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5 Troubleshooting

2.850.9110 IC Amperometric Detector

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5.3

General remarks regarding sensitivity fluctuations

Sensitivity fluctuations of up to 20% per week are normal for an
unchanged system in constant operation.

The sensitivity can increase to approximately twice as much for a short
time when new working electrodes are inserted or when the conditions
change.

5.4

Problems with sensitivity

Problem

Cause

Remedy

Declining sensitivity.

Measuring cell – Auxiliary
electrode contaminated.

Clean the auxiliary electrode (see measuring
cell manual).

Incorrect eluent in the ref-
erence chamber.

Remove the purge stopper on the measuring
cell, wait until approx. 1 mL of eluent has
emerged, screw the purge stopper back in
tightly.

Sample concentration is no
longer correct.

Replace the sample and/or the standard solu-
tion.

Temperature fluctuations.

￭

Amperometric detector – Use preheating
capillary.

￭

IC instruments – Use column oven.

Replace the measuring cell.

￭

Use a measuring cell of the same type.

￭

Use the same spacer.

￭

Use the same electrodes.

Software – Measurement
potential incorrect.

Optimize the measurement potential.

Measuring cell – Working
electrode contaminated.

Clean the working electrode (see the leaflet for
the working electrode).

IC system – Eluent contam-
inated.

Prepare a new eluent.

IC system – pH of the elu-
ent has changed.

Check the pH value of the eluent and optimize
it if necessary.

Содержание 2.850.9110

Страница 1: ...IC Professional Detector IC Amperometric Detector Manual 8 850 8062EN 2020 09 25 ...

Страница 2: ......

Страница 3: ...trohm AG CH 9100 Herisau Switzerland Phone 41 71 353 85 85 Fax 41 71 353 89 01 info metrohm com www metrohm com IC Professional Detector IC Amperometric Detector 2 850 9110 Manual 8 850 8062EN 2020 09 25 ...

Страница 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 ...

Страница 5: ... 6 2 2 Rear 7 3 Installation 8 3 1 Setting up the instrument 8 3 1 1 Packaging 8 3 1 2 Check 8 3 1 3 Location 8 3 2 Inserting the amperometric detector 8 3 3 Putting the amperometric detector into operation 11 3 3 1 Instrument test with dummy cell 11 3 3 2 Testing the leak sensor 13 3 3 3 Testing the preheating capillary 14 3 3 4 Testing the detector outlet capillary 15 3 3 5 Testing the measuring...

Страница 6: ...2 Problems with the baseline 24 5 3 General remarks regarding sensitivity fluctuations 27 5 4 Problems with sensitivity 27 5 5 Problems with the pressure 28 5 6 Problems with the measuring signal 28 5 7 Problems with the chromatogram 29 5 8 Other problems 30 5 9 Systematic error diagnostics 31 6 Technical specifications 33 6 1 Amperometric detector 33 7 Accessories 35 Index 36 ...

Страница 7: ... Table of figures 2 850 9110 IC Amperometric Detector V Table of figures Figure 1 Front 6 Figure 2 Rear 7 Figure 3 Inserting the detector 9 ...

Страница 8: ......

Страница 9: ... installed preheating capillary ensures a constant eluent temperature on the cell On the one hand the built in leak sensor detects fluid that has escaped in the interior of the detector while on the other it also responds when too much fluid has backed up in the tray on the front side of the detector As a result of this the leaking instrument is shut down and the ongoing determinations are cancele...

Страница 10: ...spect to the application of the fire prevention measures prescribed for laboratories is also mandatory 1 3 Safety instructions 1 3 1 General notes on safety WARNING Operate this instrument only according to the information contained in this documentation This instrument left the factory in a flawless state in terms of technical safety To maintain this state and ensure non hazardous operation of th...

Страница 11: ...olvents and chemicals WARNING All relevant safety measures are to be observed when working with flammable solvents and chemicals Set up the instrument in a well ventilated location e g fume cup board Keep all sources of flame far from the workplace Clean up spilled liquids and solids immediately Follow the safety instructions of the chemical manufacturer 1 3 5 Recycling and disposal This product i...

Страница 12: ...maintenance work that can be carried out by the user The technical specifications of the IC Amperometric Detector Possible problems and their solutions The supplied and the optional accessories Further information Detailed information regarding the preparation of the measuring cell and its maintenance can be found in the manuals for the Wall Jet cell IC equip ment Information on the utilization ca...

Страница 13: ...ttention to a possible hazard due to 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 a possible damage of instruments or instrument parts Note This symbol marks additional information and tips ...

Страница 14: ...inside the instrument labeled with Eluent to cell 6 Drain nozzle At the bottom of the tray sealed with a stopper 7 Leak sensor 8 Connection socket For the working electrode labeled with WE working electrode 9 Eluent input Input of the preheating capillary inside the instrument labeled with Eluent in 10 Connection socket For the reference electrode labeled with RE reference electrode 11 Detector ho...

Страница 15: ...rode labeled with AE auxiliary electrode 16 Capillary feed through For leading capillaries into the cell chamber and out of the cell chamber 2 2 Rear 1 2 3 4 Figure 2 Rear 1 Front cover Removable 2 Type plate With serial number 3 Connector plug For connecting the detector to the detector connection socket of the IC instrument 4 Connection socket For a testing instrument for service only ...

Страница 16: ... ber of the IC instruments For the location the same conditions apply as for the IC instrument 3 2 Inserting the amperometric detector The IC Amperometric Detector can be used with the following IC instru ments insofar as they have an unoccupied detector connection All 850 Professional ICs All 881 Compact IC pros All 882 Compact IC pluses The IC Amperometric Detector is placed in the detector cham...

Страница 17: ...allation 2 850 9110 IC Amperometric Detector 9 2 3 4 5 1 Figure 3 Inserting the detector NOTICE With the instruments of the 850 Professional line of instruments up to two detectors can be placed and connected ...

Страница 18: ...t surface intended for this purpose and slide it as far as the limit stop to the front 4 Replace the rear panel Insert the detector cable in a cable feed through on the rear panel Replace the rear panel The detector cable must hang freely from the cable feed through 5 Tighten the knurled screws Optional with 850 instruments Reattach the handle higher up and use it as a holder for MPaks Tighten the...

Страница 19: ... the preheating capillary see chapter 3 3 3 page 14 Testing the detector output capillary see chapter 3 3 4 page 15 Testing the measuring cell see chapter 3 3 5 page 16 Deaerating the measuring cell see chapter 3 3 6 page 18 3 3 1 Instrument test with dummy cell When you are putting the IC Amperometric Detector into operation for the first time or when problems occur which may be caused by signal ...

Страница 20: ...nto the WE socket of the detector Plug the straight plug of the reference electrode connection cable black sleeve into the RE socket of the detector Plug the straight plug of the auxiliary electrode connection cable blue sleeve into the AE socket of the detector 3 Inserting the dummy cell Place the dummy cell into the tray of the detector Attach the front cover NOTICE The metal parts of the cable ...

Страница 21: ...ector data is not correctly transmitted 6 Removing the dummy cell Pull out the electrode connection cables from the connectors AE WE and RE of the dummy cell Remove the dummy cell from the tray The dummy cell incorporates a resistor 300 MΩ and a capacitor 100 nF connected in parallel If in DC mode a potential of 0 8 V is applied then a current of 2 667 nA 7 is measured in the dummy cell The capaci...

Страница 22: ...both leaks and block ages proceed as follows Testing the preheating capillary 1 Connecting the detector inlet capillary Use a pressure screw 6 2744 014 to fasten the detector inlet capil lary to the Eluent in connector on the detector 2 Adjusting the settings in MagIC Net In the program part Manual of MagIC Net set the maximum pressure of the high pressure pump to 5 MPa Set the flow rate to 0 1 mL...

Страница 23: ...r inlet capillary is connected to the Eluent in connector The high pressure pump runs with a flow rate of 0 1 mL min 1 Connecting the detector outlet capillary Use a pressure screw 6 2744 014 to fasten the detector outlet capil lary to the Eluent to cell connector 2 Adjusting the settings in MagIC Net In the program part Manual of MagIC Net increase the flow rate to 1 0 mL min and wait until the p...

Страница 24: ...e measuring cell is completely assembled see measuring cell man ual The working electrode and the reference electrode are inserted see measuring cell manual 1 Connecting the measuring cell Connecting the measuring cell inlet When the preheating capillary is used Use a pressure screw 6 2744 014 to fasten a piece of the PEEK capillary 6 1831 010 to the Eluent to cell connector on the detector Use a ...

Страница 25: ... otherwise the data may be transferred incorrectly or incompletely 3 Testing at low flow In the program part Manual of MagIC Net set the flow rate of the high pressure pump to 0 2 mL min and start the high pressure pump Watch the detector outlet capillary Liquid must emerge from the end of the detector outlet capillary If no liquid emerges from the end of the detector outlet capillary Detach the c...

Страница 26: ...ld emerge from the body of the measuring cell 3 3 6 Deaerating the measuring cell The cell must be deaerated in order to ensure that it contains no air bub bles The measuring cell must be deaerated after the installation and after each subsequent opening of the cell Proceed as follows Deaerating the measuring cell Prerequisites The high pressure pump is switched on and pumps the eluent through the...

Страница 27: ...y hand 4 Switch off the high pressure pump in MagIC Net 3 4 Connecting the electrode cables CAUTION The electrode cables may not be plugged or unplugged unless the mea suring cell is switched off in the software NOTICE The sockets and the plugs of the cables must be clean and dry Connecting the electrode cables to the detector Prerequisites The measuring cell is switched off 1 Plug the straight pl...

Страница 28: ...the measuring cell 1 Plug the angled plug of the working electrode cable labeled WE into the working electrode socket 2 Plug the angled plug of the reference electrode cable labeled RE into the reference electrode socket 3 Plug the angled plug of the auxiliary electrode cable labeled AE into the socket labeled AE 3 5 Attaching the front cover In order to obtain good measuring results we recommend ...

Страница 29: ...ation of the instrument may result in functional disruptions and a reduction in the life time of the sturdy mechanics and electronics CAUTION Even though design measures ensure that this will largely be prevented the detector should be switched off without delay in the event that aggressive media have found their way into the interior of the detector It is only thus that massive damage to the inst...

Страница 30: ... must not exceed 5 MPa In order to ensure this set the maximum pressure of the high pressure pump to 5 MPa in MagIC Net 4 4 2 Preheating capillary maintenance The preheating capillary can become blocked e g if the IC system has inadvertently been run dry To dissolve this blockage proceed as follows Rinsing the preheating capillary 1 Removing the separation column Remove the separation column from ...

Страница 31: ...placed by a Metrohm Service employee 4 5 Shutting down If the instrument is not used for a longer period the whole IC system without separation column must be rinsed salt free with methanol ultra pure water 1 4 in order to prevent eluent salts from forming crystals which may cause subsequent damage Rinsing salt free the IC system To rinse the system proceed as follows 1 Remove the guard column and...

Страница 32: ...gh pressure pump Con taminated valves Clean valves see Chapter Operation and maintenance in the manual for the IC instru ment High pressure pump Defective piston seal Replace the piston seals see Chapter Opera tion and maintenance in the manual for the IC instrument High pressure pump Quality of the pump is not sufficient for the selected sensitivity Use a pulsation absorber Use a higher performan...

Страница 33: ...asuring cell see Deaerat ing the measuring cell page 18 Short circuit bridge between the electrodes Examine the working electrode for promi nent deposits Polish the working electrode see the leaflet for the working electrode Replace the working electrode Clean the measuring cell Check the spacer The reference electrode is worn out Replace the reference electrode The cause is not clear Perform a sy...

Страница 34: ... Unexpectedly high or low baseline Pd reference electrode Working conditions not yet achieved Equilibrate until the electrode has adjusted to the new elution conditions over night DC method Working con ditions not yet achieved An excessively high baseline is normal at the start of the equilibration Equilibrate until the baseline corresponds to the one in the Appli cation Works Detector parameters ...

Страница 35: ...er Remove the purge stopper on the measuring cell wait until approx 1 mL of eluent has emerged screw the purge stopper back in tightly Sample concentration is no longer correct Replace the sample and or the standard solu tion Temperature fluctuations Amperometric detector Use preheating capillary IC instruments Use column oven Replace the measuring cell Use a measuring cell of the same type Use th...

Страница 36: ...uld always be micro filtered see Chapter Operation and maintenance Inline sample preparation in the manual for the IC instrument Amperometric detector Preheating capillary blocked Perform a maintenance procedure for the pre heating capillary see chapter 4 4 2 page 22 Amperometric detector Detector outlet capillary not free of blockage Test the detector outlet capillary see chapter 3 3 4 page 15 5 ...

Страница 37: ...n column see Chap ter Operation and maintenance in the manual for the IC instrument IC system Eluent is old Prepare a new eluent The ionic strength of the sample or the pH value of the sample deviates greatly from the eluent Dilute the sample or optimize the pH value of the sample Absorption of analyte at the electrodes Use a suitable combination of electrodes and eluent The retention times in the...

Страница 38: ... a new eluent Software Measurement potential pulse settings incorrect Optimize the parameters Very wide peaks through substances with delayed elution Wait for the complete elution of these sub stances Unstable tempera ture The set temperature is too low Set the temperature to at least 8 C higher than the highest ambient temperature to be anticipated Current display charge display in the software i...

Страница 39: ...od parameters of the detector and reset them to values that you know will function Check the measuring range and reset it to values that you know will function or select a larger measuring range Check manual changes to the settings and reset them to values that you know will function Check manual settings in the time program and reset them to val ues that you know will function If the problem has ...

Страница 40: ... of the measuring cell Replace the body of the measuring cell with another one of the same type If the problem has not yet been localized continue with Step 8 8 Requesting Metrohm Service If none of these measures help please request Metrohm Service NOTICE Please note that when the electrodes are replaced the system requires a longer run in time before the earlier values can be reproduced ...

Страница 41: ...IPAD flexible IPAD CV Measuring unit AutoRange yes DC only Digital signal range DC mode 0 00012 pA 2 mA PAD mode 0 012 pA 2 mA flexIPAD mode 0 12 pC 200 µC CV 0 12 pA 20 mA Electronic noise DC mode 2 pA PAD mode 10 pA flexIPAD mode 30 pC Filter DC mode Hardware filter can be selected by the user All modes Software filter can be set by the user Temperature con trol Temperature stability at the heat...

Страница 42: ...og Out Output voltage 0 1000 mV Full scale Can be adjusted within the digital signal range Offset Can be adjusted within the digital signal range System standby Automatic function test at start up Leak sensor Temperature stability monitoring Output channels Current rating Charge GLP conformity Yes optional ...

Страница 43: ...hm com into your Internet browser 2 Enter the article number e g 2 850 9110 into the search field The search result is displayed 3 Click on the product 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 is created NOTICE Once you have received your new product we recommend download ing the...

Страница 44: ...A Amperometric detector Placement 8 Technical specifications 33 C Care 21 E Electrode cable Connect 19 Electrostatic charge 3 R Rinsing Detector 22 S Safety instructions 2 Service 2 22 Shutting down 23 T Technical specifications Amperometric detector 33 ...

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