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Technical Communication Metrohm AG CH-9100 Herisau 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.
3.14 Connecting the instrument to the power grid ....26 3.15 Initial start-up ..............27 3.16 Connecting and rinsing the guard column ....... 29 3.17 Connecting the separation column ........31 3.18 Conditioning ................ 35 4 Operation ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Protecting the separation column .......... 62 5.13.3 Storing the separation column ..........62 5.13.4 Regenerating the separation column ........62 5.14 Quality management and qualification with Metrohm ... 63 6 Troubleshooting ..................... 64 7 Technical specifications Reference conditions ............67 Instrument ................
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■■■■■■■■■■■■■■■■■■■■■■ Table of contents Injection valve ..............70 7.10 Detector ................70 7.11 Power connection ............... 70 7.12 Interfaces ................70 8 Accessories Index ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Removing the piston cartridge from the pump head ......52 Figure 18 Inserting the piston seal into the tool ..........53 Figure 19 Parts of the piston cartridge ............54 Figure 20 Inline filter – Removing the filter ............58 ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Leak sensor The leak sensor detects leaking liquid that collects in the instrument's base tray. Liquid that leaks in the instrument is routed to the base tray using drainage tubing and detected there. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Detector Metrohm offers a series of different detectors for various analysis tasks. A suitable detector type must be ordered as a separate device. Separation column The intelligent separation column separates different components accord- ing to their interactions with the column.
Front Bottle holder Column holder Offers space for the eluent bottle and addi- For hanging the separation column (iCol- tional accessories. umn). With column recognition. Column oven Inline filter Injection valve Pulsation absorber ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Pumps the eluent through the IC system. Offers space for an embedded detector and additional accessories. Rear Figure 2 Rear Bottle holder Drainage tubing connection For connecting the drainage tubing, which guides escaped fluids away from the bottle holder. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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For connecting the instrument to the com- USB devices. puter with the USB cable (6.2151.020). 19 Power socket Power socket for connecting the power cable and power switch for switching the instrument on and off. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
The two Luer connections above are not actually openings; the capillaries are fastened to the Luer connection from within using PEEK pressure screws. You can use a syringe to inject or draw out liquid from the out- side. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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 the instrument. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
High-pressure pump, purge valve, inline filter, pulsation absorber, separation columns 6.2744.090 Pressure screw, long MCS, sample degasser, 10- port valve Pressure screws are tightened and loosened by hand. A tool is not nee- ded. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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(6.2739.000). ■ In order to achieve optimum analysis results, capillary connections in an IC system must be absolutely tight and free of dead volume. Dead volume ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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2 Heat the colored sleeve, e.g. with a hairdryer. The colored sleeve shrinks and adapts to the shape of the capillary. NOTE In order to arrange capillaries more clearly, they can be bundled with the spiral band (6.1815.010). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
For the vacuum pump. Only present if the For the high-pressure pump. instrument has a degasser or a CO Suppres- sor (MCS). 1 Remove all of the transport locking screws with the hex key. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Accessories For this step you need the following parts from the accessory kit: Vario/ Flex Basic (6.5000.000): 2 × silicone tubing (6.1816.020) ■ Y connector (6.1807.010) ■ You also need scissors. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Attach the loose end to the right-side drainage tubing connection on the base tray. 6 Attach one end of the second piece of silicone tubing to the left-side drainage tubing connection on the base tray. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
The temperature of the column oven can be configured in the software. The column oven is completely connected. No installation work is required. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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 ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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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 filter holder. ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Then fix it in place using the M8 tubing nipple. Seal the M6 opening on the bottle cap with the M6 threaded ■ stopper from the accessory set. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Fill the adsorber tube and close it again using the plastic cover. Insert the adsorber tube into the bottle cap's large opening. Fas- ■ ten it to the bottle cap using the SGJ clip (6.2023.020). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
■ The purge valve used for bleeding the pump head. ■ Figure 9 High-pressure pump with purge valve Pump head Purge valve The high-pressure pump is completely connected. No installation work is required. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
The quantity of sample solution injected is determined by: the volume of the sample loop or ■ by an 800 Dosino when the Metrohm intelligent Partial Loop Injection ■ Technique (MiPT) is used. The choice of sample loop depends on the application. The following...
Only use PEEK pressure screws (6.2744.010) to connect capillaries and the sample loop to the injection valve. Figure 12 Exchanging the sample loop Pressure screw Sample loop Fastened to Port 6. Pressure screw Fastened to Port 3. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
(6.2744.040). Accessories For this step, you need the following accessories: Coupling (6.2744.040) ■ 2 × pressure screw (6.2744.010) ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
If the instrument is connected to the computer, then it must be switched off. Accessories For this step, you need the following accessories: USB connection cable (6.2151.020) from the accessory kit: Vario/Flex ■ Basic (6.5000.000) ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Unplug the power plug immediately if you suspect that moisture has ■ gotten inside the instrument. Only personnel who have been issued Metrohm qualification may ■ perform service and repair work on electrical and electronic parts. ■■■■■■■■...
Also see: MagIC Net Tutorial and online help. 2 Preparing the instrument Ensure that the eluent aspiration tubing is immersed in the eluent ■ and that there is enough eluent in the eluent bottle. Switch on the instrument. ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Switch off the high-pressure pump in MagIC Net. ■ Seal the purge valve using the rotary knob. ■ Remove the syringe from the purge needle. ■ Pull the purge needle out of the purge capillary. ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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.
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When inserting the guard column, ensure that it is inserted cor- rectly based on the marked flow direction (if specified). Fasten the inlet of the guard column to the column inlet capillary ■ using a short pressure screw (6.2744.070). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
NOTE Information regarding which separation column is suitable for your application can be found in the Metrohm Column Program, the product information for the separation column or it can be obtained through your representative.
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(follow the information provided by the manufacturer). NOTE Connect the separation column only after the initial start-up of the instrument. Until that point, insert a coupling (6.2744.040) instead of the guard column and separation column. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Connecting the separation column 1 Removing the stoppers Remove the stoppers from the separation column. ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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6 Inserting the separation column Insert the separation column with the chip into the column holder ■ until you hear it snap in place. The separation column is now detected by MagIC Net. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Ensure that the eluent aspiration tubing is immersed in the eluent ■ and that there is enough eluent in the eluent bottle. 3 Starting equilibration Start the equilibration in MagIC Net: Workplace ▶ Run ▶ Equili- ■ bration ▶ Start HW. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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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. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
The 930 Compact IC Flex Oven is operated solely using the MagIC Net software. You can find information on operating the software in the tuto- rial for MagIC Net or in the online help. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Maintenance by Metrohm Service Maintenance of the instrument is best carried out as part of an annual service performed by specialist personnel from Metrohm. A shorter main- tenance interval is recommended if you frequently work with caustic and corrosive chemicals. Metrohm Service offers every form of technical advice for maintenance and service of all Metrohm instruments.
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).
Column oven – Replacing the capillaries There are preheating grooves in the inner side wall of the column oven, where the column inlet capillary has already been inserted and fastened in place with a holder plate. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
For hanging the separation column (iCol- umn). With column recognition. Preheating grooves Holder plate For threading in the capillary to be tempera- For securing the capillary in place. ture-conditioned. Recesses Prevent the capillaries from being pinched. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
"p.a.". They may be diluted only by using ultrapure water (resistance > 18.2 MΩ*cm). (These specifications apply generally for all reagents used in ion chromatography.) Newly manufactured eluents always need to be microfiltered (0.45 µm fil- ter). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
To protect the high-pressure pump from foreign particles, we recom- ■ mend filtering the eluent through a filter with a pore size of 0.45 µm and aspirating it via an aspiration filter (6.2821.090). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Servicing the high-pressure pump 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/. Figure 14 High-pressure pump – Parts Pressure screw, short (6.2744.070) Outlet valve holder Fastened to the outlet valve holder.
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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 parts in the accessory kit: Vario/Flex Basic (6.5000.000). Adjustable wrench (6.2621.000) ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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RBS™ solution or acetone. The rinsing solution may only come out at the valve outlet. The outlet valve must be replaced if it is still clogged after cleaning. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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¼ turn using the adjustable wrench (3). Tighten the connection capillary to the auxiliary piston back onto ■ the outlet valve holder. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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RBS™ solution or acetone. The rinsing solution may only come out at the valve outlet. The inlet valve must be replaced if it is still clogged after cleaning. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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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 pump switched off? ■ Has the pressure been released? ■ Is the instrument switched off? ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Servicing the piston Carry out the following work on both pistons in turn. Servicing a piston consists of the following tasks: Replace the piston seal. Clean or replace the zirconium oxide piston. Reinstall the piston. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
(6.5000.000). Adjustable wrench (6.2621.000) ■ Tool for piston seals (6.2617.010) consisting of a tip (16-1) for remov- ■ ing the old piston seal and a sleeve (16-2) for inserting the new piston seal. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Loosen the piston cartridge (17-1) 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 (17-2) out of the piston opening. Set it aside. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Press the seal into the pump head recess using the wide end of the tip (16-1) of the tool. Cleaning or replacing the zirconium oxide piston Prerequisites: ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
Place the backup ring you put aside with the remaining parts. ■ Figure 19 Parts of the piston cartridge Piston cartridge screw Retaining washer Zirconium oxide piston (6.2824.070) Spring retainer Spring (6.2824.060) Inner plastic sleeve Protects from metallic abrasion. Piston cartridge Backup ring ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Clean the second piston cartridge in the same way. Mounting 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). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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The bore hole with the greatest depth must therefore be aligned with the longest bolt. Push the pump head onto the four fastening bolts (1). ■ Tighten the four fastening screws using the hex key (6.2621.030) ■ alternating crosswise. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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.
3 Unscrewing the filter screw Use two adjustable wrenches (6.2621.000) to loosen the filter screw (20-2) from the filter housing (20-1) and unscrew it by hand. 4 Removing the filter Remove the old filter (20-3) using tweezers. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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4 Rinsing the inline filter Dismantle the guard column (if present) and the separation col- ■ umn and replace with a coupling (6.2744.040). Rinse the instrument with eluent. ■ Reinsert the columns after 10 minutes. ■ ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
1 Emptying the sample path Pump air through the sample path (pump tubing, tubing connec- tions, capillary in the degasser, sample loop) for several minutes until all liquid is displaced by the air. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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A. The smaller 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. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
You can find detailed information on the separation columns available from Metrohm in the leaflet provided along with your separation column, in the Metrohm IC Column Program (available from your Metrohm representative) or on the Internet at http://www.metrohm.com...
Metrohm offers you comprehensive support in implementing quality man- agement measures for instruments 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.
Constantly stir the eluent. ■ The pressure in the The inline filter Replace the filter (6.2821.130) . system markedly (6.2821.120) is blocked. increases. Guard column – Blocked. Replace the guard column (see Chapter 3.16, page 29). ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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Replace the separation column (see "Con- ■ necting the separation column", page 33). Note: Samples should always be microfiltered . Injection valve – blocked. Have the valve cleaned (by a Metrohm service engineer). The retention times Eluent - Incorrect concen- Create eluent with correct concentration.
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Use the sample degasser . bubbles in the sample. Sample – The rinsing vol- Increase the rinsing time (see Chapter 5.12, ume is too small. page 60). Injection valve – Defective. Request Metrohm Service. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
+0 - +80 °C, in 0.1 °C increments perature range Heating Ambient temperature of +5 °C - ambient temperature of +40 °C Temperature ±0.2 °C reproducibility Stability < 0.05 °C Heating time < 30 minutes from 20 to 40 °C ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
The shutdown mechanism is inactive at 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 ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
The PDF file with the accessories data will be created. NOTE When you receive your new instrument, we recommend downloading the accessories list from the Internet, printing it out and keeping it together with the manual for reference purposes. ■■■■■■■■ 930 Compact IC Flex Oven (2.930.2100)
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