Metrohm 917 Coulometer Tutorial
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Metrohm 917 Coulometer Tutorial

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917 Coulometer
Tutorial
8.917.8001EN

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  • Page 1 917 Coulometer Tutorial 8.917.8001EN...
  • 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 917 Coulometer Tutorial 8.917.8001EN 01.2019...
  • 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.

  • Page 5: Table Of Contents

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents Table of contents 1 Introduction Structure of the tutorial ............1 Additional information ............1 Symbols and conventions ............ 1 2 Installation Setting up and connecting the instrument ......3 Setting up the titration cell for coulometry ....... 7 2.2.1 Inserting the titration cell ............
  • Page 6 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents Carrying out the water content determination ....40 7 Performing titration with supplementary functions Saving the determination and the PC/LIMS report ..45 Modifying the titration parameters ........47 Creating a sample table ............. 48 Carrying out titrations using the sample table ....51 8 Setting up the user administration Creating a user list ..............
  • Page 7 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Table of figures Figure 1 Connecting the power supply unit ............. 3 Figure 2 USB/RS-232 adapter ................4 Figure 3 Connecting the USB cable ..............6 Figure 4 Inserting the titration cell ..............7 Figure 5 Filling the adsorber tube ..............

  • Page 9: Structure Of The Tutorial

    Additional information General information regarding coulometric Karl Fischer titration can be found in the monograph "Water Determination by Karl Fischer Titration" at www.metrohm.com (8.026.5011 DE; 8.026.5013 EN). Symbols and conventions The following symbols and formatting may appear in this documentation:...
  • Page 10 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1.3 Symbols and conventions WARNING This symbol draws attention to a possible biological hazard. CAUTION This symbol draws attention to possible damage to instruments or instrument parts. NOTE This symbol highlights additional information and tips. ￭￭￭￭￭￭￭￭...

  • Page 11: Setting Up And Connecting The Instrument

    2 Installation Setting up and connecting the instrument Connecting the power supply unit The 917 Coulometer has an external power supply unit for a 24 V power supply (DC). This is connected to the power socket of the Coulometer. WARNING An incorrect supply voltage can damage the instrument.

  • Page 12: Figure 2 Usb/Rs-232 Adapter

    For this purpose, check the manual for the balance. The following table offers an overview of the balances that you can use together with the 917 Coulometer and of which cable you will need for connection to the RS-232 interface: ￭￭￭￭￭￭￭￭...
  • Page 13 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation Balance Cables AND ER, FR, FX with RS-232 inter- 6.2125.020 + 6.2125.010 face (OP-03) Mettler AB, AG, PR (LC-RS9) In the scope of delivery for the balance Mettler AM, PM, PE with interface 6.2146.020 + 6.2125.010 option 016 Also from Mettler: ME 47473 adapter and either ME 42500 hand switch or ME 46278 foot...

  • Page 14: Figure 3 Connecting The Usb Cable

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.1 Setting up and connecting the instrument Connecting printers or other USB devices Figure 3 Connecting the USB cable A printer can be connected to the USB connector (Type A) (with a 6.2151.020 connecting cable), as can a USB keyboard, a barcode reader or a USB flash drive (for storing and loading methods, etc.).

  • Page 15: Setting Up The Titration Cell For Coulometry

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation Setting up the titration cell for coulometry 2.2.1 Inserting the titration cell Figure 4 Inserting the titration cell Set up the titration cell on the magnetic stirrer as follows: 1 Attach the 6.2047.040 titration vessel holder to the magnetic stirrer. 2 Insert the 6.1464.320 titration cell into the titration vessel holder.

  • Page 16: Figure 5 Filling The Adsorber Tube

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 Setting up the titration cell for coulometry 6.1403.030 6.2811.000 Figure 5 Filling the adsorber tube 1 Insert a small cotton plug into the bottom of the adsorber tube. Do not pack the cotton too tightly. 2 Fill the adsorber tube to ¾ with molecular sieve granulate. 3 Place a small cotton plug on the molecular sieve.

  • Page 17: Figure 6 Equipping The Titration Cell

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation Equipping the titration cell 6.1403.030 6.2713.020 6.0341.100 6.0345.100 6.0344.100 6.2713.000 6.1437.000 6.2701.040 6.2713.010 6.1448.020 6.1464.320 6.1903.030 Figure 6 Equipping the titration cell Equip the titration cell as follows: 1 Place the 6.1903.030 stirring bar in the titration cell. 2 Cut the 6.2713.0x0 ground-joint sleeves to the correct length and attach them to the ground joints of the inserts (electrodes, adsorber tube, etc.).
  • Page 18 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 Setting up the titration cell for coulometry 4 Insert the 6.0345.100 generator electrode without diaphragm or the 6.0344.100 generator electrode with diaphragm together with the adsorber tube into the large ground-joint opening at the rear. 5 Insert the 6.0341.100 indicator electrode into the left ground-joint opening.

  • Page 19: Mounting The Addition And Aspiration Tube

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation 2.2.3 Mounting the addition and aspiration tube Figure 7 Mounting the addition and aspiration tube Insert the addition and aspiration tube as follows into the titration cell: 1 Attach the 6.2713.000 ground-joint sleeve that has been cut to size to the ground joint of the 6.1437.000 stopper.

  • Page 20: Titration Cell With Aspiration Equipment (Utilization With Dosino)

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 Setting up the titration cell for coulometry 2.2.4 Titration cell with aspiration equipment (utilization with Dosino) A Dosino allows the automatic replacement of reagents. For aspiration, the 6.5617.000 aspiration equipment is used, along with a complete dosing unit and a 50 mL glass cylinder. For aspirating greasy samples when only the sample and not the whole reagent is to be aspira- ted, we recommend using a dosing unit with a 20 mL cylinder.

  • Page 21: Using The Titration Cell With A Karl Fischer Oven

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation Figure 8 Titration cell with aspiration apparatus 4 Place the stopper with the attached aspiration tip into the ground- joint opening with the ground-joint sleeve. Insert the aspiration tip into the titration cell until it almost touches the vessel base.

  • Page 22: Using The Titration Cell With A Sample Changer

    Box (6.2141.340) cable. The cable transfers start and stop signals of the 885 Compact Oven Sam- ple Changer to the connected 917 Coulometer, and (in the opposite direc- tion) status signals of the coulometer (Cond OK, EOD) to the 885 Com- pact Oven Sample Changer.

  • Page 23: Connecting Sensors

    2 Installation Figure 9 Remote connection 885 Compact Oven SC – Remote Box – 917 Coulometer The 917 Coulometer is operated in KFC mode. The sample series is started on the 885 Compact Oven Sample Changer. 2.2.7 Connecting sensors The measuring interface contains the following measuring inputs: Gen.

  • Page 24: Figure 10 Unscrewing The Protective Cap From The Generator Electrode

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 Setting up the titration cell for coulometry Figure 10 Unscrewing the protective cap from the generator elec- trode 2 Tighten the 6.2104.120 electrode cable to the generator electrode. 6.2104.120 Figure 11 Screwing the electrode cable to the generator electrode Connecting the electrode cable to the coulometer 1 Plug the electrode plug into the Gen.

  • Page 25: Figure 12 Connecting A Generator Electrode

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation Figure 12 Connecting a generator electrode NOTICE The electrode cable is protected against accidental disconnection of the cable by means of a pull-out protection. If you wish to pull out the plug again, you first need to pull back the outer plug sleeve.

  • Page 26: Figure 14 Screwing The Electrode Cable To The Indicator Electrode

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 Setting up the titration cell for coulometry 6.2104.020 Figure 14 Screwing the electrode cable to the indicator electrode Connecting the electrode cable to the coulometer 1 Plug the electrode plug into the Ind. socket of the coulometer. Figure 15 Connecting an indicator electrode ￭￭￭￭￭￭￭￭...
  • Page 27 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation NOTICE The electrode cable is protected against accidental disconnection of the cable by means of a pull-out protection. If you wish to pull out the plug again, you first need to pull back the outer plug sleeve. 2.2.7.3 Connecting a temperature sensor A temperature sensor of the Pt1000 or NTC type can be connected to the...

  • Page 28: Setting Up The Aspiration And Reagent Bottle

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.3 Setting up the aspiration and reagent bottle Setting up the aspiration and reagent bottle Mode of operation of the built-in pump With the built-in pump, one can on the one hand add fresh reagent easily at the press of a button, while on the other hand one can also empty the titration cell (coulometry) at the press of a button.
  • Page 29 The reagent is pumped out of the supply bottle by overpressure and into the titration cell. All of the bottle cap connectors must be leak-proof for this reason. Metrohm offers suitable thread adapters for bottles with other threads than GL 45. 6.1805.200 6.1609.010...
  • Page 30 Setting up the aspiration bottle The aspiration bottle is used as a waste container and must be sealed against leaks. Metrohm offers suitable thread adapters for bottles with other threads than GL 45. ￭￭￭￭￭￭￭￭...
  • Page 31 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation 6.1801.120 6.1805.200 6.1808.050 6.1819.050 6.1446.040 6.1446.090 6.1602.105 6.1623.000 6.1608.030 To equip the aspiration bottle, proceed step-by-step as follows: 1 Place a 6.1446.040 threaded stopper in the M6 connector (smallest opening) of a 6.1602.105 bottle cap and screw it tightly. 2 Introduce the 6.1623.000 overflow protection into the M8 connec- tor from below (second-smallest opening) of the bottle cap.

  • Page 32: Connecting A Pump

    8 Insert a 6.1805.200 PTFE tubing with M8 connector into the opening of the stopper and screw it tightly. Connecting a pump Connecting tubings to the pump The pump connectors of the 917 Coulometer are located on the rear of the instrument. Figure 16 Connecting the PVC tubings Take care to ensure that you connect the tubings to the pump correctly.

  • Page 33: Switching The Instrument On And Off

    Information about changing the dialog language can be found in the following section. Proceed as follows: Press the power switch on the left-hand side of the back panel of ￭ the 917 Coulometer. The 917 Coulometer is initialized. A system test is performed. This process takes some time. ￭￭￭￭￭￭￭￭...
  • Page 34 Switching off the instrument CAUTION The 917 Coulometer must be switched off by pressing the power switch on the rear of the instrument before the electricity supply is interrupted. If this is not done, then there is a danger of data loss.

  • Page 35: Selecting The Dialog Language

    The current data is saved and the system is shut down. This process takes just a short time. At the same time, all other instruments con- nected to the 917 Coulometer via a USB cable are also being switched off.

  • Page 36: Touch-Sensitive Screen

    You can always return to the main dialog by touching [ In order to activate an element on the 917 Coulometer user interface, just touch the screen with your fingertip, finger nail, the eraser of a pencil or a stylus (special tool for operating instruments with touch-sensitive screens).
  • Page 37 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Fundamentals of operation Table 1 Fixed keys which are always available [Home] always opens the main dialog. [Back] saves the entry and opens the next-higher dialog page. [Help] opens the online help for the dialog displayed. [Print] opens the printing dialog. [Manual] opens the manual control.

  • Page 38: Status Display

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.3 Status display Status display The current status of the system is displayed in the upper right-hand cor- ner of the title bar. Table 3 Status displays The instrument is in normal status. The working medium is being conditioned. Conditioning has been paused.

  • Page 39: Entering Text And Numbers

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Fundamentals of operation Entering text and numbers In the editing dialog for text or numerical input, enter the individual char- acters by tapping in the input field. The following functions are available: Text editor Table 4 Editing functions [OK] The modification is applied and the editing dialog is exited.
  • Page 40 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.4 Entering text and numbers Number editor Table 5 Editing functions [OK] The modification is applied and the editing dialog is exited. [Cancel] The editing dialog is exited without applying the modification. [Delete entry] The content of the input field is deleted com- pletely.

  • Page 41: Preparing Instruments And Material

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Setup and configuration 5 Setup and configuration Preparing instruments and material What you will need: A 917 Coulometer, including accompanying accessories ￭ An analytical balance ￭ A water standard with a water content, e.g., of 1 mg/g ￭...

  • Page 42: Configuring A Printer

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.3 Configuring a printer NOTICE A suitable method (aspirating used reagent, adding fresh reagent) must be available for automatic reagent replacement. This will be started automatically when the set limit has been reached. NOTICE Note that the catholyte solution must be replaced manually when a generator electrode with diaphragm is used for automatic reagent replacement.
  • Page 43 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Setup and configuration 2 Entering the printer data Select Printer and tap on [Edit]. ￭ Tap on the selection symbol next to the input field Printer and ￭ select a printer type. Once you have connected a USB printer, tap on the selection sym- ￭...

  • Page 44: Creating A Titration Method

    Creating a titration method Below you will find a description of how to create your own method for water content determination. The 917 Coulometer contains method tem- plates which are already configured except for a few parameters. The water content of a sample should be determined by means of a triple determination.
  • Page 45 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Carrying out the water content determination of a sample 2 Selecting a Karl Fischer command Highlight the line KFC. ￭ Tap on [Edit command]. ￭ A selection of parameters (e.g. start conditions) and instruments (e.g. dosing devices, see next step) appears, which can be selected and adjusted individually.
  • Page 46 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.1 Creating a titration method NOTICE The calculation is carried out continuously, i.e. the calculation is updated after every determination that is carried out until the defined number of determinations has been reached. Under [More options], define parameters, e.g., Save result in ￭...
  • Page 47 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Carrying out the water content determination of a sample Tap on [Method options]. ￭ Here you can define the statistics function for this method. You can specify the number of determinations for which the respective statistical calculations are to be carried out. These settings apply for all determinations which are carried out with this method.

  • Page 48: Carrying Out The Water Content Determination

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.2 Carrying out the water content determination 7 Saving a method Tap on [Save method]. ￭ You can save the method in the instrument's internal memory, on a USB storage medium or in a shared data directory in a network. In addition, you can also create different groups and/or folders for the methods.
  • Page 49 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Carrying out the water content determination of a sample The water seeping in is titrated off continuously (basic drift). Entering sample data in the main dialog 1 Entering sample identification and sample size Tap on the input field Identification 1. ￭...
  • Page 50 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.2 Carrying out the water content determination 2 Tare the balance with the prepared sample and then remove the sample from the balance once again. 3 Tap on the start key [ Conditioning is stopped. The request for adding the sample will be displayed for 8 s.
  • Page 51 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Carrying out the water content determination of a sample NOTICE The sample size can also be adopted directly from a connected balance. The titration curve is shown live. ￭ After the completion of the titration, the results dialog is dis- played.
  • Page 52 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.2 Carrying out the water content determination If you would like to exclude a titration from the statistical calculation, you can select it and then tap on [Result on/off] or [Determ. on/off]. The recalculation of the statistics data will be performed immediately. If you would like to add other titrations to the statistics, you can do this in the statistical overview.

  • Page 53: Performing Titration With Supplementary Functions

    PC through a serial connection. PC/LIMS reports can be saved either as TXT file (in accordance with ISO 8859-1) or UTF8 file. The tiBase database software from Metrohm is available to you for administering the determination data on the PC. Defining the automatic saving...
  • Page 54 (memory location in a computer network). A USB flash drive (external memory 1) must be plugged in on the 917 Coulometer before a determination is carried out. This mem- ory location must already be defined in the device manager at the time of the selection of a shared memory location in a computer network.

  • Page 55: Modifying The Titration Parameters

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Performing titration with supplementary functions NOTICE The settings for the PC/LIMS report (memory, RS-232, coding) must be undertaken in the "Edit instrument/PC/LIMS report" dia- log. Modifying the titration parameters You can optimize a titration run by modifying individual titration parame- ters according to the needs of your analysis.

  • Page 56: Creating A Sample Table

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.3 Creating a sample table Modifying the settings for the titration 1 Setting an extraction time NOTICE The input of an extraction time is recommended, e.g., with sam- ples that release water slowly or if a Karl Fischer oven (e.g., 885 Compact Oven SC) is used.
  • Page 57 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Performing titration with supplementary functions Filling the sample table with sample data 1 Activating the sample table In the main dialog, tap on [Control]. ￭ Activate the Sample table check box. ￭ Return to the main dialog with the [ ] fixed key.
  • Page 58 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.3 Creating a sample table 2 Entering the sample data Tap on [Sample table]. ￭ The sample table is still empty. The first line is highlighted. Tap on [Edit]. ￭ Tap on the selection symbol next to the input field Method. ￭...

  • Page 59: Carrying Out Titrations Using The Sample Table

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Performing titration with supplementary functions Fill out the fields for sample identification and the sample size. ￭ The line number is automatically increased by one after the sam- ple size has been entered. The next sample size can be entered directly.

  • Page 60: Setting Up The User Administration

    8 Setting up the user administration If different persons are working on the instrument, we recommend that the user administration of the 917 Coulometer be used. This means that everyone can use their user identification to log on to the instrument. The reports will then automatically contain the respective user name.
  • Page 61 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Setting up the user administration 2 Creating a new user Tap on [New]. ￭ Tap on the input field User and enter an unambiguous user iden- ￭ tification (e.g.,abbreviation). Close the input dialog with [OK]. Tap on the input field Full name and enter the name of the user. ￭...

  • Page 62: Automatic Login With Usb Flash Drive

    1 Plugging in the USB flash drive Return to the main dialog with [ ￭ Plug in a USB flash drive into the rear of the 917 Coulometer. ￭ Wait until a message appears which confirms that the USB flash ￭...
  • Page 63 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Setting up the user administration Setting the login options NOTICE The following steps are possible only if the user has administrator rights. Proceed as follows: 1 Opening the login options In the user administration, tap on [Login options]. ￭...

  • Page 64: Login With Password

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8.3 Login with password 3 Logging in Tap on [OK] after the request that you plug in the USB flash drive ￭ with your ID profile. In order to log in another user with ID profile, tap in the main dia- ￭...
  • Page 65 Activate Password required. ￭ Many settings are possible in the login options. Consult the manual of the 917 Coulometer to look these up if necessary. NOTICE The login dialog is called up as soon as you exit the login options dialog...
  • Page 66 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8.3 Login with password 2 Defining a password Tap on the input field New password. ￭ Enter a password. It may not be more than 10 characters long. ￭ NOTICE Note the password. Confirm the entry with [OK]. ￭ Enter the password once again under Confirm password.

  • Page 67: Index

    ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index Index Instrument Addition and aspiration tube Reagent bottle Switch off ......26 Mount ........ 11 Set up ........ 21 Switch on ......25 Adsorber tube Fill ........7 Sample changer Aspiration bottle Karl Fischer oven With oven module ....14 Set up ........

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