 50 930 Compact IC Flex SeS 2 930 1400 Connecting the separation column 1 Removing the stoppers Remove the stoppers from the separation column ...

Page 59: ... 2744 070 3 Rinsing the separation column Place a beaker under the outlet of the separation column Start manual control in MagIC Net and select the high pressure pump Manual Manual control Pump Flow Increase gradually up to the flow rate recommended in the column leaflet On Rinse the separation column with eluent for approx 10 minutes Stop the high pressure pump in the manual control in MagIC Net ...

Page 60: ... the flow rate permitted for the corresponding column refer to the column leaflet and chip data record Start the MagIC Net computer program Open the Equilibration tab in MagIC Net Work place Run Equilibration Select or create a suitable method Also see MagIC Net Tutorial and online help 2 Preparing the instrument Ensure that the column is inserted correctly in accordance with the flow direction ma...

Page 61: ...g out anywhere tighten the corresponding pressure screw further or loosen the pressure screw check the end of the capil lary and shorten it using the capillary cutter if necessary and retighten the pressure screw 4 Conditioning the system Continue rinsing the system with eluent until the desired stability level for the baseline has been attained The instrument is now ready for measuring samples ...

Page 62: ...t IC Flex SeS 2 930 1400 4 Operation The 930 Compact IC Flex SeS is operated solely using the MagIC Net soft ware You can find information on operating the software in the tutorial for MagIC Net or in the online help ...

Page 63: ...strument has been designed so that liquid is largely prevented from being able to get inside the instrument However unplug the power plug immediately if you suspect that corrosive media have got ten inside the instrument This is the only way to prevent extreme dam age to the instrument electronics Notify Metrohm Service WARNING Electric shock caused by live parts Never open the housing of the inst...

Page 64: ...ectly with each other using a coupling 6 2744 040 3 Rinse the IC system for 15 minutes with methanol ultrapure water mixture 1 4 4 Optional Only if the IC system is equipped with a suppressor In the software switch the Metrohm Suppressor Module MSM twice during the rinsing process at five minute intervals in each case STEP command 5 Optional Only if the IC system is equipped with a suppressor and ...

Page 65: ...ing it Only hold the instrument by the housing 5 4 Handling the eluent Careful handling of the eluent ensures stable analysis results Keep the fol lowing general measures in mind when handling the eluent The supply bottle with the eluent must be connected as indicated in chapter 3 5 page 19 This is particularly important for eluents with vol atile solvents e g acetone Avoid condensation in the elu...

Page 66: ...horter retention times and faster separation but also to a higher background conductivity sig nal pH pH changes lead to shifts in dissociation equili bria and thus to changes in retention times Organic solvents Adding organic solvents e g methanol acetone or acetonitrile to a watery eluent generally speeds up lipophilic ions 5 4 2 Changing the eluent Ensure that no precipitates can form when chang...

Page 67: ... Salt crystals between the piston and seal cause abrasive particles that can find their way into the eluent These particles lead to contaminated valves an increase in pressure and in extreme cases scratched pistons and thus to leakages in the high pressure pump Immediately successive solutions must always be miscible If the system must be rinsed with organic solvents use several solvents with risi...

Page 68: ...ctor Consists of a coupling with a pressure screw 8 Pressure screw short 6 2744 070 Fastened to the pump output Maintenance interval The following parts of the high pressure pump must be serviced at least once per year Inlet valve 6 2824 170 Outlet valve 6 2824 160 Piston seal 6 2741 020 Zirconium oxide piston 6 2824 070 Maintenance tasks can also be carried out if the following problems occur Uns...

Page 69: ...ve piston b Dismantle the piston c Replace the piston seal d Replace the zirconium oxide piston e Assemble the piston f Insert the piston 4 Reinstall the pump head You can find brief video sequences on the following maintenance steps on the Internet at http ic help metrohm com Servicing the outlet valve and inlet valve Accessories For this step you need the following accessories You can find these...

Page 70: ...e outlet valve from the outlet valve holder 3 2 Cleaning the outlet valve Start by rinsing the outlet valve in the direction of eluent flow using a wash bottle filled with ultrapure water RBS solution or acetone The direction of eluent flow is marked on the valve by an arrow The rinsing solution must come out at the valve outlet If no more solution comes out then the valve is blocked Rinse the out...

Page 71: ...rt the outlet valve into the outlet valve holder the seal must be visible 1 Screw the outlet valve holder up into the pump head 2 and tighten it firmly by hand and then retighten it one additional turn using the adjustable wrench 3 Tighten the connection capillary to the auxiliary piston back onto the outlet valve holder ...

Page 72: ... inlet valve from the inlet valve holder 3 2 Cleaning the inlet valve Start by rinsing the inlet valve in the direction of eluent flow using a wash bottle filled with ultrapure water RBS solution or ace tone The direction of eluent flow is marked on the valve by an arrow The rinsing solution must come out at the valve outlet If no more solution comes out then the valve is blocked Rinse the inlet v...

Page 73: ...nd then retighten it one additional turn using the adjustable wrench 3 Refasten the connection capillary to the connection of the eluent aspiration tubing 15 7 Removing the pump head Accessories For this step you need the following accessories You can find these parts in the accessory kit Vario Flex Basic 6 5000 000 4 mm hex key 6 2621 030 Removing the pump head Prerequisites Is the high pressure ...

Page 74: ...ve the pressure screw on the pump head s outlet 15 8 3 Loosen and remove the four fastening screws 15 3 using the hex key 4 Remove the pump head 15 4 Servicing the piston Carry out the following work on both pistons in turn Servicing a piston consists of the following tasks 1 Replace the piston seal 2 Clean or replace the zirconium oxide piston 3 Reinstall the piston ...

Page 75: ... 6 Inlet valve 6 2824 170 7 Inlet valve holder 8 Zirconium oxide piston 6 2824 070 9 Piston cartridge Accessories For this step you need the following accessories You can find these parts in the accessory kit Vario Flex Basic 6 5000 000 Adjustable wrench 6 2621 000 Tool for piston seals 6 2617 010 consisting of a tip 17 1 for remov ing the old piston seal and a sleeve 17 2 for inserting the new pi...

Page 76: ...on seal 6 2741 020 Replacing the piston seal Figure 18 Removing the piston cartridge from the pump head 1 Piston cartridge 2 Backup ring 1 Removing the piston cartridge Loosen the piston cartridge 18 1 using the adjustable wrench and then unscrew it from the pump head by hand Set it aside 2 Removing the backup ring Shake the backup ring 18 2 out of the piston opening Set it aside ...

Page 77: ...ew piston seal into the tool Insert the new piston seal into the recess of the sleeve 19 1 of the tool for piston seal The sealing spring must be visible from the out side Figure 19 Inserting the piston seal into the tool 1 Tool for piston seal 6 2617 010 Sleeve for inserting the new piston seal 2 Piston seal 6 2741 020 5 Inserting the new piston seal into the pump head Guide the sleeve 17 2 of th...

Page 78: ...opening the piston cartridge counteract the pressure from the spring and carefully unscrew the cartridge Loosen the piston cartridge s screw with an adjustable wrench and carefully unscrew the screw by hand while counteracting the pressure from the taut spring Remove the zirconium oxide piston and place it on a paper towel Remove the spring retainer the spring and the inner plastic sleeve from the...

Page 79: ...sher Assemble the retaining washer at the same point on the new pis ton 4 Putting the piston cartridge together Insert the inner plastic sleeve the spring and the spring retainer into the piston cartridge Slide the zirconium oxide piston carefully into the piston cartridge until its tip emerges from the small opening of the piston car tridge Attach the screw and tighten it by hand Mounting the pis...

Page 80: ...mounted the wrong way as it has fastening bolts with different bore hole depths i e one fastening bolt is longer than all others The bore hole with the greatest depth must therefore be aligned with the longest bolt 1 Push the pump head onto the four fastening bolts 1 Tighten the four fastening screws using the hex key 6 2621 030 alternating crosswise ...

Page 81: ...t 2 5 7 Servicing the inline filter NOTE You can find a video sequence for this task in the Multimedia Guide IC Maintenance or on the Internet at http ic help metrohm com Maintenance interval The filter must be replaced at least every 3 months it may need to be replaced more frequently depending on the application Accessories For this task you need the following accessories Two adjustable wrenches...

Page 82: ... Part of the acces sories 6 2821 120 3 Filter 6 2821 130 Pack contains 10 pieces 1 Shutting off the flow Switch off the high pressure pump in the software 2 Removing the inline filter Unscrew both pressure screws from the inline filter 3 Unscrewing the filter screw Use two adjustable wrenches 6 2621 000 to loosen the filter screw 21 2 from the filter housing 21 1 and unscrew it by hand 4 Removing ...

Page 83: ...ilter screw 21 2 back into the filter housing 21 1 and tighten by hand Then use two adjustable wrenches 6 2621 000 to tighten it slightly 3 Remounting the inline filter Screw pressure screws back onto the inline filter Take care to ensure that the flow direction matches that inscribed on the inline filter 4 Rinsing the inline filter Dismantle the guard column if present and the separation col umn ...

Page 84: ...utlet capillaries according to the diagram outlined in Chapter Connecting the Metrohm Suppressor Module MSM page 31 The Metrohm Suppressor Module MSM consists of three suppressor units which in rotation are 1 used for suppression 2 regenerated with regeneration solution and 3 rinsed with ultrapure water or with suppressed eluent In order to record each new chromatogram under comparable conditions ...

Page 85: ...ssor housing CAUTION The transparent suppressor housing can become fogged The suppressor housing is made of PMMA poly methyl methacrylate It can become scratched and foggy if cleaned improperly This can make viewing the rotor difficult or impossible Do not use any scouring agents for cleaning Do not use any solvents for cleaning 5 10 3 Servicing the Metrohm Suppressor Module MSM 5 10 3 1 Parts of ...

Page 86: ... heavy metals or elevated backpressure 1 mol L H2SO4 0 1 mol L oxalic acid Contamination with organic cationic complexing agents 0 1 mol L H2SO4 0 1 mol L oxalic acid acetone 5 Heavy contamination with organic substances 0 2 mol L H2SO4 acetone 20 Contamination by certain environmental samples 1 mol L H3PO4 NOTE If phosphoric acid has been used once as regeneration solution in an IC system you wil...

Page 87: ...generant from the coupling 3 Rinsing the Metrohm Suppressor Module MSM After regeneration each of the three suppressor units must be rinsed with degassed ultrapure water for about 15 minutes Connect the capillary labeled rinsing solution to the outlet of the high pressure pump using a coupling 6 2744 040 Set the flow of the high pressure pump to 0 5 mL min in the soft ware Connect the ultrapure wa...

Page 88: ...system with eluent until the suppressor unit is completely exhausted indicated by a significant increase in conductivity This can take up to 240 minutes under standard conditions 3 Regenerating the second cation suppressor unit In the software use the Step command to switch to the next sup pressor unit Repeat step 2 4 Regenerating the third cation suppressor unit In the software use the Step comma...

Page 89: ... the housing you can push it out as fol lows Put a pointed object into the slot in the housing and use it to push out the rotor Loosen the connecting piece from the rotor with a turning move ment 3 Rinsing the capillaries Connect each of the six PTFE capillaries connected to the connect ing piece 22 2 in sequential order to the high pressure pump and pump ultrapure water through them Check whether...

Page 90: ...urning If the rotor cannot be turned or removed it can be moved into the correct position from below by means of a pointed object e g a screwdriver 6 Cleaning the connecting piece Clean the sealing surface of the connecting piece 22 2 with ethanol using a lint free cloth 7 Inserting the connecting piece See also Chapter 3 10 1 page 28 Insert the connecting piece 22 2 into the housing in such a way...

Page 91: ...trohm Suppressor Module MSM from the IC system Switch off the instrument Disconnect all capillaries of the MSM from the IC system 2 Dismantling the Metrohm Suppressor Module MSM Unscrew the union nut 22 1 from the housing 22 4 Pull the connecting piece 22 2 out of the housing together with the rotor 22 3 If the rotor gets stuck in the housing you can push it out as fol lows Put a pointed object in...

Page 92: ...e suppressor drive if the rotor is inserted correctly If this is not the case then the rotor must be moved into the cor rect position using careful turning If the rotor cannot be turned or removed it can be moved into the correct position from below by means of a pointed object e g a screwdriver 5 Cleaning the new connecting piece Clean the sealing surface of the new connecting piece 22 2 with eth...

Page 93: ...sorption car tridges CW are available under the order number 6 2837 100 Maintenance interval The CO2 adsorption cartridge CW 6 2837 100 loses capacity over time Depleted cartridges change their color to violet New cartridges are white The CO2 adsorption cartridge CW needs to be replaced once of its color has changed to violet after 12 months at the latest Removing the depleted CO2 adsorption cartr...

Page 94: ...y of the peristaltic pump or of the Dosino that is used for the sample transfer The total capillary volume The volume of the gas removed from the sample by the sample degas ser if a sample degasser is present and connected The transfer time can be determined as follows Determining the transfer time 1 Emptying the sample path Pump air through the sample path pump tubing tubing connec tions capillar...

Page 95: ...r this ratio the smaller the amount of sample carry over This ratio can be changed by varying the rinsing time This can be used to determine the required rinsing time for the application 5 14 Separation column 5 14 1 Separating efficiency The analysis quality that can be attained depends in a large part on the separating efficiency of the separation column being used The separating efficiency of t...

Page 96: ...om your Metrohm representative the leaflet provided along with your separation column or the product information about the separation column at http www metrohm com Ion Chromatography product area or it can be obtained directly from your representative Use the pulsation absorber 5 14 3 Storing the separation column Always store separation columns you do not need in a sealed and filled state accord...

Page 97: ...struments and software Qualification Please contact your local Metrohm representative for support in qualifica tion of instruments and software The Installation Qualification IQ and Operational Qualification OQ are offered by Metrohm represen tatives as a service They are carried out by trained employees using stand ardized qualification documents and in accordance with the currently applicable re...

Page 98: ...uality of the chemicals and the water High pressure pump Defective piston seals Replace the piston seals see Chapter 5 6 page 59 MCS The CO2 adsorber cartridge CW is depleted Replace the CO2 adsorber cartridge CW see Chapter 5 11 1 page 85 The pulsation absorber is not connected or is defec tive Connect see Chapter 3 8 page 25 or replace the pulsation absorber MCS The vacuum pump is defective Cont...

Page 99: ... concen tration Create eluent with correct concentration Separation column Diminished separating effi ciency Regenerate the separation column see Chapter 5 14 4 page 88 Replace the separation column see Con necting the separation column page 50 The eluent contains gas bubbles Deaerate the high pressure pump see Fig ure page 45 High pressure pump Defective Request Metrohm Service Peak areas are low...

Page 100: ...ct the MSM see Chapter 3 10 page 28 The incorrect eluent is being used Change the eluent see Chapter 5 4 2 page 58 MSM No or insufficient flow of regeneration solu tion or rinsing solution Check the flow of the regeneration solution and of the rinsing solution MCS The CO2 suppressor is not connected Connect the CO2 suppressor The retention times are poorly reprodu cible The eluent path has a leak ...

Page 101: ...n ished efficiency Replace the guard column see Chapter 3 17 page 46 Separation column Dead volume at the column head Install the separation column in the oppo site flow direction if the leaflet says this is permissible and rinse into a beaker Replace the separation column see Con necting the separation column page 50 Precision problems the measured values are highly scattered Injection valve Samp...

Page 102: ... equilibrium 7 2 Instrument IC system Metal free IC system Compact system with modular design Material Painted CFC free polyurethane hard foam fire class V0 Operating pres sure range 0 50 MPa 500 bar high pressure pump 0 35 MPa 350 bar standard PEEK system Intelligent com ponents iPump iDetector iColumn MagIC Net 7 3 Ambient conditions Operation Ambient tem perature 5 45 C Humidity 20 80 relative ...

Page 103: ...23 67 kg without accessories 7 6 Leak sensor Type Electronic no calibration necessary 7 7 High pressure pump Type Serial dual piston pump Intelligent pump head recognition Chemically inert Metal free pump heads Materials in contact with the eluent PEEK ZrO2 PTFE PE Self optimizing flow and pressure Flow rate Adjustable flow range 0 001 20 mL min 0 01 5 mL min with standard PEEK pump head Flow incr...

Page 104: ...0 MPa The shutdown mechanism becomes active two minutes after sys tem start The pump is automatically shut down after three piston strokes below the minimum pressure limit 7 8 Injection valve Actuator switch ing time typ 100 ms Maximum operat ing pressure 35 MPa 350 bar Material PEEK 7 9 Metrohm Suppressor Module MSM Resistance to sol vents No restriction Switching time typ 100 ms 7 10 Metrohm CO2...

Page 105: ...standby conductivity detector to 40 C Power supply unit Up to 300 W maximum electronically monitored internal fuse 3 15 A 7 13 Interfaces USB Input 1 USB upstream type B labeled PC for connecting to a computer Output 2 USB downstream type A labeled USB 1 and USB 2 MSB 2 MSB 8 pin Mini DIN female labeled MSB 1 and MSB 2 for Dosino stirrer remote lines etc Detector 1 15 pin high density D sub female...

Page 106: ...wser 2 Under Find products accessories and applications by enter the article number e g 2 930 1400 The search result is displayed 3 Under Products click on More information Detailed information regarding the product is shown on various tabs 4 On the Included parts tab click on Download the PDF The PDF file with the accessories data will be created NOTE When you receive your new instrument we recom...

Page 107: ...Equilibration 45 52 F Feed through For cables 10 For capillaries 10 Filter Aspiration filter 57 see Inline filter 24 Flow fluctuations 60 Flow increment 95 Flow range 95 Flow rate 95 Frequency 97 G Guard column Installation 46 Rinse 48 H Heavy metals Contamination of suppressor 78 High pressure pump Maintenance 59 Protection 17 59 Technical specifications 95 Housing 95 Humidity 94 I IC column see ...

Page 108: ...ty shutdown 96 Sample Carry over 86 Sample loop 26 Transfer time 86 Sample loop 26 Sample path Rinse 86 Separation column Installation 48 Protection 2 25 88 Regeneration 88 Rinse 51 Separating efficiency 87 Storage 88 Service 3 55 Shutting down 56 Storage 94 Supply voltage 4 97 Suppression rotor see Suppressor 78 80 Suppressor Clean 80 Install rotor 28 Installation 28 Maintenance 76 Operation 76 R...

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