806 Exchange Unit. Manual EN

Transcription

1 806 Exchange Unit Manual EN

2

3 Metrohm AG CH-9101 Herisau Switzerland Phone Fax Exchange Unit Manual EN ek/dm

4 Teachware Metrohm AG CH-9101 Herisau This documentation is protected by copyright. All rights reserved. Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above. Documentation in additional languages can be found on under Literature/Technical documentation.

5 Table of contents Table of contents 1 Introduction About the documentation Symbols and conventions Safety instructions Tubing and capillary connections Flammable solvents and chemicals Filling the dosing cylinder Recycling and disposal Construction of the 806 Exchange Unit Total view Components of the 806 Exchange Unit Installation Setting up the instrument Packaging Checks Location Start-up Preparing the exchange unit Attaching the exchange unit Filling the tubings Buret tips Removing the exchange unit Mounting the components Mounting the thermostat casing Mounting the flat stopcock Mounting the tubings on the flat stopcock Mode of operation Filling the dosing cylinder and dosing Handling and maintenance Care and upkeep Disassembling the exchange unit Cleaning the cylinder and piston Assembling the exchange unit Flat stopcock blocked Chemical resistance and materials Solutions Body Exchange Unit III

6 Table of contents Materials GLP - Validation Troubleshooting Problems Appendix Buret data Dosing accuracy Typical measurement deviation The ISO/EN/DIN standard Accessories Scope of delivery Exchange Unit xxx Optional accessories Index 36 IV 806 Exchange Unit

7 Table of figures Table of figures Figure Exchange Unit... 4 Figure Exchange Unit - Components... 6 Figure 3 Thermostat casing Figure 4 Flat stopcock Figure 5 Dosing/Filling Exchange Unit V

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9 1 Introduction 1 Introduction The 806 Exchange Unit is a versatile buret unit which can be operated with various Metrohm dosing devices or titrators. The 806 Exchange Unit is suitable for simple dosings or titrations. Specifications concerning the exchange unit and the reagent can be stored in the integrated data chip. This data can be read out and updated by a suitable instrument. 1.1 About the documentation Symbols and conventions The following symbols and styles are used in this documentation: Cross-reference to figure legend The first number refers to the figure number, the second to the instrument part in the figure. Instruction step Carry out these steps in the sequence shown. Method File New [Next] Dialog text, parameter in the software Menu or menu item Button or key Warning This symbol draws attention to a possible life hazard or risk of injury. Warning This symbol draws attention 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. 806 Exchange Unit 1

10 1.2 Safety instructions Caution This symbol draws attention to a possible damage of instruments or instrument parts. Note This symbol marks additional information and tips. 1.2 Safety instructions Tubing and capillary connections CAUTION Leaks in tubing and capillary connections are a safety risk. Tighten all connections well by hand. Avoid applying excessive force to tubing connections. Damaged tubing ends lead to leakage. Appropriate tools can be used to loosen connections. Check the connections regularly for leakage. If the instrument is used mainly in unattended operation, then weekly inspections are mandatory Flammable solvents 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. Keep all sources of flame far from the workplace. Clean up spilled liquids and solids immediately. Follow the safety instructions of the chemical manufacturer Exchange Unit

11 1 Introduction Filling the dosing cylinder CAUTION If a buret tip is clogged, then it could happen that no liquid will be aspirated when the dosing cylinder is being filled. A vacuum can arise as a result. If you then remove the exchange unit from the instrument, the piston could destroy the dosing cylinder. Do not fail to loosen the tubing connections on the dosing cylinder first, before you remove the exchange unit. This will eliminate the vacuum. 1.3 Recycling and disposal This product is covered by European Directive 2002/96/EC, WEEE Waste from Electrical and Electronic Equipment. The correct disposal of your old equipment will help to prevent negative effects on the environment and public health. More details about the disposal of your old equipment can be obtained from your local authorities, from waste disposal companies or from your local dealer. 806 Exchange Unit 3

12 2.1 Total view 2 Construction of the 806 Exchange Unit 2.1 Total view Figure Exchange Unit 1 Tubing connection ( ) 2 Threaded stopper ( ) 4 Length 25 cm 806 Exchange Unit

13 2 Construction of the 806 Exchange Unit 3 Bottle attachment ( ) Of PFA/PP, thread GL45 5 PCTFE/PTFE flat stopcock ( ) Or ceramic stopcock Plate holder ( ) For name plates 9 Data chip On the underside of the buret 11 SGJ clip ( ) Of POM 13 Bottle with thread ( ) Amber glass, thread GL45 4 Tubing connection ( ) Length 13 cm ( with 1 ml cyl.) 6 Storage vessel ( ) For buret tips or electrodes 8 Nominal volume 10 Adsorber tube ( ) Adsorber tube Tubing connection ( ) Length 40 cm 14 Antidiffusion tip ( ) Of ETFE/FEP, for titrations 15 Link stopper ( ) 16 Storage vessel ( ) For buret tips or electrodes 17 Body ( XXX).110 for 1 ml cylinder.150 for 5 ml cylinder.210 for 10 ml cylinder.220 for 20 ml cylinder.250 for 50 ml cylinder 806 Exchange Unit 5

14 2.2 Components of the 806 Exchange Unit 2.2 Components of the 806 Exchange Unit Figure Exchange Unit - Components 1 Tubing connection ( ) Length 25 cm 3 Tubing connection ( ) Length 13 cm ( with 1 ml cyl.) 5 Torque key ( ) For loosening tubing nipples 7 Insert for key ( ) For loosening the light protection 2 Tubing connection ( ) Length 40 cm 4 Threaded stopper ( ) 6 Paraffin fat ( ) For dosing pistons, 2 g 8 Light protection ( ) Of PETG Exchange Unit

15 2 Construction of the 806 Exchange Unit 9 Mounting ring for the cylinder ( XXX).000 for 5, 10 ml cylinder.010 for 20 ml cylinder.020 for 50 ml cylinder 11 Dosing cylinder ( XXX) Clear glass ml cylinder ml cylinder ml cylinder ml cylinder ml cylinder 13 Plate holder ( ) For name plates 15 Storage vessel ( ) For buret tips or electrodes 17 Adsorber tube ( ) Adsorber tube SGJ clip ( ) Of POM 21 Canula ( ) Of FEP, thread M6 23 Holding clamps ( ) For reagent bottles 25 PTFE piston ( XXX) with coupling.110 for 1 ml cylinder.150 for 5 ml cylinder.210 for 10 ml cylinder.220 for 20 ml cylinder.250 for 50 ml cylinder 10 Name plates ( ) For labeling the reagent, 10 x 12 Flat stopcock PCTFE/PTFE Ceramic Switching lever For switching the flat stopcock 16 Nominal volume 18 Adapter NS14 for adsorber tube Of ETFE 20 Bottle attachment ( ) Of PFA/PP, thread GL45 22 Bottle with thread ( ) Amber glass, thread GL45 24 Storage vessel ( ) For buret tips or electrodes 26 Antidiffusion tip ( ) Of ETFE/FEP, for titrations 806 Exchange Unit 7

16 2.2 Components of the 806 Exchange Unit 27 Dosing tip open ( ) of ETFE/FEP, for dosings 29 Body ( XXX).110 for 1 ml cylinder.150 for 5 ml cylinder.210 for 10 ml cylinder.220 for 20 ml cylinder.250 for 50 ml cylinder 28 Link stopper ( ) 30 Data chip On the underside of the buret Exchange Unit

17 3 Installation 3 Installation 3.1 Setting up the instrument Packaging The instrument is supplied in highly protective special packaging together with the separately packed accessories. Keep this packaging, as only this ensures safe transportation of the instrument Checks Immediately after receipt, check whether the shipment has arrived complete and without damage by comparing it with the delivery note Location The instrument has been developed for operation indoors and may not be used in explosive environments. Place the instrument in a location of the laboratory which is suitable for operation, free of vibrations, protected from corrosive atmosphere, and contamination by chemicals. The instrument should be protected against excessive temperature fluctuations and direct sunlight. 3.2 Start-up Preparing the exchange unit Proceed as follows: 1 Mount the holding clamps in such a way that the reagent bottle rests safely on the exchange unit. 2 Check whether the reagent bottle contains solvent. 3 Fill the adsorber tube with a suitable adsorber material. CO 2 adsorption: Soda lime KF reagent: Molecular sieve If no special adsorber material is necessary, the adsorber tube may also be used as dust filter when filled with cotton. 4 Attach the filled adsorber tube onto the reagent bottle. 806 Exchange Unit 9

18 3.2 Start-up 5 Control, whether the tubing connections are fastened. Tighten the tubing connection with the key if necessary. NOTE Do not use any other aids! The threads of the tubing nipples and the tubing openings may not be deformed. 6 Write the name of the solvent in the reagent bottle on a colored plate. 7 Slide the plate into the labeling holder. 8 Store the buret tip or the electrode in the two storage vessels. Usage of original reagent bottles You may eventually need a special bottle attachment or a thread adapter in addition to the supplied standard bottle attachment: Bottle attachment Order number Bottles with GL45 thread Standard Bottles with S40 thread Bottles with GL32 thread / Bottles with 28 mm thread / Attaching the exchange unit Attach an 806 Exchange Unit as follows: 1 Before attaching the exchange unit, check whether the stopcock can be switched manually by the switching lever. For attaching, the switching lever must be directed to the right (stopcock in dosing position). The arrow marking must point upwards Exchange Unit

19 3 Installation 2 Check the position of the piston rod on the underside of the exchange unit. The recess of the piston rod must be tight with the buret base and the smooth surface with the opening must be directed to the rear. 3 Correct the position of the piston rod with the key if necessary. NOTE In case of carelessly handling the key, the data chip of the exchange unit may be damaged. Avoid touching the white ceramic holder of the data chip! 4 Attach the exchange unit from the front onto the control device and push all the way to the rear, so that it snaps in and the LED Status flashes slowly. It must snap in audibly. 806 Exchange Unit 11

20 3.2 Start-up Filling the tubings 5 If the exchange unit does not snap in, check the following: Position of the piston rod Stopcock position of the exchange unit The switching lever must be directed to the right (stopcock in dosing position). The arrow marking must point upwards (see step 1). If the exchange unit is attached correctly, its initialization is being activated by a micro switch which is triggered by the guide bolts of the exchange unit. It is being recognized and the data is being read automatically from the data chip. The control device automatically rotates the stopcock and returns the stopcock in dosing position. After this, the LED Status on the control device lights up constantly. The proceeding during the filling of the tubings of the exchange unit depends on the control device and control software. Consult the corresponding manual for manual dosing and filling. The function Preparing or PREP of the control software is used to rinse the cylinder and tubings of the exchange unit and fill them air bubble-free. You should carry out this function before the first determination or once per day Exchange Unit

21 3 Installation Buret tips The following buret tips are included in the standard equipment of the dosing unit: Open dosing tip For tasks during which the top is not immersed, e.g. dosings. The buret tip can be stored in the same solvent as the one contained in the reagent in order to prevent reagent crystallization. We recommend that the storage vessel be filled with solvent and that the buret tip be placed inside it. In the event that KF reagent is used as the titrant, use methanol or ethanol for storing the dosing tip. Antidiffusion tip It is used for work requiring the immersion of the tip, e.g. titrations. This tip prevents the diffusion of liquids into the buret tip. The pressure of the surrounding liquid and the internal stress of the membrane press on the tubing end, thus sealing off the opening. The backpressure of the dosed liquid is overcome during the dosing process. The membrane opens up the tubing end. The tubing end is sealed off again automatically after the dosing is completed. CAUTION Do not disassemble the antidiffusion tip. 806 Exchange Unit 13

22 3.3 Mounting the components Removing the exchange unit To remove the exchange unit, proceed as follows: 1 Carry out the 'Filling' function on the control device. NOTE Do not try to remove the exchange unit when the piston of the exchange unit or the piston rod of the drive is in zero position. 2 Carefully remove the exchange unit to the front. If it is not possible to remove the exchange unit, check the status of the control device. 3 If the control device is still busy, press the key <STOP> and wait until the device is ready. 4 If the control device is overloaded and a corresponding error message is displayed, switch it off and on again. 5 If the device is displaying that it is busy with filling the cylinder but apparently nothing happens, the filling rate is maybe set too low. Try to increase the filling rate and wait until the device is ready. 3.3 Mounting the components Mounting the thermostat casing If a solvent with a constant temperature is necessary for a titration, the thermostat casing is used. Water with a certain temperature is pumped through the thermostat casing and this way the temperature of the content in the dosing cylinder is kept constant. The thermostat casing may only be used with a thermostat equipped with a pressure and suction pump (the feeding pressure must not be too high). The thermostat casing may only be used in a temperature range from C Exchange Unit

23 3 Installation Figure 3 Thermostat casing Mount the thermostat casing as follows: 1 Loosen the tubing connection to the glass cylinder. 2 Unscrew the light protection. 3 Screw out the glass cylinder with holder. 4 Loosen the screw nipple on the glass cylinder. 5 Roll the O-ring out of the groove and upwards on the glass nozzle. Do not use any hard items to remove the O-ring, otherwise the edge of the glass nozzle may chip off! 6 Replace the union nut of the cylinder by the sealing ring of the thermostat casing (threaded side upwards). 7 Slightly grease the O-ring and attach it on the glass nozzle. 8 Fasten the sealing ring with the screw nipple. 9 Insert the glass cylinder with holder into the thermostat casing and press firmly. 10 Tighten the thermostat casing with the cylinder in the body. 11 Connect the thermostat tubings. 806 Exchange Unit 15

24 3.3 Mounting the components Mounting the flat stopcock Figure 4 Flat stopcock Mount the flat stopcock as follows: 1 Check whether the flat stopcock can be moved. Twist the lower and upper part of the flat stopcock against each other. For mounting the stopcock, move the lower part to the right as far as the limit stop, i.e. in clockwise direction. 2 Check whether the switching lever on the exchange unit is directed to the right. 3 Insert the stopcock into the holder (see Figure 2, page 6). The rectangular recess of the stopcock is to be directed to the groove on the edge (on the left side) of the holder. 4 Check whether the stopcock can be moved by the switching lever. 5 Rotate the switching lever to the right to the dosing position. 6 Attach the exchange unit onto the control device. Types of flat stopcocks There is a PCTFE/PTFE stopcock ( , standard equipment) and a ceramic stopcock available, which can be ordered separately. Generally, the ceramic stopcock is to be preferred if hard crystals can precipitate out of the solution. If only soft crystals precipitate or for reagents only occasionally used, we recommend the PCTFE/PTFE stopcock. The PCTFE/PTFE stopcock is subject to a certain wearing. This stopcock has to be replaced more often than the ceramic stopcock. We especially recommend the following type of flat stopcocks: Exchange Unit

25 3 Installation Solution PCTFE/PTFE Ceramic Alkaline, aqueous EDTA, complexone HClO4 in glacial acetic acid Iodine solution Karl Fischer reagent KOH in ethanol Organic solvents Permanganate, KMnO4 Acids, aqueous Silver nitrate, AgNO3 TBAOH Thiosulphate, Na2S2O Mounting the tubings on the flat stopcock Mounting the tubings on the flat stopcock Fasten the tubing on the flat stopcock and on the bottle attachment of the reagent bottle. 806 Exchange Unit 17

26 3.3 Mounting the components 2 Fasten the tubing on the flat stopcock and on the dosing cylinder. 3 Fasten the tubing on the flat stopcock. 4 Fasten the buret tip on the tubing. 5 Tighten the tubing connection by hand or with the key if necessary. NOTE Do not use any other aids! The thread of the tubing nipple and the tubing openings may not be deformed. 6 Carry out 'Filling'. 7 Fill the tubings by several dosings and fillings of the cylinder or with the PREP/Prepare function. By the several dosings and fillings, the air bubbles are driven out. It is important that the tubing connection between the buret and the flat stopcock is bubble-free. If necessary, knocking against the tubings helps to remove the bubbles remained Exchange Unit

27 4 Mode of operation 4 Mode of operation 4.1 Filling the dosing cylinder and dosing Figure 5 Dosing/Filling 1 Filling tube For aspirating the solvent out of the reagent bottle. 3 Dosing piston For ejecting and aspirating a solution. 5 Dosing tubing For dosing the solvent via the dosing tip. 2 Dosing cylinder Contains the solution for dosing. Volume 1 ml, 5 ml, 10 ml, 20 ml or 50 ml. 4 Piston rod With coupling. For moving the dosing piston in the dosing unit. 6 Flat stopcock For switching between filling and emptying the dosing cylinder. 7 Switching lever For manually switching the flat stopcock. 806 Exchange Unit 19

28 4.1 Filling the dosing cylinder and dosing When ejecting the titrant, the piston rod of the drive moves upwards the dosing piston in the dosing cylinder. The flat stopcock is in dosing position. The switching lever is directed to the right. The liquid in the cylinder is pushed trough the flat stopcock into the dosing tubing. After switching the flat stopcock, i.e. rotating the flat stopcock (switching lever is directed to the left), liquid is aspirated out of the filling tubing as a result of the dosing piston being pulled downwards by the piston rod of the drive. Because of the fact that the exchange units are interchangeable, the coupling of the piston rod exhibits a low mechanical tolerance which has an effect on the accuracy of the dosing when the dosing piston changes its direction of movement. This tolerance is mechanically compensated by the drive during automated procedures. The piston movements are controlled by the precise electronic fine mechanics of the drive. Independent of the cylinder volume, it exhibits a resolution of 20'000 increments across the entire piston stroke. The rate, at which a solution is to be dosed and the rate, at which the cylinder is to be filled, depend on the cylinder volume of the exchange unit. The maximum and minimum filling and dosing rates are: Cylinder volume (ml) max. filling- dosing rate (ml/min) min. filling- dosing rate (µl/ min) (depending on device) NOTE Enter lower rates for high-viscosity liquids Exchange Unit

29 5 Handling and maintenance 5 Handling and maintenance 5.1 Care and upkeep The exchange unit needs appropriate care. NOTE Exchange units must be monitored regularly and cleaned from time to time. Monthly inspections are called for in the event that alkaline, corrosive or high-concentration reagents are used. If non-problematic reagents are used, then the inspection intervals can be extended to several months Disassembling the exchange unit It is recommended to disassemble and clean the exchange unit when replacing the reagent. At the same time, the dosing piston and cylinder of the exchange unit can be checked. When using alkaline, corrosive or high-concentration reagents, it should be checked whether the glass cylinder has been attacked by e.g. aggressive alkalis or whether solids have crystallized out of the solution. WARNING Do not disassemble the exchange unit if it is still on the drive! Remove the exchange unit from the control device before loosening the tubing connections. Escaping reagents may access the inside of the device. Proceed as follows: 1 Eject the reagent as far as possible without have the cylinder newly filled. 2 Loosen the tubing connection on the reagent bottle. 3 Move the piston to zero position, i.e. carry out 'Filling'. 4 Remove the exchange unit from the drive. 806 Exchange Unit 21

30 5.1 Care and upkeep 5 Remove all tubings. 6 Unscrew and remove the cylinder unit with light protection or the thermostat casing. If necessary for loosening the light protection, use the key (standard equipment of the dosing device or titrator) with the insert ( ). 7 Remove the cylinder holder with cylinder out of the light protection. Press above on the screw connector. 8 Remove the holder of the glass cylinder upwards. 9 Thoroughly empty the cylinder with the key and carefully remove the piston Cleaning the cylinder and piston Proceed as follows: 1 Check the leak-tightness of the dosing piston and cylinder. If there is liquid under the piston, the dosing cylinder is not or not thoroughly greased. Inspect the dosing piston for deformations or damage to the sealing lips. The piston and the cylinder must be replaced in the event that any changes are discovered. 2 Clean the dosing cylinder and piston with a liquid cleaning agent. Do not use any abrasive cleaning powder which could scratch the cylinder. 3 Afterwards, rinse the individual parts with plenty of deionised (or distilled) water. 4 Degreasing the piston and the glass cylinder is part of the cleaning procedure. Use a suitable cleaning agent or solvent and eventually an ultrasonic bath. Note the recommendations of the cleaning agent manufacturer. 5 Slightly grease the piston with paraffin grease ( ) on the sides. Wipe off the edge of the piston to avoid that the reagent will be in contact with the grease. Wipe off excess grease with a soft, lint-free cloth. Do not grease the piston for pipettings Exchange Unit

31 5 Handling and maintenance 6 Check the piston and cylinder for any changes once more before assembling the exchange unit. If the dosing cylinder should exhibit scratches or rough areas, then it must be replaced Assembling the exchange unit Mounting the cylinder Proceed as follows: 1 Insert the greased piston (see above) carefully into the cylinder for approx. 1 cm. 2 Slide the cylinder holder from above over the cylinder (O-ring must be on the upper side) and press firmly. 3 Insert the cylinder with holder into the light protection and press firmly. 4 Attach the exchange unit onto the control device. 5 Dose manually until the piston rod of the drive protrudes just out of the body of the exchange unit. 6 Insert the cylinder with light protection from above into the cylinder holder. 806 Exchange Unit 23

32 5.1 Care and upkeep 7 Couple the piston rod with the push rod of the drive. The clamp of the push rod must tightly fit into the opening of the piston rod, see picture. 8 Carefully push the light protection downwards and tighten in the thread of the body. Thereby the dosing piston is pressed into the cylinder. 9 Dose manually and move the piston upwards to the limit stop Flat stopcock blocked 1 Check whether the stopcock is in dosing position. The switching lever must be directed to the right. 2 Loosen the flat stopcock out of the holder. Rotate the plate holder to the left and slightly lift the clip on the side of the holder with a finger nail or a sharp object. Then the flat stopcock can easily be removed from the holder. 3 Put the stopcock into a solvent. with aqueous solutions hot water with non-aqueous solutions suitable solvent (see chapter 8) with KF reagent - methanol, then water, then methanol. 4 Eventually clean the stopcock with a suitable solvent (see above) in an ultrasonic bath and let it dry afterwards. 5 When the stopcock can be moved again, it can be inserted back into the exchange unit, see above Exchange Unit

33 5 Handling and maintenance 5.2 Chemical resistance and materials Solutions Metrohm exchange units are designed for usage with aqueous solutions and the most common solvents. The temperature of the dosing material may not exceed 50 C. The exchange unit and its components cannot be autoclaved. The sterility of a germ-free dosing material cannot be guaranteed. With the 806 Exchange Unit various solutions can be dosed. The materials of the individual components used have been selected for maximum resistance to chemicals and functionality. It can however not be assumed that all types of aggressive or high-concentration solutions can be conveyed without difficulty. It is the responsibility of the user to determine the resistance of the various individual components to specific, aggressive media. Many problems involving aggressive media can be prevented by regular cleaning and inspections Body The body is made of polybutylene terephthalate. It is only partly resistant to chemicals. Good resistance Acids, organic solvents Materials Limited resistance Alkalis (with a conc. > 1 M) The exchange unit is not dishwater-safe. In most cases, the exchange unit is to be cleaned with lukewarm water and dishwashing detergent. Body Dosing piston PBT (polybutylene terephthalate) PTFE (polytetrafluoroethylene) Dosing cylinder Borosilicate 3.3 Flat stopcock Light protection PCTFE/PTFE or ceramic PETG (polyethylene terephthalate, glycol-modified) or PVDF 806 Exchange Unit 25

34 5.3 GLP - Validation 5.3 GLP - Validation Every drive and every dosing unit manufactured by the Metrohm Co. is subjected to rigorous quality controls prior to shipment. Every dosing unit is issued a quality certificate attesting conformance with the strict quality criteria of Metrohm. GLP (Good Laboratory Practice) requires, among other things, periodic inspection of analytical measuring devices with respect to precision and correctness on the basis of standard operating procedures Standard Operating Procedure, SOP). This may also include an inspection of dosing accuracy. Recommended literature Metrohm brochure "Quality management with Metrohm", detailed information concerning the principles and procedural methods of Good Laboratory Practice Metrohm Applications Bulletin 283/1 Validation of Metrohm burets The validation of burets is carried out by the Metrohm service with special software. The Metrohm agents worldwide offer the possibility of on-site inspections and certifications of dosing units and Dosinos with respect toaccuracy. It is recommended that an accuracy inspection be performed when the dosing cylinders and dosing pistons of a dosing unit are replaced Exchange Unit

35 6 Troubleshooting 6 Troubleshooting 6.1 Problems Problem Cause Remedy Air bubbles in the cylinder or in the dosing tubing Leaking connection Check the ends of the tubing, in particular that of the aspiration tubing. Tighten all of the tubing connections with the wrench Check the locking mechanism of the housing. Suggestion: Remove the housing and then reattach it. The reagent degasses excessively, e.g. released air forms bubbles. Carry out [PREP] / [Preparing] Reduce the filling rate. Suggestion: Degas the reagent with ultrasound, nitrogen or in a vacuum. Wear Replacing piston and cylinder. [PREP] / [Preparing] is not carried out or false parameters- Carry out [PREP] / [Preparing] Correct tubing length and diameter. An incorrect volume is dosed Dosing unit either mounted or assembled incorrectly. Remove the dosing unit and then reattach it. Check whether the nominal volume on the housing and the effective cylinder volume match one another. Data of the dosing unit cannot be read. Data chip of the dosing unit mechanically damaged or impaired by chemicals. Remove the dosing drive and set it up again. Clean the data chip and the contact surfaces. Have the data chip replaced by the Metrohm Service Dept. Exchange unit recognized either not at all or incorrectly. The exchange unit has not correctly been attached. Remove the exchange unit and set it up again. Check the correct placing of the exchange unit. Check the piston and flat stopcock position. Switch the instrument off and on again. 806 Exchange Unit 27

36 6.1 Problems Problem Cause Remedy If necessary contact the Metrohm Service Dept. LED "Status" is flashing fast. LED "Status" is not illuminated although an exchange unit is attached. The dosing drive is overloaded because the stopcock is blocked. The dosing drive is overloaded because the piston is blocked.this error is displayed by the software (Touch Control or PC Control / tiamo). The data of the exchange unit cannot be read because the data chip has been damaged mechanically or by chemicals. The exchange unit has not correctly been attached. Switch off the Touch Control or exit PC Control. Check wether the exchange unit can be removed. If it cannot be removed, check wether the flat stopcock still can be turned. Switch it manually to the exchange position turning it to the right. Remove the exchange unit and proceed as described in the manual for the exchange unit. Switch the control device off and then on again. The dosing device is being initialized during switching on. Remove the exchange unit and clean it as described in the manual for the exchange unit in chapter "Care and maintenance". Contact the Metrohm service if removing the exchange unit is not possible. Have the data chip being replaced by the Metrohm service.until the data chip is being replaced you can remove the data chip yourself in order to be able to still use the exchange unit. The cylinder volume is automatically recognized nevertheless, but no data can be read from the exchange unit or be saved on it anymore. Remove the exchange unit and attach it again until it snaps in. The LED flashes during data is read from an intelligent exchange unit and lights up constantly if the exchange unit has correctly been recognized. No dosing takes place at all Tubing connections are blocked or dosing unit is not assembled correctly. Check whether the dosing tip is blocked. Check whether the dosing tubing is connected to the correct port. Check whether the dosing port is sealed off with a stopper. Check whether the VENT port is sealed off with a stopper (vacuum in the supply bottle!). The VENT port must be open for pressure compensation Exchange Unit

37 6 Troubleshooting Problem Cause Remedy Remove the dosing drive and check whether the dosing piston is connected to the dosing drive. The piston stopper must be flush with the upper side of the housing. Check whether the connection cable is attached to the dosing drive. The exchange unit cannot be attached. The exchange unit cannot be removed and the LED "Status" is flashing slowly. The flat stopcock of the exchange unit is not in the exchange position. The piston rod in the exchange unit is not in the right position. It is being dosed or filled and/or the Titrando is not in the exchange position. Switch the flat stopcock manually to the exchange position (lever switch directed to the right). Switch the piston rod to the right position. Stop the run or carry out a "filling". 806 Exchange Unit 29

38 7.1 Buret data 7 Appendix 7.1 Buret data 7.2 Dosing accuracy The 806 Exchange Unit is equipped with a data chip which contains the specifications for the exchange unit, the tubing connections and the reagent used. Indications on exchange unit / tubing connections Order number of the exchange unit Serial number of the exchange unit Serial number of the dosing cylinder Length and diameter of the tubings on the dosing ports Validation date etc. Indications on the reagent Name of the reagent Titer of the reagent Concentration of the reagent Production and expiry date of the reagent etc The 806 Exchange Unit makes it possible to read and overwrite data with the aid of a suitable device (e.g. Titrando). Consult the respective manual in order to determine whether the Metrohm device which you are using is capable of accomplishing this. Every exchange unit is subjected to a strict quality inspection prior to shipment. Every exchange unit is issued a quality certificate attesting conformance with the quality criteria of Metrohm Typical measurement deviation The accuracy of exchange units can be seen in the following table. The values listed are to be regarded as typical values which can be achieved with a Titrando Exchange Unit

39 7 Appendix Table 1 Typical measurement deviation of Metrohm exchange units Cylinder volume max. systematic deviation 1 ml ± 3 µl 5 ml ± 15 µl 10 ml ± 20 µl 20 ml ± 30 µl 50 ml ± 50 µl The ISO/EN/DIN standard The Metrohm exchange units fulfil the requirements of the ISO/EN/DIN standard Volume measurement instruments with pistons Part 3: Piston burets. Metrohm guarantees that its exchange units are in compliance with the following limit values at the time of shipment: Table 2 Permissible limit values as per ISO/EN/DIN Cylinder volume max. systematic measurement deviation max. permissible measurement deviation 1 ml ± 0.6 % ± 6 µl ± 0.1 % ± 1 µl 5 ml ± 0.3 % ± 15 µl ± 0.1 % ± 5 µl 10 ml ± 0.2 % ± 20 µl ± 0.07 % ± 7 µl 20 ml ± 0.2 % ± 40 µl ± 0.07 % ± 14 µl 50 ml ± 0.2 % ± 100 µl ± 0.05 % ± 25 µl The Metrohm agents worldwide offer the possibility of on-site exchange unit inspections and certifications with respect to accuracy. We recommend that an accuracy inspection be performed when the dosing cylinders and dosing pistons of an exchange unit are replaced. 806 Exchange Unit 31

40 8.1 Scope of delivery 8 Accessories 8.1 Scope of delivery NOTE Subject to change without notice Exchange Unit xxx Qty. Order no. Description xxx 806 Exchange Unit Exchange unit with integrated data chip with 1, 5, 10, 20 and 50 ml glass cylinder and light protection. PCTFE/PTFE flat stopcock, FEP tubing connection, antidiffusion buret tip and standard amber glass reagent bottle : 1 ml : 5 ml : 10 ml : 20 ml : 50 ml Tip / Thread M6 Tip with M6 thread. Together with the capillary tubing and the link stopper it provides the entire buret tip. Material: ETFE/FEP Length (mm): Exchange Unit

41 8 Accessories Qty. Order no. Description Adsorber material, complete for the exchange unit Holding clamp for bottles Holding spring for reagent bottles and exchange units Labeling plates for intelligent exchange unit Set of 10 pieces, in various colors Wrench For tightening connectors Length (mm): Insert for For exchange units ( xxx), all volumes. 806 Exchange Unit 33

42 8.2 Optional accessories Qty. Order no. Description Grease (2 g) Special quality (silicone-free). For grease-free ground joint connections, see XXX ML 806 Exchange Unit Manual 8.2 Optional accessories Order no. Description Thermostat casing for 806 Exchange Units For exchange units XXX Exchange unit body / 20 ml Material: PBTE Volume (ml): Exchange Unit

43 8 Accessories Order no. Description Round glass bottle / 1000 ml / GL 45 Material: Clear glass Height (mm): 223 Volume (ml): PE bottle / 1000 ml / GL 45 For exchange units. Bottle for auxiliary solutions Material: PE Width (mm): 96 Height (mm): 223 Volume (ml): Exchange Unit 35

44 Index Index A Accuracy Antidiffusion tip B Bottle attachment Buret data Buret tip Crystallizing Storage C Certification Crystallizing D Data chip... 11, 28, 30 Data exchange Dosing accuracy Dosing cylinder Material Dosing piston Material Dosing position... 9 Dosing tip Open Dosing tubing E Exchange unit... 29, 28 F Filling tube Flat stopcock of ceramic of PCTFE/PTFE Function PREP Preparing G GLP Good Laboratory Practice L LED Status... 11, 12, 28, 29, 28 Light protection Material O Order number P PETG Piston blocked Piston rod... 9, 11, 19 Production date Q Quality certificate Quality control R Reagent Concentration Crystallizing Expiry date Name Production date Titer S Serial number SOP Stopcock Material Stopcock blocked Storage vessel Switching lever... 9, 10, 19 T Thread Tubing diameter Tubing length V Validation Validation date Exchange Unit