Digestion Unit K-424
Contents
1 Scope of delivery
2 Safety
2.1
Symbols
2.2
Requirements for the operator
2.3
Regulation use
2.4
Non-regulation use
2.5
General hazards
2.6
Safety measures
3 Function
3.1
Principle of operation
4 Putting into operation
4.1
Setup location
4.2.
Unpacking
4.3
Connection to the mains
4.4
Hose connections
5 Operation
5.1
Operating elements
5.2
Operating elements and their function
5.3
General information
5.4
Execution of the Kjeldahl disintegration
5.5
Malfunctions
6 Maintenance
6.1
General information
6.2
Upkeep
6.3
Gaskets
6.4
Replacing the insulation
6.5
Replacing the O-rings
6.6
Fuses
6.7
Customer service
Read these instructions thoroughly before you use the
Digestion Unit K-424 . Store these instructions in the immediate vicinity of the apparatus so that they may be consulted at any time.
The unit must only be connected to the mains and switched on after having completed all necessary preparations.
7 Taking out of operation
7.1
Storage/Transport
7.2
Disposal
Chapter 2 contains important safety information. Knowledge of this is imperative for the safe operation of the Digestion unit.
8
Subject to technical change without notice. No part of these instructions may be reproduced in any form whatsoever or processed, reproduced or disseminated by means of electronic or optical systems without the express written permission of Büchi Labortechnik AG. All rights reserved.
Copyright © Büchi Labortechnik AG 2008
Replacement parts
9 Appendix
9.1
Technical Data
9.2
Materials used
9.3
FCC requirements
9.4
Declaration of conformity
Contents
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15
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19 en, Version E
K-424 Operating instructions
Order No.
96711
1
1 Scope of delivery
Fig.1: Overview K-424
1 Scope of delivery
Digestion Unit K-424
Description
Versions:
K-424 standard
K-424 standard
Table 1: Versions
120 V
230 V
50 / 60 Hz
50 / 60 Hz
Enclosed parts:
4 Digestion tubes
1 Rack
1 Upper insulating plate
1 Suction module complete
1 Connection to suction module
1 Digestion tube holder complete
1 EPDM Hose 8mm
1 Mains cables:
Type CH
Type Schuko
Type GB
Type AUS
Type USA
1 Operating instructions in one of the following languages
German
English
French
Italian
Spanish
1 Packaging
Table 2: Enclosed parts
Accessories:
Water jet pump plastic
Glass cap
Gasket PTFE to suction tube
Collection tube for suction tube
Condensation bottle complete
Suction module for H
2
O
2
digestion
Büchi B-414 Scrubber
Suction pipe with condensation gutter
Non Kjeldahl digestion set
Suction pipe with ball joint
Table 3: Accessories
Order No.
37963
37962
37377
26730
26736
26842
26875
38080
26275
10021
10029
17833
17834
33756
96710
96711
96712
96713
96714
26799
02913
17396
22442
27737
25100
37399
37876
26880
43677
40158
2
Digestion Unit K-424 2 Safety
2 Safety
The apparatus has been built in accordance with state-ofthe art technology and recognized safety regulations.
Nonetheless risks and dangers can arise from the apparatus:
• If the apparatus is operated by insufficiently trained personnel.
• If the apparatus is not used as directed.
2.1
Symbols
Stop
Information on dangers which can lead to serious damage to property, to severe or life-threatening injuries.
Warning
Information on dangers which can lead to damage to health or property.
Please note
Information on technical requirements. Noncompliance can lead to faults, inefficiency and production losses.
2.2
Requirements for the operator
The unit is only to be used by laboratory and specialist personnel and other persons, who, because of their training or professional experience, are able to assess the dangers which can result while operating the equipment.
2.3
Regulation use
The unit is conceived and built as a piece of laboratory equipment. Its regulation use is the heating of concentrated sulfuric acid used in the oxidation of organic samples.
2.4
Non-regulation use
Any other use than listed as well as any use which does not correspond to the technical data is a misuse. The operator bears sole risk for eventual damage related to such use.
In particular the following uses are not allowed:
• operation in explosion-prone areas
• operation with samples that can explode or ignite due to impact, friction, heat or sparking.
3
2 Safety Digestion Unit K-424
2.5
General hazards
General hazards arise from:
• Hot sulfuric acid
• Combustible gases or vapors in the immediate vicinity of the apparatus
• Damaged glassware
• Location of the apparatus to close to the wall (see section 4.1 Set up location)
• Hot surfaces
Except for authorized repair personnel it is forbidden to remove covers using commercially available tools.
The device must not be put into operation with damaged glass parts.
Contact with electrically live parts presents a danger to life and limb!
2.6
Safety measures
It is recommended that the apparatus be operated exclusively under an exhaust hood.
The wearing of personal safety equipment such as safety glasses , gloves and lllll aboratory coats is necessary.
As a necessary part of the digestion unit K-424, this instruction manual must at all times be available to the operating personnel at the location where the apparatus is being used. This also applies to the further editions in other languages which may be ordered seperately.
Modifications
Any modifications on the apparatus itself or on replacement or accessory parts, and any use of replacement or accessory parts other than those listed in these operating instructions is permissible only with the express written approval of Büchi Labortechnik AG.
Responsibilities of the operator
The operator is responsible for providing proper instruction for his staff. For that purpose, these operating instructions may also be ordered in other languages.
The operator must inform the manufacturer immediately of any and all events relevant to product safety that arise during his operation of the apparatus.
If assuming that a safe operation is not possible any more the unit must be put out of operation and secured against unintended further operation.
4
Digestion Unit K-424 2 Safety
It is to be assumed that a safe operation is not possible any more s if the unit is visibly damaged, s If the unit is not functioning any more s after long storage under anfavourable conditions, s after being transported under difficult conditions.
The unit must not be operated with combustible substances.
If you need the assistance of Büchi Service, it is required to indicate and declare eventually remaining dangerous substances (e.g., as defined in EC guidelines L 360, 1976/
79 or VBG 16) in or on the apparatus for reason of on-thejob safety or pollution control.
5
3 Function Digestion Unit K-424
3 Function
The digestion unit K-424 is suitable for digestions involving concentrated boiling sulfuric acid at a temperature of approximately 370° C.
3.1 Principle of operation
Sample tubes
Heating
Suction module
Hose to water jet pump or to Scrubber B-414.
Fig. 2: Principle of operation K-424
6
Digestion Unit K-424 4 Putting into operation
4 Putting into operation
4.1
Setup location
The digestion unit must be installed on a stable, clean and flat base.
For reasons of safety, a gap of at least 30 cm must be left open between the back of the machine and the wall or other objects. Never place any containers, chemical products or other equipment behind the digestion unit.
4.2
Unpacking
The original package must be kept for possible later transport.
If the package has been damaged, check the machine carefully for broken glass or damage to the housing.
Make certain that the socket voltage is the same as that shown on the machine nameplate. Always connect the machine to an earthed (grounded) socket. This avoids risks due to an internal defect.
4.3
Connection to the mains
Before switching on the K-424 for the first time check that the voltage on the socket corrsponds to the voltage indicated on the apparatus identification plate.
Always connect the apparatus to a grounded (earthed) socket.
External couplings and extension cords must contain a protective conductor ( 3-pole couplings, cables, and plugin devices). Any and all interruptions in the protective conductor are forbidden. This avoids risks due to an internal defect.
7
4 Putting into operation
Scrubber E
D
B
Digestion Unit K-424
C
4.4
Hose connections
Mount the safety shield (A) with the fitted hoses on the unit
(see photograph).
Assemble the connection to the suction module (B) and install on the hose (C) and on the suction modules (D).
Connect the EPDM hose to the scrubber B-414 or to the water jet pump (e.g. made from plastic) Art. No. 02913.
Fig. 3: Hose connections enlarged section
026757
A
B
002073
When working with a water jet pump unpleasant odours may escape into the environment if the suction is not powerful enough.
026240 003577
Fig. 4: Connection to fume exhaust
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Digestion Unit K-424 5 Operation
5 Operation
5.1
Operating elements
Main switch
Energy regulator
Heater pilot lamp
Mains connector
Fig. 5: Arrangement of the control and display elements front
5.2
Operating elements and their function
Main switch
Switching the apparatus ON/OFF. In case of an mains load over 12 A a bimetal switch cuts the circuit causing the mains switch switching to OFF.
After switch back to ON the apparatus is ready to operate again.
Energy regulator
Regulates the heating in stages from 1 -10.
Fig. 6: Arrangement of the control and display elements rear
Fig. 7: Condensation zone of the sulfuric acid
5.3
General information
The heating process heats the digestion tubes uniformly from the side, leading to good boiling behaviour (no retardation of boiling). Boiling chips are used only when larger quantities of water (>10 ml) are evaporated (no glass beads used).
It is important that the condensation zone of the sulfuric acid does not rise too high ( maximum 5 cm under the glass rim).
For the digestion of approx. 1 g of organic material, normally
18 - 20 ml H
2
SO
4
are used.
For each additional gramm of organic material an addition of 3 - 5 ml (by fat or mineral-oil 5 - 10 ml) H
2
SO
4
has to be used.
9
Fig. 9: K-424
10
5 Operation
Fig. 8: Gaskets
Digestion Unit K-424
This apparatus is used for procedures that require the use of heat and hazardous sulphuric acid. Wear goggles and protective clothing and exercises extreme caution when working in this area.
Seal off unused connecting branches with the glass cap
(item n o 17396)
It is essential, that the gaskets are fitted correctly on the suction tube and are leaned symmetrical on the glass!
Regulation of the heating power depends on a variety of factors such as the quantity to be digested, the types of reagents, etc.
To carry out the digestion in the minimum time, the samples are digested at full power.
The digestion time depends on the material to be digested and must be determined by experiment. (Continue boiling for about 15 minutes after the solution has become clear.)
After the sample has cooled, the digestion tube can be connected direct to a Büchi Distillation Unit for carrying out the distillation.
If a digested sample takes a relatively long time to cool, it may solidify. Before it is distilled, the sample must be liquefied again:
by the careful addition of a small quantity of distilled water, or
by gentle heating in the Digestion Unit.
Digestion Unit K-424 5 Operation
Fig. 10: Operation of the K-424
5.4
Carrying out the Kjeldahl digestion
• Switch the unit on and preheat for approx. 5 minutes on stage 10.
• Wear protective goggles!
• Place the digestion tubes in the digestion tube holder on the rack .
• Introduce the sample and reagents into the digestion tubes .
• Seal off unused connecting branches with the glass cap (item No. 17396) .
Never install empty digestion tubes!
• Place the suction module with the fitted gaskets on the digestion tube holder.
• Turn on scrubber or water jet pump bevor any gases can develop.
Malfunction
Heating elements do not heat up
Lamp does not light up (H 1)
Table 4: Malfunctions
5.5
Malfunctions
Possible cause
1. Mains plug not plugged in
2. Unit switched OFF
3. Energy regulator in position „0“
4. Energy regulator faulty
5. Heating elements faulty
Lamp faulty
Remedy
- Connect unit to the mains
- Switch ON
- Set to position "10"
- Replace regulator
- Replace heating element
Replace lamp
11
5 Maintenance Digestion Unit K-424
6 Maintenance
6.1
General information
The housing of the digestion unit K-424 ist made of metal and is coated with an acid-resistant material.
In order to avoid damage to this synthetic coating, any drops of acid which might fall on it should be wiped off with a damp cloth.
Absolutely avoid any scratching of the surface whatsoever.
6.2
Upkeep daily:
• Check glass parts for damage
• Clean the plastic parts with a damp cloth.
The glass parts are cleaned.
6.3
Gaskets
The gaskets are subject to wear and must be replaced when damaged or at loss of closeness.
Inspection and maintenance duty
All specifications and regulations aimed at maintaining the digestion unit K-424 in a proper working condition must be followed.
This includes periodic cleaning and checking for damage.
After any repair work the operator must check the proper function bevor putting back into operation.
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Digestion Unit K-424
Fig. 11: Replacing the O-rings
➬
2
➬
1
6 Maintenance
6.4
Replacing the insulation
To avoid contact with live parts, components may only be replaced when the apparatus has been isolated from all supply points.
Electrical and electronic components are to be replaced by skilled engineers.
No components may be replaced when the apparatus is warm or hot. Allow the apparatus to cool down!
Replacing upper insulating plate
This insulation is freely accessible and can be replaced without tool.
6.5
Replacing the O-rings
• Cut damaged O-ring with a knive or a scalpel
• Remove tube holder
• Fit new O-ring over the suction module (see Fig. 11)
• Insert tube holder and fix with O-ring.
13
6 Maintenance
Figure 12: Device plug, inserted
Digestion Unit K-424
6.6
Main fuses
Please change the main fuses as follows:
• Pull out mains cables
• Pull out fuse holders
• Replace the defective mains fuse by a new one with same performance :
- 230V: T 5A L250V
- 120V: T10A L250V
• Insert again fuse holders
6.7
Customer service
Any intervention on or in the apparatus may only be carried out by authorized service technicians. These are persons with a sound technical training and knowledge of the dangers which result from not observing safety regulations. Authorized
Büchi serve centers have available to them a special service manual for this apparatus. That manual can only be obtained by authorized personnel.
The addresses of the official Büchi service centers are shown on the last cover page of these operating instructions. Please contact these service centers whenever you have a malfunction, technical questions, or problems in using the equipment.
Büchi’s customer service is prepared to offer the following services:
14
Digestion Unit K-424 7 Taking out of operation
7 Taking out of operation
In order to avoid the risk of endangering people with hazardous substances the unit must be emptied and cleaned thoroughly before taking out of operation.
7.1
Storage/Transport
The unit has to be stored and transported cleaned and its original packaging.
7.2
Disposal
To ensure as ecologically sound a disposal of the apparatus as possible, the Appendix in Chap. 9 contains a list of the materials used in its most important parts.
This makes it possible for you to separate the parts and to send them on for recycling.
For disposal of electronic parts, we refer you to official regulations governing such action. In addition, all pertinent regional and local laws must be observed.
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8 Replacement parts
8 Replacement parts
Digestion Unit K-424
Only original Büchi accessories and replacement parts guarantee safe use and reliable operation of the apparatus. The use of other than Büchi replacement parts and accessories is only allowed with the permission of the manufacturer. Replacement parts may be used only for purposes of assembly and disassembly in connection with Chapter 6, Maintenance. Their production using this manual is forbidden.
8.1
Replacement parts
No.Description
Connection to suction pipe, complete
Seals Viton Standard (6 seals)
Seal PTFE (1 seal)
O-Ring
Suction pipe
Glass holder set for suction pipe, including 2 O-rings (26785)
Upper insulation plate
Contact guard
Digestion glass holder, complete
Cap for digestion glass holder
Order code
26875
38122
22442
26785
26755
26877
26736
26797
38080
26791
Flat spring (12 springs)
Plug cap
Digestion glasses (4 glasses)
Rack
EPDM hose 8 mm
Fuses T10A L250V (10 pcs)
Fuses T5A L250V (10 pcs)
Suction pipe with ball joint
Suction module for H
2
O
2
digestion
Rubber gukos for H
2
O
2 suction module
Funnel with frit for H
2
O
2 suction module
Table 5: Replacement parts
38123
17396
37377
26730
26275
16952
33703
40158
37399
44495
44494
16
Digestion Unit K-424 9 Appendix
9 Appendix
Dimensions (Width x Heigth x Depth)
Nominal voltage
Connected load
Power consumption
Weight (net)
Ambient conditions
Overvoltage category
Pollution degree
Table 6: Technical data
Part
Housing front and rear panels side panels
Glass parts
Safety shield
Insulation
Metals
Hoses
Table 7: Materials used
9.1
Technical data
275 x 600 x 570 mm
230 V ± 10%, 50/60 Hz
120 V ± 10%, 50/60 Hz
1100 W
5 A approx. 13,5 kg for indoor use only, below 2000 m.s.l.
maximum relativ humidity 80% for temperatures up to 30°C, temperature 10 - 40°
II
2
9.2
Materials used
Material
Polyurethane
Stainless steel / Perfluoralkoxy
Borosilicate glass 3.3
Polyphenylensulfrole
Saprolan 85K / Porextherm WDS Ultra
Stainless steel
Ethylene propylene diene monomer rubber
Material code
PUR
1.4435 / PFA
DIN/ISO 3585
PPS
EPDM
17
9 Appendix Digestion Unit K-424
9.3
FCC requirements (for USA and Canada)
English:
This equipment has been tested and found to comply with the limits for a Class A digital device, pusuant to both Part
15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.
This equipment generates, uses and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is like to cause harmful interference in which case the user will be required to correct the interference at his own expense.
Français:
Cet appareil a été testé et s'est avéré conforme aux limites prévues pour les appareils numériques de classe A et à la partie 15 des règlementation FCC à la règlementation des radio-interférences du Canadian Department of communications. Ces limites sont destinées à fournir une protection odéquate contre les interférences nétastes lorsque l'appareil est utilisé dans un environnement commercial.
Cet appareil génère, utilise et peut radier une énergie à fréquence radioélectrique, il est en outre susceprible d'engendrer des interferences avec les communications radio, s'il n'est pas installé et utilisé conformément aux instructions du mode d'emploi. L'utilisation de cet appareil dans les zones résidentielles peut causer des interférences nèfastes, auquel cas l'exploitant sera amené à prendre les dispositions utiles pour polier aux interférences à ses propres frais.
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Digestion Unit K-424
9.4
Declaration of confomity
9 Appendix
19
BÜCHI Labortechnik AG
CH-9230 Flawil 1 / Switzerland
T +41 71 394 63 63
F +41 71 394 65 65
www.buchi.com Quality in your hands
