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Summary of Contents for Metrohm 860 KF Thermoprep
- Page 1 860 KF Thermoprep Manual 8.860.8003EN / 2019-12-02...
- Page 3 Metrohm AG CH-9100 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 / 2019-12-02...
- Page 4 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.
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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 ............ 28 5.1.1 Preparing the KF titration cell ..........28 5.1.2 Preparing the 860 KF Thermoprep ......... 29 Determining the blank value ..........32 Determining samples ............33 6 Operation and maintenance General ................35 Care ..................
- Page 7 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Table of figures Figure 1 Front 860 KF Thermoprep ..............6 Figure 2 Rear 860 KF Thermoprep ..............7 Figure 3 Loosening the adapter ............... 9 Figure 4 Mounting the support rod ............... 10 Figure 5 Mounting the tubing ...............
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Page 9: Introduction
1 Introduction Instrument description The 860 KF Thermoprep is used wherever the heating of a sample and/or the thermal expulsion of moisture in solids or liquids is required. In combi- nation with a coulometric or volumetric KF titrator, the 860 KF Thermo-... -
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 water content determination using Karl Fischer titration (coulometric or volumetric). -
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 glasses and working clothes suitable for laboratory work while operating the 860 KF Thermoprep. WARNING The oven and the sample vessels can reach temperatures of up to 250 °C! Avoid direct skin contact. Use the provided septum crimping tongs or another suitable holding device to insert the sample vessels into or remove them from the oven. -
Page 13: Flammable Samples And Solvents
The correct disposal of your old instrument will help to prevent negative effects on the environment and public health. More details about the disposal of your old instrument can be obtained from your local authorities, from waste disposal companies or from your local dealer. ￭￭￭￭￭￭￭￭ 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 holder (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: Setting Up The Instrument
Unplug the power plug immediately if you suspect that moisture has ￭ gotten inside the instrument. Only personnel who have been issued Metrohm qualifications may ￭ perform service and repair work on electrical and electronic parts. ￭￭￭￭￭￭￭￭... -
Page 17: Mounting The Support Rod
1 Move the guide head of the support rod a bit downwards by press- ing the locking lever. Figure 3 Loosening the adapter 2 Loosen the adapter on the head of the support rod with a hex key. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 18: Figure 4 Mounting The Support Rod
6 Pull out the tubing inside the support rod as far as possible. You might want to use a piece of sand paper to be able to better grasp the tubing. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 19: Figure 5 Mounting The Tubing
Figure 6 Attaching the adapter 9 Attach the adapter to the support rod. Fasten the screw into the sup- port rod with the aid of a hex key. 10 Carefully push the support rod downwards. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 20: Mounting The Sample Holder
The screw and the corresponding hex key are enclosed separately with the instrument. Mounting the sample holder 6.2063.010 6.2627.000 Figure 8 Mounting the sample holder NOTICE The sample holder may not be inserted or removed unless it has cooled down. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 21: Mounting The Needles
3 Installation The dimensions of the supplied sample holder are optimized for the usage of 6.2419.007 6-mL sample vials by Metrohm. This ensures the best possi- ble transfer of heat between oven and sample. 1 Place the 6.2627.000 oven insert into the oven from above. -
Page 22: Figure 9 Mounting The Needles
Ensure that the white PTFE seal sits firmly on the needle. 4 Screw the 6.1805.100 FEP tubing onto the opening of the distri- butor by hand. Screw the other end of the tubing onto the opening on the upper side of the support rod. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 23: Mounting The Heating Tubing
The cable holder prevents the cable of the heating tubing from coming into contact with parts of the housing that are hot. 4 Connect the heating tubing cable to the Outlet heater connector on the rear of the instrument. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 24: Mounting The Dust Filter
The installed air pump must be protected from dust. For this reason, a 6.2724.010 dust filter must be placed on the air inlet (Inlet filter) on the right-hand side of the housing.. 6.2724.010 Figure 12 Mounting the dust filter The dust filter should be replaced once a year. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 25: Assembling Drying Flasks
Tighten the caps by hand. NOTICE If drying flask caps or filter tubes are not tightened well, the gas flow may not be precise and regular. The error message "Flow rate error" usually occurs when screw connections are not tight. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 26: Figure 14 Mounting The Tubings
4 Screw the 6.1805.010 FEP tubing (13 cm length) tightly onto the remaining M6 connectors of the drying flasks. The Drying flask marking on the right-hand side of the instrument displays the diagram for the tubing. NOTICE Tighten the screw connections well by hand. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 27: Assembling The Air/Nitrogen Connector
3.10 Inserting the heating tube into the KF titration cell The 860 KF Thermoprep can be used in combination with a KF coulometer or a volumetric KF titrator. The mounting of the tip of the heating tube is accomplished in different ways for the respective KF titration cells. -
Page 28: Figure 16 Coulometric 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. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 29: Figure 17 Volumetric Kf Titration Cell
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... -
Page 30: Switching The Instrument On And Off
[FLOW] Switches the gas flow on or off. [TEMP] Switches between the two target temperatures. [QUIT] No function. [OK] Opens parameter menu. [◀] Reduces the gas flow by 1 mL/min during operation. Press the key shortly. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 31: The Display
Table 1 Icons of the status display Icon Meaning The oven is heated. The oven is cooled. The predefined temperature has been reached. An error has occurred. The error type is shown in the sta- tus display. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 32: Error Messages
Selection of predefined values from a list. Parameters with selection ￭ lists are marked with a colon (:). Modifying numerical values. ￭ The various parameters can be selected using the [▼] and [▲] arrow keys. The current line will be displayed reversed. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 33: Selecting From A Selection List
Modified values are applied by pressing [OK]. A modification is discar- ded with [QUIT]. Temp. 1 Default value for temperature 1. Input range 50 - 250 °C (Increment: 1) Default value 100 °C Temp. 2 Default value for temperature 2. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... - Page 34 Only if 'gas type' = 'other'. Input range 0.001 - 2.000 (Increment: 0.001) Default value 1.000 Flow source Selection of the gas supply. Selection pump | valve Default value pump pump Built-in air pump. valve Inlet valve for inert gas. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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Page 35: Configuration
-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 engineer. Contact your responsible Metrohm supplier. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 36: 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 37: 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 38: Figure 21 Insert The Sample Vessel Into The Oven
Inserting the needle 1 Grip the guide head with both hands and press the fixing lever. Figure 22 Move the guide head down 2 Move the guide head down and insert the needle into the sample vessel. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 39: Figure 23 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 40: 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 30 ff. -
Page 41: 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 42 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 30 ff.
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Page 43: Operation And Maintenance
6 Operation and maintenance 6 Operation and maintenance General The 860 KF Thermoprep requires appropriate care. Excess contamination of the instrument may result in malfunctions and a reduction in the service life of the sturdy mechanical and electronic components. Severe contamination can also have an influence on the measured results. -
Page 44: 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 45: Appendix
An individual measuring factor can be entered with the Meas. factor parameter so that the corrected gas flow is displayed. At the same time, however, other must be selected for the Gas type parameter. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 46: Literature
The system must be conditioned with an empty, sealed sample vial (condi- tioning vial) before a determination is made. Literature ® Manual, Riedel-de Haën E. Scholz, Hydranal ￭ P. Bruttel, R. Schlink, Water Determination by Karl Fischer Titration ￭ Monograph, Metrohm, 2006, Order no. 8.026.5013 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 47: Technical Specifications
Under normal conditions, calibrated with air at approx. +25 °C and 1,013 mbar. Deviations of gas amount per time unit of ±20% are possible. Outlet heater Socket connection U = 16 ±1 V I ≤ 0.8 A Typical tubing approx. 50 °C temperature ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 48: Power Connection
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 bottom: Steel sheet, stove-enameled Oven covering PTFE Operating unit Polycarbonate / Acrylonitrile butadiene styrene (PC/ABS) ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 49: 10 Accessories
The PDF file with the accessories data is created. NOTICE Once you have received your new product, we recommend download- ing the accessories list from the Internet, printing it out and keeping it together with the manual for reference purposes. ￭￭￭￭￭￭￭￭ 860 KF Thermoprep... -
Page 50: Index
Fan ..........7 KF titration cell ....19 Valve ........26 Fixing lever ......6, 30 Needle ....... 13 Flow rate ........23 Sample holder ....12 Flow rate error ......17 Flow source ......26 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep...
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