Metrohm 917 Coulometer Operation instructions

917 Coulometer
Tutorial
8.917.8001EN

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
917 Coulometer
Tutorial
8.917.8001EN 01.2019

Technical Communication
Metrohm AG
CH-9100 Herisau
[email protected]
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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
￭￭￭￭￭￭￭￭ III
Table of contents
1 Introduction 1
1.1 Structure of the tutorial ....................................................... 1
1.2 Additional information ......................................................... 1
1.3 Symbols and conventions .................................................... 1
2 Installation 3
2.1 Setting up and connecting the instrument ........................ 3
2.2 Setting up the titration cell for coulometry ....................... 7
2.2.1 Inserting the titration cell ......................................................... 7
2.2.2 Preparing the titration cell ........................................................ 7
2.2.3 Mounting the addition and aspiration tube ............................ 11
2.2.4 Titration cell with aspiration equipment (utilization with Dos-
ino) ....................................................................................... 12
2.2.5 Using the titration cell with a Karl Fischer oven ...................... 13
2.2.6 Using the titration cell with a sample changer ........................ 14
2.2.7 Connecting sensors ............................................................... 15
2.3 Setting up the aspiration and reagent bottle .................. 20
2.4 Connecting a pump ............................................................ 24
3 Switching the instrument on and off and selecting the dia-
log language 25
3.1 Switching the instrument on and off ................................ 25
3.2 Selecting the dialog language ........................................... 27
4 Fundamentals of operation 28
4.1 Touch-sensitive screen ....................................................... 28
4.2 Display elements and controls .......................................... 28
4.3 Status display ...................................................................... 30
4.4 Entering text and numbers ................................................ 31
5 Setup and configuration 33
5.1 Preparing instruments and material ................................. 33
5.2 Configuring reagent data .................................................. 33
5.3 Configuring a printer .......................................................... 34
6 Carrying out the water content determination of a sam-
ple 36
6.1 Creating a titration method ............................................... 36

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭
6.2 Carrying out the water content determination ............... 40
7 Performing titration with supplementary functions 45
7.1 Saving the determination and the PC/LIMS report ......... 45
7.2 Modifying the titration parameters .................................. 47
7.3 Creating a sample table ..................................................... 48
7.4 Carrying out titrations using the sample table ................ 51
8 Setting up the user administration 52
8.1 Creating a user list .............................................................. 52
8.2 Automatic login with USB flash drive ............................... 54
8.3 Login with password .......................................................... 56
Index 59

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures
￭￭￭￭￭￭￭￭ V
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 .................................................................... 8
Figure 6 Equipping the titration cell ................................................................. 9
Figure 7 Mounting the addition and aspiration tube ...................................... 11
Figure 8 Titration cell with aspiration apparatus ............................................ 13
Figure 9 Remote connection 885 Compact Oven SC – Remote Box – 917 Coul-
ometer ............................................................................................ 15
Figure 10 Unscrewing the protective cap from the generator electrode ........... 16
Figure 11 Screwing the electrode cable to the generator electrode ................. 16
Figure 12 Connecting a generator electrode ................................................... 17
Figure 13 Unscrewing the protective cap from the indicator electrode ............ 17
Figure 14 Screwing the electrode cable to the indicator electrode ................... 18
Figure 15 Connecting an indicator electrode ................................................... 18
Figure 16 Connecting the PVC tubings ............................................................ 24

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Structure of the tutorial
This tutorial describes the installation and the first steps with the 917
Coulometer. You will be guided step-by-step through the most important
dialog pages by using a water content determination with a water stan-
dard. In addition, you will find information regarding titrations with
extended functions and for user administration.
1.2 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).
1.3 Symbols and conventions
The following symbols and formatting may appear in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the sec-
ond to the instrument part in the figure.
Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
[Next] Button or key
WARNING
This symbol draws attention to a possible life-threat-
ening 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.

1.3 Symbols and conventions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭
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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation
￭￭￭￭￭￭￭￭ 3
2 Installation
2.1 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.
Operate the instrument only with the supply voltage specified for it. Use
the supplied power supply unit exclusively.
Figure 1 Connecting the power supply unit
Proceed as follows:
1Connect the plug of the external power supply unit with the power
socket of the Coulometer (see figure 1, page 3).

2.1 Setting up and connecting the instrument ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭
NOTICE
The plug of the power supply unit is protected against accidental
disconnection of the cable by means of a pull-out protection fea-
ture. If you wish to pull out the plug, you first need to pull back
the outer plug sleeve marked with arrows.
2Connect the power cord with the external power supply unit of the
Coulometer and with the power grid.
CAUTION
Switch off the Coulometer correctly by pressing the power switch
before you disconnect the electricity supply. If this is not done, then
there is a danger of data loss.
Connecting a balance
As a rule, balances are equipped with a serial RS-232 interface. To connect
a balance, you require a USB/RS-232 adapter (6.2148.050).
Figure 2 USB/RS-232 adapter
The USB/RS-232 adapter can be connected to the 917 Coulometer directly
or by means of a USB hub.
Connect the 9-pin plug of the respective balance connecting cable to the
RS-232 connector. Consult the manual for the balance to select the cor-
rect connecting cable.
The parameters for the RS-232 interface must match those on the instru-
ment and those on the balance. 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:

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation
￭￭￭￭￭￭￭￭ 5
Balance Cables
AND ER, FR, FX with RS-232 inter-
face (OP-03)
6.2125.020 + 6.2125.010
Mettler AB, AG, PR (LC-RS9) In the scope of delivery for the
balance
Mettler AM, PM, PE with interface
option 016
or
Mettler AJ, PJ with interface
option 018
6.2146.020 + 6.2125.010
Also from Mettler: ME 47473
adapter and either ME 42500
hand switch or ME 46278 foot
switch
Mettler AT 6.2146.020 + 6.2125.010
Also from Mettler: ME 42500
hand switch or ME 46278 foot
switch
Mettler AX, MX, UMX, PG, AB-S,
PB-S, XP, XS
6.2134.120
Mettler AE with interface option
011 or 012
6.2125.020 + 6.2125.010
Also from Mettler: ME 42500
hand switch or ME 46278 foot
switch
Ohaus Voyager, Explorer, Analyti-
cal Plus
Cable AS017-09 from Ohaus
Precisa balances with RS-232-C
interface
6.2125.080 + 6.2125.010
Sartorius MP8, MC, LA, Genius,
Cubis
6.2134.060
Shimadzu BX, BW 6.2125.080 + 6.2125.010
Connecting the barcode reader
The barcode reader is used as an aid for text and numerical input. You can
connect a barcode reader with USB interface.

2.1 Setting up and connecting the instrument ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
6￭￭￭￭￭￭￭￭
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.).
If several USB devices are to be connected, then it is recommended that a
USB hub (available from specialty stores) be used. The USB hub then func-
tions as a distributor to which several USB devices can be connected.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation
￭￭￭￭￭￭￭￭ 7
2.2 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:
1Attach the 6.2047.040 titration vessel holder to the magnetic stirrer.
2Insert the 6.1464.320 titration cell into the titration vessel holder.
2.2.2 Preparing the titration cell
Filling the adsorber tube
Before setting up the titration cell, the 6.1403.030 adsorber tube must be
filled with the 6.2811.000 molecular sieve. Proceed as follows:

2.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭
6.1403.030
6.2811.000
1
2
3
4
Figure 5 Filling the adsorber tube
1Insert a small cotton plug into the bottom of the adsorber tube. Do
not pack the cotton too tightly.
2Fill the adsorber tube to ¾ with molecular sieve granulate.
3Place a small cotton plug on the molecular sieve. Do not pack the
cotton too tightly.
4Seal the adsorber tube with the appropriate cover.
NOTICE
Note that the molecular sieve must be replaced at regular intervals.
Each time you refill the adsorber tube with the molecular sieve, you
can, for example, write the date directly on the adsorber tube.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation
￭￭￭￭￭￭￭￭ 9
Equipping the titration cell
6.1903.030
6.1464.320
6.2713.010
6.1437.000
6.0345.100
6.2713.020
6.1403.030
6.1448.020
6.2701.040
6.2713.000
6.0341.100
2
1
2
5
2
3
4
6
6.0344.100
Figure 6 Equipping the titration cell
Equip the titration cell as follows:
1Place the 6.1903.030 stirring bar in the titration cell.
2Cut 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.).
Please take care to ensure that the edges of the ground-joint sleeves
are cut to size cleanly and that there are no fringes. The ground-joint
sleeves must not protrude at the lower edge of the ground-joint
opening.
3Insert the 6.1403.030 adsorber tube into the generator electrode.

2.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭
4Insert 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.
5Insert the 6.0341.100 indicator electrode into the left ground-joint
opening.
6Place the 6.1448.020 septum on the front opening of the titration
cell and screw it shut with the 6.2701.040 screw cap.
Tighten the screw cap only enough so that sealing is ensured. The
septum must not bend.
Filling the titration cell (generator electrode without dia-
phragm)
Proceed as follows when using a generator electrode without a dia-
phragm:
1Fill approximately 100 mL of reagent into the titration cell with the
aid of the 6.2738.000 funnel.
2Close the remaining ground-joint opening on the right with the
6.1437.000 ground-joint stopper (with ground-joint sleeve attached).
Filling the titration cell (generator electrode with dia-
phragm)
Proceed as follows when using a generator electrode with a diaphragm:
1Fill approximately 5 mL of catholyte into the generator electrode.
2Fill approximately 100 mL of anolyte into the titration cell with the
aid of the 6.2738.000 funnel. The level of the anolyte should be
roughly 1 - 2 mm above the level of the catholyte.
3Close the remaining ground-joint opening on the right with the
6.1437.000 ground-joint stopper (with ground-joint sleeve attached).

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Installation
￭￭￭￭￭￭￭￭ 11
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:
1Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the 6.1437.000 stopper.
2Insert the stopper into the 6.1439.010 addition and aspiration tube.
3Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the addition and aspiration tube.
4Insert this assembly into the ground-joint opening.
5Connect the tubing for the reagent addition at the upper connector
of the addition and aspiration tube (5).
6Connect the tubing for the aspiration of the titration cell at the lower
connector of the addition and aspiration tube (6).
Details regarding how to connect the addition tubing and the aspiration
tubing can be found in the chapter "Setting up the aspiration und reagent
bottle" (see chapter 2.3, page 20).

2.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
12 ￭￭￭￭￭￭￭￭
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. For highly
viscous samples, a dosing unit with a 10 mL cylinder is more suitable.
Mounting the aspiration tip
2
6.1543.070
3
1
6.1446.060
6.2730.030
Insert the aspiration tip into the titration cell as follows:
1Screw the 6.2730.030 nipple with stopper and O-ring onto the
6.1446.060 stopper.
2Pull out the stopper.
3Slide the 6.1543.070 aspiration tip through the stopper.