Metrohm 832KF User Manual

CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com

832 KF Thermoprep

Instructions for Use

8.832.1023 10.2004/ dm

Teachware Metrohm AG Oberdorfstr. 68 CH-9101 Herisau teachware@metrohm.com

Although all the information given in these instructions has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please inform the author at the address given above.

II 832 KF Thermoprep

1 Introduction 1

1.1 Description of the instrument ..........................................................1

1.2 Information about these Instructions for Use.................................2

1.3 Parts and controls ............................................................................3

1.3.1 Individual parts and standard accessories ..............................................3

1.3.2 Rear view...................................................................................................4

1.3.3 Temperature controller..............................................................................5

1.3.4 Sample holder for standard vials ..............................................................5

2 Safety information 6

2.1 General..............................................................................................6

2.2 Electrical safety ................................................................................6

3 Installation 7

3.1 Instrument setup...............................................................................8

3.1.1 Packaging .................................................................................................8

3.1.2 Checks ......................................................................................................8

3.1.3 Location.....................................................................................................8

3.2 Mains connection .............................................................................8

3.3 Assembling the 832 KF Thermoprep............................................ 10

3.3.1 Assembling the needles..........................................................................10

3.3.2 Attaching the drying bottles ....................................................................11

3.3.3 Attaching the dust filter ...........................................................................11

3.4 Assembling the coulometric cell .................................................. 12

3.5 Assembling the titration vessel for volumetric KF titrators ........ 12

4 Operation 13

4.1 Inserting and removing sample vials ........................................... 13

4.2 Needle penetration ........................................................................ 13

4.3 The pump ....................................................................................... 14

4.4 The temperature controller ........................................................... 15

4.4.1 Two set temperatures .............................................................................15

4.4.2 Setting a temperature..............................................................................15

4.4.3 Self-optimization of the control parameters............................................16

4.4.4 Key lock function.....................................................................................16

4.5 Working procedure........................................................................ 17

4.5.1 Preparing the 832 KF Thermoprep/756/831 Coulometer system ..........18

4.5.2 Determination with blank value subtraction............................................18

4.5.3 Determination without blank value subtraction.......................................19

4.6 Practical information ..................................................................... 20

5 Maintenance information 21

6 GLP validation 21

832 KF Thermoprep III

7 Troubleshooting 22

7.1 Problems ........................................................................................ 22

8 Annex 23

8.1 Technical data................................................................................ 23

8.1.1 Oven........................................................................................................23

8.1.2 Air pump..................................................................................................23

8.1.3 Temperature controller............................................................................23

8.1.4 Power supply ..........................................................................................23

8.1.5 Safety specifications ...............................................................................23

8.1.6 Electromagnetic compatibility (EMC) .....................................................24

8.1.7 Ambient temperature ..............................................................................24

8.1.8 Dimensions and materials ......................................................................24

8.2 Standard equipment ...................................................................... 25

8.2.1 832 KF Thermoprep................................................................................25

8.3 Optional accessories..................................................................... 27

8.3.1 Sample vials............................................................................................27

8.4 Warranty and conformity............................................................... 28

8.4.1 Warranty ..................................................................................................28

8.4.2 EU Declaration of Conformity for 832 KF Thermoprep ..........................29

8.4.3 Declaration of Conformity .......................................................................30

Index 31

List of illustrations

Fig. 1 Front view ...................................................................................................................3

Fig. 2 Rear view ....................................................................................................................4

Fig. 3 Temperature controller ...............................................................................................5

Fig. 4 Sample holder .......................................................................................................... 5

Fig. 5: 832 KF Thermoprep – peripheral devices ..................................................................7

Fig. 6 Fuse holder.................................................................................................................9

Fig. 7 Needle assembly ...................................................................................................... 10

Fig. 8 Guide head with needles..........................................................................................10

Fig. 9 Coulometer cell......................................................................................................... 12

Fig. 10 Volumetric KF cell ..................................................................................................... 12

Fig. 11 Crimping pliers.......................................................................................................... 13

Fig. 12 Loosening the guide head........................................................................................13

Fig. 13 Needle in lowered position ....................................................................................... 14

IV 832 KF Thermoprep

1.1 Description of the instrument

1 Introduction

Thanks to its reliability and simple handling, the Metrohm 832 KF Thermoprep is a very versatile instrument. It has been designed for use in production and laboratories and covers a wide range of applications. The 832 KF Thermoprep can be used wherever it is necessary to heat up a solid or liquid sample and/or to drive off water by the application of heat. When combined with a coulometric or volumetric KF titrator, the 832 KF Thermoprep forms the ideal analytical system for determining the water content of samples which contain interfering components or which only release their moisture slowly. Among the decisive advantages of the KF Thermoprep is the reduction of sample preparation to a minimum. By using hermetically sealed sample vessels (headspace vials) the samples can be filled directly on site. The PTFE-coated septa guarantee a constant and true water content, even when the sample have been allowed to stand for a long time.

1.1 Description of the instrument

The 832 KF Thermoprep has been designed primarily for the determination of moisture by the oven method. The samples are heated in the oven block and release their moisture in the form of water vapor; this is transferred to a measuring cell by a carrier gas. The carrier gas stream is produced by a built-in air pump. An inlet valve is also provided for the use of nitrogen or other inert gases. The determination of moisture in the measuring cell can be carried out either coulometrically or volumetrically according to the Karl Fischer method. The 832 KF Thermoprep is characterized by its compact construction; the oven heating block, air pump, temperature controller, flowmeter and flow controller as well as the drying bottles are already built in.

832 KF Thermoprep, Introduction 1

1.2 Information about these Instructions for Use

Please read through these Instructions for Use before you start to use the 832 KF Thermoprep. The following notations and pictograms are used in these instructions:

Operating element

The operating elements are explained on pages 3ff.

Danger This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components by electricity.

Danger/Warning This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components.

Attention This symbol indicates important information. Read the information provided before you continue.

2 832 KF Thermoprep, Introduction

1.3 Parts and controls

1.3.1 Individual parts and standard accessories

Fig. 1 Front view

Guide head

Transfer tubing 6.1805.460

Spacer 4.832.4190

Penetration and outlet needle

6.2816.070 and 6.2816.080 Dosing tip 6.1543.060

Septum stopper 6.2730.050

Sample holder

Pump switch

Temperature selection switch

832 KF Thermoprep, Introduction 3

Temperature controller

Clamping lever

Guide rod

Inlet tubing 6.1805.020

Air/Nitrogen outlet

Drying bottles 6.1608.050

With 6.1602.140 inset, filled with

6.2811.000 molecular sieve

Bottle holder

Flow indicator

Flow controller

1.3 Parts and controls

1.3.2 Rear view

WARNING - Fire Hazard -

for conti nued pro tection replac e only with the same ty pe and rating of fuse

100 - 120 V: 4 A (T) 220 - 240 V: 2 A (T) f = 50/60 Hz S = 350 VA

Inlet filt er

Key lock

Off

Fig. 2 Rear view

Vorsicht: Heisse Gehäuseteile (üb er 60° C)

Attention: Hot parts (a bove 6 0°C)

Cuidado: Partes calientes (mas de 60°C)

Attention: Parties chaudes (p lus de 60°C)

Type 1.832.0010 Nr.

Made by Metrohm Switzerland

0010/01104

Tubing guide

Ventilation slots

Mains switch

Mains connection

Fuse holder

Adjustment nuts

Transfer tubing connection

Guide spring

Needle base

Hot air outlet

Key lock switch

Air/nitrogen outlet

Connection for dust filter (6.2724.010)

4 832 KF Thermoprep, Introduction

1.3 Parts and controls

1.3.3 Temperature controller

Actual value display

red, 4-place

Set value display

green, 4-place

Program key

for selecting the parameters

Decrement key

for changing values

Fig. 3 Temperature controller

Output status display

yellow, for outputs 1 to 3 (K1 and K3: oven heating, K2: fan)

LED for ramp/program function

green, lights if configured

EXIT key

to exit the dialog levels

Increment key

for changing values

1.3.4 Sample holder for standard vials

The dimensions of the 6.2063.000 sample holder are optimized for the Metrohm 6.2419.007 standard sample vials (6 mL). This ensures the highest possible heat flow from the oven to the sample. If other sample containers with different dimensions shall be used custom made sample holders can be delivered. For this the precise dimensions (incl. dimensional tolerances) must be known. The measures of non-standard sample containers must vary within the following dimensional limits:

Diameter 10.0 … 32.0 mm

Fig. 4 Sample holder

832 KF Thermoprep, Introduction 5

Depth of immersion 20.0 … 45.0 mm

2.1 General

2 Safety information

Warning! This instrument should only be used in accordance with the information given in these Instructions for Use.

2.1 General

This instrument left our works in perfect condition from the point of view of its operational safety (see Technical data, safety specification). To keep it in this condition and to continue to operate safely the following information must be carefully observed.

2.2 Electrical safety

Please observe the following guidelines:

• Only qualified Metrohm personnel should carry out service work on electronic components.

• Do not open the instrument housing as this could damage the instrument. The housing contains no components which could be serviced or exchanged by the user.

Electrical safety when handling the instrument is guaranteed within the scope of Standard IEC 61010. However, please observe the following point:

Protection against electrostatic charges

Warning! Electronic components are sensitive to electrostatic charges and can be destroyed by a discharge. Always remove the mains connection cable from socket 12 before making or breaking electrical connections on the rear panel of the instrument.

Connection to the electricity supply:

This instrument must only be operated at the specified mains voltage.

Repair and maintenance:

If faults or malfunctions occur while using the 832 KF Thermoprep we recommended that you first check that the connection to the control instrument has been made correctly.

The instrument must not be opened. This is reserved exclusively for authorized service personnel.

6 832 KF Thermoprep, Safety information

2.2 Electrical safety

3 Installation

This section describes the things you should pay attention to when unpacking and starting up the 832 KF Thermoprep. It also tells you how a complete automation system is built up. The following illustration provides an overview of the peripheral devices which can be used with an 832 KF Thermoprep:

800

Dosino

Titriermittel

835

835 Titrando

Titrando

836

836 Titrando

Titrando

Titrandos

USB

PC Control tiamo

KFKF

Touch ControlTouch Control

Fig. 5: 832 KF Thermoprep – peripheral devices

LPT 1

USB

PC Software

COM 1

COM 2

USB

RS232

Tinet 2.x / VESUV 3.0

832 TP832 TP

832 Thermoprep

RS232

756 KF756 KF

831 KF831 KF

KF Coulometer 831 / 756

Titrierm ittelTitrierm ittel

Titrierm ittel

KFD 758

KFP 785

KFP 795KFP 795

KF Titrino 795 / 787 / 758

832 KF Thermoprep, Installation 7

+ 25 hidden pages

Metrohm 832KF User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Table of contents

List of illustrations

1 Introduction

1.1 Description of the instrument

1.2 Information about these Instructions for Use

1.3 Parts and controls

1.3.1 Individual parts and standard accessories

1.3.2 Rear view

1.3.3 Temperature controller

1.3.4 Sample holder for standard vials

2 Safety information

2.1 General

2.2 Electrical safety

3 Installation