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Related Manuals for Metrohm 860 KF
Summary of Contents for Metrohm 860 KF
- Page 1 860 KF Thermoprep Manual 8.860.8003EN...
- Page 3 Metrohm AG CH-9101 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com 860 KF Thermoprep Manual 8.860.8003EN 07/2011 dm...
- Page 4 Teachware Metrohm AG CH-9101 Herisau teachware@metrohm.com 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...
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Page 5: Table Of Contents
3.10 Inserting the heating tube into the KF titration cell ..19 4 Operation Switching the instrument on and off ....... 22 The keypad ................22 The display ................23 4.3.1 Display elements ..............23 4.3.2 Status display ................ 23 4.3.3 Error messages ..............24 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... - Page 6 5 Performing a determination Conditioning the system ............ 29 5.1.1 Preparing the KF titration cell ..........29 5.1.2 Preparing the 860 KF Thermoprep ......... 30 Determining the blank value ..........33 Determining samples ............34 6 Handling and maintenance General ................36 Care ..................
- Page 7 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents 10.3 Quality Management Principles ........46 11 Accessories 11.1 Scope of delivery 2.860.0010 ..........48 11.2 Optional accessories ............55 Index ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
- Page 8 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Table of figures Figure 1 Front 860 KF Thermoprep ..............6 Figure 2 Rear 860 KF Thermoprep ..............7 Figure 3 Connecting the mains cable .............. 8 Figure 4 Loosen the adapter ................9 Figure 5 Mounting the guidance rod .............
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Page 9: Introduction
1 Introduction Instrument description The 860 KF Thermoprep is used whenever the heating up of a sample and/or the thermal expulsion of moisture in solid substances or liquids is required. In combination with a coulometric or volumetric KF titrator, the... -
Page 10: Intended Use
1.2 About the documentation 1.1.2 Intended use The 860 KF Thermoprep is designed for usage as an auxiliary device for sample preparation in analytical laboratories. Its main area of application is moisture determination according to Karl Fischer (coulometric or volumet- ric). -
Page 11: Safety Instructions
Electrical safety The electrical safety when working with the instrument is ensured as part of the international standard IEC 61010. Warning Only personnel qualified by Metrohm are authorized to carry out service work on electronic components. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 12: Personnel Safety
Personnel safety Warning Wear protective goggles and working clothes suitable for laboratory work while operating the 860 KF Thermoprep. Warning The oven and the sample vessels can be at a temperature of up to 250 °C! Avoid direct skin contact. Use the septum-sealing tongs sup- plied or another suitable holding device for inserting the sample vessels in the oven or removing them. -
Page 13: Flammable Samples And Solvents
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. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 14: Overview Of The Instrument
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument Figure 1 Front 860 KF Thermoprep Guide head Needle holder (6.2049.040) With needle adapter. Spring sleeve Guidance rod With vessel stripper. Sample vessel (6.2419.007) Sample insert (6.2063.010) With 6 ml content. Oven module Fixing lever With sheet metal housing. -
Page 15: Figure 2 Rear 860 Kf Thermoprep
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument Figure 2 Rear 860 KF Thermoprep Air pump inlet Mains switch With 6.2724.010 dust filter. Mains connection socket Type plate Contains specifications concerning mains voltage and serial number. Outlet heating connection Air/nitrogen connector For the heating tube. -
Page 16: Installation
Connecting the mains cable Warning This instrument must not be operated except with the mains voltage specified for it (see rear of the instrument). Protect the connection sockets against moisture. Figure 3 Connecting the mains cable ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 17: Mounting The Guidance Rod
4 Insert the tubing jutting out of the housing from below into the guid- ance rod. Note This tubing conveys the gas from the flow controller upward through the guidance rod to the guide head. From there the gas is guided to the double hollow needle, see next chapter. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 18: Figure 5 Mounting The Guidance Rod
Figure 6 Mounting tubing 7 Fasten the tubing on the olive of the 4.860.4260 adapter. 8 Pull out the guidance rod as far as possible in order that the adapter rests close on the guidance rod. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 19: Figure 7 Fix The Adapter
10 Carefully push the guidance rod downwards. Figure 8 Guidance rod mounted 11 Fix the guidance rod with the V.0434.008 hexagon screw according to the drawing. The screw and the associated hexagon key are pack- aged separately with the instrument. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 20: Mounting The Sample Insert
The dimensions of the supplied sample insert are optimized for the usage of 6 mL sample vials 6.2419.007 from Metrohm. This ensures the best possible transfer of heat between oven and sample. 1 Place the 6.2627.000 oven insert into the oven from above. -
Page 21: Mounting The Needles
The 6.2049.050 needle holder can be ordered from Metrohm if required. Needle holders with the dimensions required for situations calling for spe- cial sample vessels can be supplied by Metrohm upon request. 6.1805.100 6.2816.070 6.2049.040... -
Page 22: Mounting The Heating Tubing
Mounting the heating tubing 6.2060.010 6.1830.030 Figure 11 Mounting the heating tubing (view from rear) Proceed as follows: 1 Screw the M6 connector of the 6.1830.030 heating tubing into the side opening of the distributor on the guide head. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 23: Figure 12 Connecting The Heating Tubing
40...50 °C as soon as the instrument is switched on. This prevents the condensation of moisture in the tubing when this is expelled from the sample and transferred with the aid of a carrier gas into a KF titration cell. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 24: Mounting The Dust Filter
Dust (e. g. from the desiccant) must be prevented from finding its way into the sample vessel. 6.1602.145 6.1821.040 6.2811.000 6.1608.050 Figure 14 Preparing the drying flasks Prepare both drying flasks as follows: 1 Fill both 6.1608.050 drying flasks with 6.2811.000 molecular sieve. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 25: Figure 15 Mounting The Tubings
2 Screw one 6.1805.080 FEP tubing (25 cm length) to the gas outlet (at the front, labeled 1). Screw the other tubing end on the front dry- ing flask to the M6 connector without point marking (see left-hand arrow). ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 26: Air/Nitrogen Connector
If gas is supplied from a pressure line or a pressure vessel, then it is imperative that a pressure reduction valve be placed upstream. The gas pressure may not exceed a maximum overpressure level of 0.3 bar. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 27: Inserting The Heating Tube Into The Kf Titration Cell
3.10 Inserting the heating tube into the KF titration cell The 860 KF Thermoprep can be used for either coulometric or volumetric water determinations. The mounting of the tip of the heating tube is accomplished in different ways for the respective KF titration cells. -
Page 28: Figure 18 Volumetric Kf Titration Cell
E.3010.032 O-ring. The latter you will still need. A 6.2730.020 septum stopper is enclosed with every KF titrator ￭ made by Metrohm. Disassemble this septum stopper into three parts and remove the septum. It will not be required. 6.1830.030 6.2730.020 E.3010.032... - Page 29 The tip must not however be permitted to get in the way of the stirring bar in the KF titration cell. Afterwards give the septum stop- per its final tightening. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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Page 30: Operation
Figure 20 Keypad and operating unit The key functions in the main dialog [FLOW] Switches the gas flow on and off. [TEMP] Switches between the two target temperatures. [QUIT] No function. [OK] Opens the parameters menu. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 31: The Display
Temp. 2). Status display Shows status and error messages. 4.3.2 Status display Table 1 Symbols of the status display Symbol Significance The oven is being heated. The oven is being cooled. The pre-selected temperature was reached. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 32: Error Messages
Adj. data missing The adjustment The instrument must be data of the instru- readjusted. Inform a serv- ment are not cor- ice technician. rect. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 33: Modifying Numerical Values And Settings
2 Use the arrow keys [▲] or [▼] to modify the digits. 3 Select and modify the next digit, etc. 4 Apply the modified value with the [OK] key. Press [QUIT] if the previous value is to be restored. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 34: Parameters
Meas. factor The measuring factor for measuring the flow rate of the gas. This setting is only possible if other is selected for the gas. The corresponding measur- ing factor is automatically applied for air and nitrogen. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 35: Configuration
Parameters menu or of the gas flow rate during a determination. If the function is switched on (on), then the only switching that can be done is between Temperature 1 and Temperature 2, ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... - Page 36 -10 ... 10 °C (Increment: 1) Default value 0 °C The determination of the necessary temperature correction can be accom- plished with a special oven insert and should be performed by a service technician. Contact your responsible Metrohm supplier. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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Page 37: Performing A Determination
35 mL with a volumetric KF titration cell. The shaft of the heating tube should, however, not be immersed. 2 Align the tip of the heating tube against the vessel wall. 3 Switch on the stirrer. Set the stirring rate to high. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 38: Preparing The 860 Kf Thermoprep
It is imperative that an extraction time of at least 300 seconds be set for a determination using the heating method. 5.1.2 Preparing the 860 KF Thermoprep Switch on the 860 KF Thermoprep and select the tempera- ture The necessary settings on the 860 KF Thermoprep: 1 Switch on the instrument. -
Page 39: Figure 22 Insert The Sample Vessel Into The Oven
Inserting the needle 1 Grip the guide head with both hands and press the fixing lever. Figure 23 Move the guide head down 2 Move the guide head down and insert the needle into the sample vessel. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 40: Figure 24 Insert The Needle
Allow the system to condition for a few minutes and swirl the KF titration cell now and again in order to remove the last traces of moisture. Check whether the set oven temperature has been reached. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 41: Determining The Blank Value
Starting the blank value determination 1 Start the determination by pressing the [Start] key on the KF titrator. 2 Use both hands to move the guide head of the 860 KF Thermoprep upward while pressing the fixing lever. Refer to the illustrations on pages 31 ff. -
Page 42: Determining Samples
2 Check that the oven temperature and the gas flow rate correspond to the values which have been set. 3 Wait until the working medium in the KF titration vessel has been conditioned and the signal drift is stable. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... - Page 43 Starting the sample determination 1 Start the determination by pressing the [Start] key on the KF titrator. 2 Use both hands to move the guide head of the 860 KF Thermoprep upward while pressing the fixing lever. Refer to the illustrations on pages 31 ff.
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Page 44: Handling And Maintenance
Here you can also obtain validation documentation to provide help for carrying out the Installation Qualification (IQ = Installation Qualification) and the Operational (OQ = Operational Qualifi- cation). IQ and OQ are also offered as a service by the Metrohm agents. In ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... - Page 45 Electronic and mechanical functional groups in Metrohm instruments can and should be checked as part of regular maintenance by specialist per- sonnel from Metrohm. Please ask your local Metrohm agent regarding the precise terms and conditions involved in concluding a corresponding maintenance agreement.
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Page 46: Troubleshooting
System is leaking Check all tubing connections and drying flasks not achieved. for leaks. Pressure from external gas Adjust gas pressure (max. 0.3 bar). supply either too low or too high. Pump defective Contact a service technician. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 47: Appendix
Conditioning the system The system must be conditioned with an empty, sealed sample vial (condi- tioning vessel) before a determination is made. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 48: Literature
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8.2 Literature Literature ® -Manual, Riedel-de Haën, 1996 E. Scholz, Hydranal ￭ P. Bruttel, R. Schlink, Water determination by Karl Fischer Titration. ￭ Monograph, Metrohm, 2006, Best. Nr. 8.026.5013 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 49: Technical Data
Typical. 9 °C/min (at 180…80 °C) Dependent on temperature, sample amount and vessel dimensions Gas flow Flow range 10…150 mL/min Under normal conditions Outlet heating Socket connection U = 16 ±1 V I≤ 0.8 A Typical tubing approx. 50 °C temperature ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 50: Mains Connection
￭ EN/IEC 61000-4-2: 2001 ￭ EN/IEC 61000-4-3: 2002 ￭ EN/IEC 61000-4-4: 2004 ￭ EN/IEC 61000-4-5: 2001 ￭ EN/IEC 61000-4-6: 2001 ￭ EN/IEC 61000-4-11: 2004 ￭ EN/IEC 61000-4-14: 2004 ￭ EN/IEC 61000-4-28: 2004 ￭ NAMUR: 2004 ￭ ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 51: Ambient Temperature
Height 0.18 m (without support rod) 0.50 m (with support rod) Depth 0.23 m Weight (without 8.17 kg accessories) Material Housing Cover and base: steel sheet, stove-enameled Oven covering PTFE Operating unit Polycarbonate/Acrylonitrile butadiene styrene (PC/ABS) ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 52: Conformity And Warranty
EU directives 2006/95/EC (LVD), 2004/108/EC (EMC). It fulfils the fol- lowing specifications: EN 61326-1 Electrical equipment for measurement, control and laboratory use – EMC requirements EN 61010-1 Safety requirements for electrical equipment for measurement, control and laboratory use ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 53: Warranty (Guarantee)
Particular requirements for laboratory equipment for the heating of materials Manufacturer Metrohm Ltd., CH-9101 Herisau/Switzerland Metrohm Ltd. is holder of the SQS-certificate ISO 9001:2000 Quality man- agement system for development, production and sales of instruments and accessories for ion analysis. Herisau, 27 November, 2007 D. -
Page 54: Quality Management Principles
Components All components used in the Metrohm instruments have to satisfy the qual- ity standards that are defined and implemented for our products. Suppli- ers of components are audited by Metrohm as the need arises. - Page 55 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Conformity and warranty tional Qualification and Performance Verification of the system compo- nents or in carrying out the System Validation for the quantitative determi- nation of a substance in a given matrix. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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Page 56: Scope Of Delivery 2.860.0010
11.1 Scope of delivery 2.860.0010 Qty. Order no. Description 1.860.0010 860 KF Thermoprep Instrument for the thermal extraction of humidity from solid and liq- uid samples. 6.1446.170 Heating tube stopper for coulometric KF vessels in connection with heatable tubing con-... - Page 57 FEP tubing / M6 / 13 cm With light and kink protection Material: Inner diameter (mm): Length (mm): 6.1805.080 FEP tubing / M6 / 25 cm With light and kink protection Material: Inner diameter (mm): Length (mm): ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
- Page 58 Outer thread M6, inner thread M8. Material: PTCFE 6.1808.050 Connector tubing nozzle M8 1 M8 outer thread and 1 tubing olive. E.g. for thermostat jacket of Exchange Units and stability measuring instruments. Material: PVDF Length (mm): 31.5 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
- Page 59 Filter tube for 6.1608.050 Drying bottle. For Rancimats and Karl Fischer Ovens. Length (mm): 6.1830.030 Heatable outlet tubing Heatable outlet tubing for 860 KF Thermoprep. 6.2048.030 Guidance rod Guidance rod for 860 KF Thermoprep. 6.2049.040 Needle holder with Luer-lock for 860 KF...
- Page 60 11.1 Scope of delivery 2.860.0010 Qty. Order no. Description 6.2060.010 Cable support Used with 860 KF Thermoprep. 6.2063.010 Sample holder for 6.2419.007 sample vials (6 mL) 6.2419.007 Sample vial 6 ml / 100 pieces 6.1448.050 septum caps. Used for KF-determinations with oven.
- Page 61 Description 6.2621.120 Hexagon key 1.5 mm 6.2621.130 Hexagon key 2 mm 6.2627.000 Oven insert Used with 860 KF Thermoprep. 6.2724.010 Dust filter Dust filter for Rancimats and for Karl Fischer ovens Outer diameter (mm): Length (mm): ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
- Page 62 Injection needle Used with 832 KF Thermoprep. Material: Stainless steel (AISI 304) 6.2816.080 Outlet needle Used with KF Thermoprep and Oven Sample Processor. Material: Stainless steel (AISI 304) 6.2122.0x0 Mains cable with C13 line socket IEC-60320-C13 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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Page 63: Optional Accessories
Aluminum Material 2: Silicone Height (mm): Outer diameter (mm): 20.7 6.2049.050 Needle holder with Luer-lock for 860 KF Thermoprep Length (mm): 6.2419.000 Sample vial 6 mL / 1000 pieces For 6.1448.050 septum caps. Height (mm): Outer diameter (mm): Volume (mL): ￭￭￭￭￭￭￭￭... - Page 64 Valve ........27 KF titration cell ....19 Needle ....... 13 Sample insert ...... 12 Gas flow ....... 23, 26, 39 Warranty ........45 Tubings ......17 Gas inlet ........6 Gas outlet ........6 Needle ........13 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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Questions and answers
coulometer oven sample vessel dimensions
The sample vessel for the Metrohm 860 KF coulometer oven should have the following dimensions:
- Diameter: 10.0 to 32.0 mm
- Immersion depth: 20.0 to 45.0 mm
The oven is optimized for 6.2419.007 6-mL sample vials.
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