Buchi K-355 Operation Manual
Buchi K-355, the high-performance distillation unit, offers precise and efficient distillation, making it an ideal choice for various laboratory applications. With its user-friendly interface and comprehensive safety features, the K-355 ensures a safe and reliable operation. From simple distillations to complex fractionations, this versatile unit handles a wide range of solvents and sample volumes, delivering accurate and reproducible results.
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Operation Manual
Distillation Unit
K� 355
93036 en
Table of contents
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.1 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.4 Warning notices used in this manual . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5.1 Instrument-related hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5.2 Other hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.5.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.5.4 Safety elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3.1.2 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.1.3 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.2 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.1 Instrument overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.2 Function principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
4.3 Controls of the instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
5.3 Reagent and water connections. . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.3.1 Cooling water connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.3.2 Drainage of cooling water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.3.3 Storage tank connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can be consulted at any time.
No technical modifications may be made to the instrument without the prior written agreement of
Buchi. Unauthorized modifications may affect the system safety or result in accidents.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without prior written agreement is also prohibited.
If you need another language version of this manual, you can download it at www .buchi .com .
3 K-355 Operation Manual, Version G
Table of contents
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.1 Addition of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.1.1 Manual dosage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.1.2 Automatic dosage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.1.3 General information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.2 Setting the distillation time. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.3 Setting the steam power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.4 Program storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.4.1 Storing a program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.4.2 Selecting a stored program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.5 Steam generator status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
6.5.1 Heating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
6.5.2 Standby mode (after 30 minutes) . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
6.6 Switching ON/OFF checklist. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
6.7 Carrying out a distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
7.1 Daily maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
7.1.1 Cleaning the instrument from inside . . . . . . . . . . . . . . . . . . . . . . . . . . 26
7.1.2 Cleaning the housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
7.1.3 Cleaning the glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
7.1.4 Preparing the instrument for a standstill overnight . . . . . . . . . . . . . . . . . . . 27
7.2 Weekly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
7.2.1 Cleaning the splash protector and the rubber bung seal. . . . . . . . . . . . . . . . 27
7.3 Monthly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
7.3.1 Checking the distillate amount. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
7.4 Half-yearly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
7.4.1 Replacing the NaOH tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
7.5 Yearly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
7.5.1 Replacing the rubber bung seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
7.5.2 Replacing the NaOH pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
7.6 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
8.1 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 30
9.1 Preparing the instrument for transport . . . . . . . . . . . . . . . . . . . . . . . . . 30
9.2 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
9.3 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
10 Spare parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
10.1 Spare parts K-355 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
10.2 Hosing connection scheme . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
11 Declarations and requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 34
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
4 K-355 Operation Manual, Version G
1 About this manual
1 About this manual
This manual describes the Distillation Unit K-355 and provides all information required for its safe operation and to maintain it in good working order.
It is addressed to laboratory personnel in particular.
NOTE
The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in chapter 2.
1 .1 Abbreviations
EPDM: Ethylene Propylene Dimonomer
FEP: Fluorinated Ethylene Propylene
FPM: Fluoroelastomer
PP: Polypropylene
PTFE: Polytetrafluoroethylene
RSD: Relative Standard Deviation
5 K-355 Operation Manual, Version G
2 Safety
2 Safety
This chapter points out the safety concept of the instrument and contains general rules of behavior and warnings from hazards concerning the use of the product.
The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual chapters are strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein.
2 .1 User qualification
The instrument may only be used by laboratory personnel and other persons who on account of training or professional experience have an overview of the dangers which can develop when operating the instrument.
Personnel without this training or persons who are currently being trained require careful instruction.
The present Operation Manual serves as the basis for this.
2 .2 Proper use
The instrument has been designed and built for laboratories. It serves for the distillation of steam-volatile substances.
2 .3 Improper use
Applications not mentioned above are improper. Also, applications which do not comply with the technical data are considered improper.
The operator bears the sole risk for any damages caused by such improper use.
The following uses are expressly forbidden:
•
•
Use of the instrument in rooms which require ex-protected instruments.
Use on samples, which can explode or inflame (e.g. explosives, etc.) due to shock, friction, heat or spark formation.
6 K-355 Operation Manual, Version G
2 Safety
2 .4 Warning notices used in this manual
WARNING
Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life if the instructions are not followed.
WARNING
Hot surface.
WARNING
Electrical hazard.
WARNING
Caustic substances.
ATTENTION
With the general „Read this” symbol, ATTENTIONs indicate the possibility of equipment damage, malfunctions or incorrect process results, if instructions are not followed.
NOTE
Useful tips for the easy operation of the instrument.
2 .5 Product safety
2 .5 .1
The instrument is designed and built in accordance with state-of-the-art technology. Nevertheless, risks to users, property, and the environment can arise when the instrument is used carelessly or improperly.
The manufacturer has determined residual dangers emanating from the instrument
•
• if the instrument is operated by insufficiently trained personnel.
if the instrument is not operated according to its proper use.
Appropriate warnings in this manual serve to make the user alert to these residual dangers.
Instrument-related hazards
Pay attention to the following safety notices:
WARNING
Potential implosion risk if used with damaged glassware.
• Beware of damaged or cracked glass parts.
WARNING
Potentially hot surfaces during operation (surfare temperatures at times exceed 60 °C) and hot steam passing off the waste outlet.
• Always be aware of the risk of being burned.
WARNING
Potentially lethal voltage inside the instrument.
•
•
Do not remove covers and other parts protecting from electricity.
Always keep the areas of electric parts, such as power supply plug, mains switch, etc. dry.
7 K-355 Operation Manual, Version G
2 Safety
2 .5 .2
2 .5 .3
Other hazards
WARNING
Certain solvents in or in the vicinity of the instrument can form peroxides and/or are highly inflammable.
•
•
Always be aware of the explosion risk when working with hazardous substances or with substances of unknown composition.
Always provide a good ventilation within or in the vicinity of the system.
Safety measures
WARNING
Sodium hydroxide, acids and lye are used for applications according to Kjeldahl. For this reason, protective goggles must be worn at all times when using the instrument or working in its immediate proximity.
2 .5 .4 Safety elements
The instrument is provided with the following safety elements:
•
•
•
•
•
Protective door: Safety appliance to protect users from burns at the splash protector (distillation area), which is hot during distillation.
Protective door sensor: Prevents the start of a distillation with the protective door open and stops a running distillation and the dosing of reagents immediately when the protective door is opened during the process.
Sample tube sensor: Prevents the start of a distillation without a sample tube inserted.
Protective shield (cover) at condenser: Protection of glass parts.
Service door sensor/switch: Electrical power is disconnected immediately when the service door is opened, thus preventing electrical shock during maintenance.
8 K-355 Operation Manual, Version G
2 Safety
2 .6 General safety rules
Responsibility of the operator
The head of laboratory is responsible for training his personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed.
Duty of maintenance and care
The operator is responsible for ensuring that the instrument is operated in proper condition only, and that maintenance, service, and repair jobs are performed with care and on schedule, and by authorized personnel only.
Spare parts to be used
Use only genuine consumables and genuine spare parts for maintenance to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
Modifications
Modifications to the instrument are only permitted after prior consultation with and with the written approval of the manufacturer. Modifications and upgrades shall only be carried out by an authorized
Buchi technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.
9 K-355 Operation Manual, Version G
3 Technical data
3 Technical data
This chapter introduces the reader to the instrument specifications. It contains the scope of delivery, technical data, requirements and performance data.
3 .1 Scope of delivery
Check the scope of delivery according to the order number.
NOTE
For detailed information on the listed products see www.buchi.com or contact your local dealer.
3 .1 .1 Standard instrument
Table 3-1: Standard instrument
Product
Distillation Unit K-355 Standard with glass splash protector, 230 V, 50/60 Hz
Distillation Unit K-355 with splash protector made of fiber glass reinforced polypropylene, 230 V, 50/60 Hz
Distillation Unit K-355 Standard with glass splash protector and SO
2 nation kit
determi-
Order number
43505
43419
43070
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3 Technical data
3 .1 .2 Standard accessories
11
3
1 2
10
4
9
5
8
7
6
Table 3-2: Standard accessories
Product a 1 mains cable of the following types
Type CH
Type Schuko
Type GB
Type AUS
Type USA
Type Japan b 1 pair of glass tongs c 1 hose cooling water drain, silicone,
L = 1.8 m, Ø 10/14 mm d 1 hose chemical supply, solaflex,
L = 3.5, Ø 10/5 mm e 1 hose tygon, L = 530 mm f 3 suction tubes to tanks, FEP,
L = 580 mm g 1 hose connector PP h 1 Y hose coupling i 2 clamps Ø 7.6
i 6 clamps Ø 11.9
j 1 hose viton (acid resistant) L = 2 m k 1 cooling water hose complete: G ¾",
½", L = 1.5 m l 3 tanks 10 l, without caps m 1 cap for 10 l tanks, large n 3 tank labels o 1 cap for 10 l and 20 l tanks, small
Order number
43555
43029
43407
43565
11043
43571
43841
20344
37780
43410
25869
43434
43477
10010
10016
17835
17836
33763
10016
02004
43439
12
13
14
15
11 K-355 Operation Manual, Version G
3 .1 .3 Optional accessories
1 2 3
3 Technical data
Table 3-3: Optional accessories K-355
Product a 1 sample tube 500 ml
4 sample tubes 500 ml b 4 sample tubes 300 ml c Condenser cover, complete
Order number
26128
43982
37377
43484 d 20 l tank for chemicals e 10 l tank for chemicals
43469
43468
4
5
6
8
7 f Holder for 4 sample tubes, 500 ml g Holder for 6 sample tubes, 300 ml
16951
43039 h Holder for 12 sample tubes, 300 ml 43041
12 K-355 Operation Manual, Version G
13
3 Technical data
Table 3-3: Optional accessories K-355 (cont.)
Product Order number
Splash protector for Devarda method
K-350/K-355/K-360/K-370
43335
Constricted distillate outlet tube Ø 5 mm 43096
Sample tubes graduated, 300 ml, set of 4 43049
K-355 Operation Manual, Version G
3 Technical data
Table 3-3: Optional accessories K-355 (cont.)
Product Order number
Universal adapter for K-350, K-355,
K-360, K-370
43115
SO
2
accessory 48680
14 K-355 Operation Manual, Version G
3 Technical data
3 .2 Technical data
Table 3-4: Technical data K-355
Power consumption
Connection voltage
Frequency
Current consumption (230 V)
Mains connection
Recovery rate
Reproducibility (RSD)
Detection limit
Environmental conditions
Temperature
Altitude
Humidity
Installation category
Pollution degree
Dimensions (W x H x D)
Weight
3 .3 Materials used
Table 3-5: Materials used for the K-355
Component Material designation
Housing
Glass parts
Steam generator isolation
Steam generator housing
Protective door
Condenser cover
Connecting stopper
NaOH tube
Polyurethane
Borosilicate glass 3.3
Ceramic fiber
Stainless steel
Polymethyl methacrylate
Polymethyl methacrylate
Hypalon
Ethylene Propylene Dimonomer
Distillation Unit K-355 max. 2.2 kW
230 V ± 10% / 200 V ± 10%
50/60 Hz
II
2
8.5 A
3-pole (P, N, E) via power cord
≥ 99.5%
≤ 1%
≥ 0.1 mg Nitrogen for indoor use only
5 - 35 °C up to 2000 m maximum relative humidity 80% for temperatures up to
31 °C decreasing linearly to 67% relative humidity at
35 °C
400 x 660 x 360 mm
17 kg
Material code
PUR / UL V0
DIN/ISO 3585
Multitherm 550
1.4301
PMMA
PMMA
CSM
EPDM
15 K-355 Operation Manual, Version G
4 Description of function
4 Description of function
This chapter explains the basic principle of the instrument, shows how it is structured and gives a functional description of the assemblies.
4 .1 Instrument overview
3
2 a Splash protector b Sample tube c Protective door
Fig. 4.1: Instrument overview
16
1
4
5
6 d Condenser e Operating panel f Service door
K-355 Operation Manual, Version G
4 Description of function
4 .2 Function principle
The Distillation Unit K-355 is suitable for determining nitrogen using the Kjeldahl (TKN; Total Kjeldahl
Nitrogen) and Devarda methods as well as for other distillations of steam-volatile substances (e.g. of alcohol, SO
2
, volatile acids).
a Sample tube b Splash protector c Condenser d Distillate outlet tube e Receiving vessel with receiver solution
3
2
4
1
5
Fig. 4.2: Function principle
Steam is introduced into the sample solution (in sample tube a ) to drive out volatile components
(such as ammonia, alcohol, etc.). After condensation (in condenser c ) the condensate is collected in a receiver solution (in receiving vessel e ).
17 K-355 Operation Manual, Version G
4 Description of function
4 .3 Controls of the instrument
1
2
3
4
5
7
6
8
9
9 a STOP: Stops a distillation or the addition of reagent b TIME display c STEAM power display d START: Starts a distillation e TIME: Sets time in min:sec f UP: Increases time and steam up g STEAM: Sets steam power h DOWN: Decreases time and steam down i REAGENT: Button that adds reagent (e.g. water, sodium hydroxide solution)
Fig. 4.3: Controls of the instrument
18 K-355 Operation Manual, Version G
5 Putting into operation
5 Putting into operation
This chapter describes how the instrument is installed and gives instructions on initial startup.
NOTE
Inspect the instrument for damages during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company or transportation company.
Keep the original packaging for future transportation.
5 .1 Installation site
Install the instrument on a clean, flat and stable base and place the tank for Reagent 1 (acid) below instrument level (not more than 1 m). Place the other tanks on the same level as the instrument (not higher and not more than 1 m lower).
ATTENTION
To ensure the instrument safety do not place any object on top of it.
ATTENTION
For safety reasons, make sure that the distance between the instrument and another object or a wall is at least 30 cm.
ATTENTION
For safety reasons do not place any containers, chemicals or other instruments behind the instrument.
5 .2 Electrical connections
Fig. 5.1: Electrical connections
ATTENTION
Make sure that the voltage on the socket corresponds to the voltage given on the type plate of the instrument.
Always connect the instrument to an earthed socket. External connections and extension cables must be provided with an earthed conductor lead (3-pole couplings, cable or plug equipment) as the mains lead has a molded plug, thus avoiding risks due to inadvertent defective wiring.
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5 Putting into operation
The instrument cable must be well attainable at all times.
Make sure that no electric sparks form in the instrument or its surroundings as they might damage the instrument.
5 .3 Reagent and water connections
a a H
2
O inlet (for steam generator) from tank b Reagent 1 inlet (water or acid) c Reagent 2 inlet (NaOH) d Cooling water inlet e Cooling water outlet f Drain to waste b c d e f
5 .3 .1
5 .3 .2
Fig. 5.2: Reagent and water connections
All pumps are self-priming, no overpressure is necessary at the tanks.
Cooling water connection
Secure the cooling water hose with a hose clamp on both the instrument and the water connection side. The water pressure should be at a maximum of 4 bar. The built in valve reduces the water flow to
1.2 liters per minute.
The flanged screw coupling for the water connection has a standard screw thread of G ¾ ”.
Drainage of cooling water
Place the drain hose for the cooling water directly into the drain. For this purpose, shorten the silicone hose to the optimal length. The drain hose should not show any kinks, sharp bends and/or siphoning effect. Prevent flooding inside and outside the instrument by securing the drain hose.
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5 Putting into operation
5 .3 .3 Storage tank connection
To connect the storage tanks, proceed as follows:
•
•
•
Cut the solaflex tube into pieces of the appropriate length (use an acid resistant tube, if acid is dosed).
Insert a PTFE suction tube into the solaflex tube.
•
•
Push an EPDM sealing ring over the solaflex tube.
Now fasten the tubes to the tank with the red screw cover.
Connect the tubes at the appropriate connections at the instrument side and secure them with the clamps.
The “H
2
O” storage tank may be used to feed both the steam generator pump as well as the sample tube pump. For this purpose the Y hose coupling can be used.
Fig. 5.3: Tank connection
All pumps are self-priming, no overpressure is necessary at the tanks.
ATTENTION
To ensure proper system functioning, consider the following:
•
•
Use only distilled water for the H
2
O storage tank to keep the steam generator maintenance-free.
Make sure that the tanks are connected correctly. If the wrong tank (e. g. reagent tank containing
NaOH) is connected to the pump labelled „H
2
O steam“, the steam generator will be damaged.
21 K-355 Operation Manual, Version G
6 Operation
6 Operation
This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely.
WARNING
Risk of injury.
• Never operate the instrument when glassware is damaged.
WARNING
Sodium hydroxide, acid and lye are used for applications according to Kjeldahl. For this reason, protective goggles must be worn at all times when using this instrument or working in its immediate proximity.
NOTE
Close unused connections with plug caps.
If the connection for reagent 1 (pump) is used for the addition of strong acids (e.g. HCl), rinse the pump with distilled water at the end of the day.
6 .1 Addition of chemicals
6 .1 .1
6 .1 .2
6 .1 .3
Manual dosage
When pressing “REAGENT 1” or “REAGENT 2” the connected reagent is dosed as long as the switch is pressed.
Automatic dosage
The reagent volume dosed before the distillation is started is stored (e.g. in one of the nine different programs or as default value). This volume can be recalled after distillation (or a program containing the required volume can be recalled).
The stored volume is dosed by pressing “REAGENT” shortly. After releasing the switch, the volume is dosed automatically.
General information
The reagent switch is also active when the instrument is “Ready” or “Busy” (during distillation), so that additional dosage of reagent is possible during distillation.
During preheating, reagent addition is not possible.
The reagent volume stored before the start of the distillation is defined as the pump operating time.
The stored pump operating time (reagent volume) can be recalled after the distillation or after pressing
“STOP”.
If “STOP” is pressed during the automatic addition of reagent, the default volume is set to 0 ml.
The pumps for addition of Reagent 1 and Reagent 2 are different. Therefore different settings for the two pumps may be necessary.
22 K-355 Operation Manual, Version G
6 Operation
6 .2 Setting the distillation time
To set the distillation time, proceed as follows:
•
•
•
•
Press “TIME”, the digit for minutes starts to flash.
Press “TIME” again, the digit for seconds starts to flash.
Set the distillation time by pressing “UP” and “DOWN”.
Start the distillation by pressing “START”.
Digits stop flashing after a certain time or after starting the distillation.
When pressing “UP” and “DOWN”, the time is first counted slowly, then faster.
The distillation time can be set in a range of 1 second to 99 minutes 59 seconds.
6 .3 Setting the steam power
To set the steam power, proceed as follows:
• Press “STEAM”, the digit starts to flash.
• Set the steam power by pressing “UP” and “DOWN”.
Digits stop flashing after a certain time or after starting the distillation.
When pressing “UP” and “DOWN”, the steam power is first counted slowly, then faster.
The steam power can be set in a range of 30 to 100%.
6 .4 Program storage
6 .4 .1
6 .4 .2
The program storage function can be used optionally. Up to 9 programs can be stored. In addition the last used program is stored.
Storing a program
•
•
•
•
•
•
•
To store a program, proceed as follows:
• Select a program with “UP” and “DOWN”. The steam-display shows P and the program number.
The program settings are shown after releasing the “UP”/”DOWN” button.
Press “STEAM” and set the steam power by pressing “UP” and “DOWN”.
Press “TIME”, the digit for minutes starts to flash.
Press “TIME” again, the digit for seconds starts to flash.
Set the distillation time by pressing “UP” and “DOWN”.
Press “REAGENT 1” until you reach the required acid or water dosing volume for storage.
Press “REAGENT 2” until you reach the required sodium hydroxide dosing volume for storage.
Press “START” to store the program.
Selecting a stored program
Select a stored program by pressing “UP” and “DOWN”. The steam-display shows “P” and the program number. The program settings are shown after releasing the “UP”/”DOWN” button.
NOTE
The program settings are changed before a new distillation is started. The old program settings will be overwritten with the new settings.
23 K-355 Operation Manual, Version G
6 Operation
6 .5 Steam generator status
6 .5 .1
6 .5 .2
Heating
A constant colon (:) and an “H” in the STEAM-display indicates, that the steam generator is heating.
A flashing colon (:) and a signal sound for 1 second indicates that the steam generator is ready.
Standby mode (after 30 minutes)
The TIME display and STEAM display show (-----).
Press “START” to cancel the standby mode.
6 .6 Switching ON/OFF checklist
To switch on and preheat the instrument, proceed as follows:
•
•
•
•
•
•
•
Check the filling level of the supply tanks.
Open the main water tap.
Switch on the instrument and wait until the steam generator is ready.
Insert an empty sample tube and an empty receiving vessel.
Close the protective door.
Set the distillation time to 2 minutes (see section “Setting the distillation time”) and the steam to
100% (see section “Setting the steam power”).
Start the distillation by pressing “START”.
•
•
•
To switch off the instrument, proceed as follows:
Switch off the instrument.
Close the main water tap.
Rinse the reagent 1 pump with distilled water when it is used for the additon of strong acids.
6 .7 Carrying out a distillation
•
•
•
To carry out a distillation, proceed as follows:
•
•
•
•
Switch on the instrument and wait until the steam generator is ready.
Insert the sample tube containing the sample.
Prepare a conical flask or a similar receptacle with a volume of about 250 ml as receiving vessel.
If required, select suitable chemicals in accordance with the method and the substance you determine.
Add reagents as required.
Set the required distillation time or select a program.
Start the distillation by pressing “START”.
For Kjeldahl distillation note the following:
•
•
•
Fill boric acid solution of 4% and 2-3 drops of Sher indicator into the receiving vessel. Alternative:
Select suitable chemicals for the back titration.
Add water to dilute the sample by pressing “REAGENT 1”. The dilution with water prevents a too violent reaction when the sodium hydroxide solution is subsequently added. The sample must be diluted in a ratio of approximately 1 part of acid to 2 parts of water.
Add sodium hydroxide solution by pressing “REAGENT 2”: Recommended alkali concentration:
32%. Add alkali to the sample in a ratio of about 1 part of acid to 3 parts of sodium hydroxide
24 K-355 Operation Manual, Version G
6 Operation solution. The volume of the added sodium hydroxide solution is measured on the scale behind the sample tube. The added volume selected must produce a clear shift in color to brown or blue.
NOTE
After distillation or after “ STOP“, the last distillation time can be recalled by pressing “ START“ or will automatically be recalled when exchanging the sample tube.
25 K-355 Operation Manual, Version G
7 Maintenance and repairs
7 Maintenance
This chapter gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition.
WARNING
Electrical hazard:
• Prior to all maintenance work on the instrument switch off the power supply and remove all sources of flammable vapor.
WARNING
All maintenance and repair work requiring the opening or removal of instrument covers may only be carried out by trained personnel and with the tools provided for this purpose.
The service door may only be opened for maintenance or service purposes.
WARNING
Potentially hot service door or interior behind the service door during operation (surface temperatures at times exceed 60 °C). Danger of burns.
• Always let the instrument cool down before opening the service door.
ATTENTION
Always wear personal protective equipment such as protective eye goggles, protective clothing and gloves when maintaining the instrument.
Check the instrument for proper operation after any repair work.
7 .1 Daily maintenance
7 .1 .1
7 .1 .2
7 .1 .3
Cleaning the instrument from inside
To ensure proper instrument functioning regular cleaning is vital. Thus the generation of caustic substances within the instrument and the degradation of glassware is avoided. To clean the inside of the instrument, distill 100 ml of distilled water for a period of 2 minutes.
Rinse the reagent 1 pump with distilled water.
Cleaning the housing
Check the housing for defects (switches, plugs) and clean it with a damp cloth.
ATTENTION
Never use solvents as cleaning agents as these might damage the instrument.
• As the housing is made of polyurethane and covered with an acid-resistant coating, any acid drops must be wiped away immediately with a damp cloth.
Cleaning the glass parts
The glass parts can be taken out and cleaned with commercially available cleaning agents or in an ultrasonic bath. After the glass parts have been cleaned and fully dried, check each part visually for cracks, scratches and for any parts or sections that might have splintered off. Take out and replace any damaged glass parts.
26 K-355 Operation Manual, Version G
7 Maintenance and repairs
7 .1 .4 Preparing the instrument for a standstill overnight
To prepare the instrument for a longer standstill (e.g. overnight), fill 50 ml distilled water into the receiving vessel and 30 ml of distilled water into the sample tube.
7 .2 Weekly maintenance
7 .2 .1 Cleaning the splash protector and the rubber bung seal
Unmount the splash protector and remove the rubber bung seal.
Rinse the splash protector with water to remove sample residues.
We recommend to replace the splash protector after approximately 5000 determinations, depending on the kind of application and frequency of maintenance.
To prolong the lifetime of the seal, rinse it with water, especially if working with crystalline products.
Afterwards, dry it with a soft cloth, remount it and put the splash protector back in place.
ATTENTION
When removing and reinstalling the seal, make sure not to damage it. Always move it perpendicularly to the axis of the glass parts and ensure no damage occurs to the sealing lip.
Never apply grease to the seal and never touch it with sharp objects, otherwise it will get damaged.
7 .3 Monthly maintenance
7 .3 .1 Checking the distillate amount
To check the distillate amount, wait until the steam generator is ready, i.e. the instrument is warmed up. Then run a single sample with an empty tube and an empty receiving vessel with the following parameters:
Table 7-1: Checking the distillate amount
Parameter
Check distillate amount:
Sample tube:
Water:
NaOH:
Distillation time:
Setting
Distillation and titration empty
0 ml
0 ml
5:00
After the check is finished, measure the distillate amount by means of a measuring flask. With the above parameters it should be about 150 ml.
27 K-355 Operation Manual, Version G
7 Maintenance and repairs
7 .4 Half-yearly maintenance
7 .4 .1 Replacing the NaOH tube
We recommend to replace the NaOH tube every six months. The other tubes need to be replaced as and when required.
7 .5 Yearly maintenance
7 .5 .1
7 .5 .2
Replacing the rubber bung seal
The seal is subject to wear and tear, thus you should check it regularly. We recommend to replace it once a year.
Replacing the NaOH pump
We recommend to replace the NaOH pump once a year. The other pumps need to be replaced as and when required.
7 .6 Customer service
•
•
•
Only authorised service personnel are allowed to perform repair work on the instrument. These persons have a comprehensive technical training and knowledge of possible dangers which might arise from the instrument.
Addresses of official Buchi customer service offices are given on the Buchi website under: www.buchi.com. If malfunctions occur on your instrument or you have technical questions or application problems, contact one of these offices.
The customer service offers the following:
Spare part delivery
Repairs
Technical advice
28 K-355 Operation Manual, Version G
8 Troubleshooting
8 Troubleshooting
This chapter helps to resume operation after a minor problem has occurred with the instrument. It lists possible occurrences, their probable cause and suggests how to remedy the problem.
The troubleshooting table below lists possible malfunctions and errors of the instrument. The operator is enabled to correct some of those problems or errors by him/herself. For this, appropriate corrective measures are listed in the column “Corrective measure”.
The elimination of more complicated malfunctions or errors is usually performed by a Buchi technical engineer who has access to the official service manuals. In this case, please refer to your local Buchi customer service agent.
8 .1 Malfunctions and their remedy
Table 8-1: General malfunctions and their remedy
Error number / Error indication Possible cause
E 30
E 31
E 32
E 40
Service door open.
Protective door open.
Sample tube missing.
Steam generator overheat.
E 40 - E 47
E 50 - E 56
E 61 Cooling water flow too low
(< 0.5 l/min for > 30 seconds).
E 70 - E 76
Signal sound in a 10 seconds interval
“H” in the STEAM display
Keyboard problem.
Steam generator is heating, not ready for distillation.
Decimal point flashing in the
TIME display during distillation
Decimal point stable in the
TIME display during distillation
Electronic problem.
Steam generator problem.
Cooling water flow too high
(> 2.5 l/min).
Cooling water flow too low
(< 0.5 l/min).
Corrective measure
Close service door.
Close protective door.
Insert a sample tube.
Switch off the instrument immediately and contact the Buchi customer service.
Contact the Buchi customer service.
Water feeding problem. Control the water volume in the tank.
Control the tube connections.
Increase the cooling water flow.
Check the tightness of the cooling water circulation.
Switch off the instrument.
Contact the Buchi customer service.
Heating takes approx. 3 minutes. A flashing colon (:) and no “H” in the
STEAM display indicates that the steam generator is ready.
Reduce the cooling water flow.
Increase the cooling water flow until the decimal point disappears
(reaction time approx. 5 seconds).
Check the tightness of the cooling water circulation system.
29 K-355 Operation Manual, Version G
9 Shutdown, storage, transport and disposal
9 Shutdown, storage, transport and disposal
This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and specifies the storage and shipping conditions.
9 .1 Preparing the instrument for transport
Take out the power cord and remove all water/reagent tubing. Rinse the sodium hydroxide solution tube with distilled water. Clean the instrument thoroughly, so that all chemical residues are removed completely.
To empty the steam generator, proceed as follows:
• Turn off the instrument and disconnect the power cord.
WARNING
The steam generator gets very hot during operation. Danger of being burned.
• Always let the steam generator cool down for at least 30 minutes after having switched it off before handling it.
•
•
•
•
Open the service door.
Attach an appropriate silicone tube to the drain cock.
Place a receiving vessel with a volume of 500 ml below the end of the tube.
Slowly open the stop-cock with a screw driver and empty the steam generator completely.
9 .2 Storage and transport
Store and transport the instrument in its original packaging.
9 .3 Disposal
To dispose of the instrument in an environmentally friendly manner, a list of materials is given in chapter 3. This helps to ensure that the components are separated and recycled correctly.
Please follow valid regional and local laws concerning disposal.
30 K-355 Operation Manual, Version G
10 Spare parts
10 Spare parts
This chapter lists spare parts, accessories, and options including their ordering information.
Order the spare parts from Buchi. Always state the product designation and the part number when ordering spare parts.
Use only genuine Buchi consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
10 .1 Spare parts K-355
2
11
1
3
4
12
5
8
6
9
7
10
Table 10-1: Spare parts K-355
Product a Set of clamps Ø 7.6 / Ø 11.9 / Ø 9.6 /
Ø 10.7 / Ø 12.8 (5 pieces each) b SVL 22 screw cap c SVL 22 sealing d Outlet tube for distillate, PTFE e Set of hose connectors, bent EPDM sealing (4 pieces) f Set of hose connectors, straight, FPM sealing (4 pieces) g Set of sealings, FPM (10 pieces) h Gasket, complete (splash protector)
Gasket with ring and without screw nut (splash protector) i Set of connectors cooling water outlet
(1 piece of each) j Hose connector, PP k Splash protector, glass l Condenser m Check valve, complete n Splash protector, polypropylene
Order number
43586
03577
02073
43569
43129
40296
40040
43068
43538
43565
43332
43320
43356
43590
14
13 o Set of accessories for splash protector
K-350 and K-355
43585
15
31 K-355 Operation Manual, Version G
10 Spare parts
Table 10-1: Spare parts K-355 (cont.)
Product p Drip tray
Order number
43302
16
4 sample tubes 300 ml
Cap for 20 l tanks, large (1 piece)
10 .2 Hosing connection scheme
12
1
9
11
5
10
6
2
7
3
8
4 a Inlet b NaOH tank c H
2
O tank d Acid tank e Valve cooling water in f Pump NaOH g Pump H
2
O steam generator h Pump special
Fig. 10.1: Hosing connection scheme i Cooler j Receiving vessel k Splash protector l Check valve m Ventilation n Valve steam o Output
13
14
37377
43478
15
32 K-355 Operation Manual, Version G
103
105
106
107
108
109
110
21
22
23
101
102
111
112
113
114
16
17
18
19
20
9
10
12
14
15
Table 10-2: Tubes and components Distillation Unit K-355
Position Order number Pcs Description
1 - 2
3
4
43555
43153
43151
1
1
1
Solaflex tube Ø 10/5, L = 3500
Unisil Ø 6 x 2, L = 640
Unisil Ø 6 x 2, L = 370
7
8
5
6
43154
43572
43578
43574
1 Unisil Ø 6 x 2, L = 920
1 Viton tube Ø 9/6, L = 1200
1 Viton tube Ø 10/7, L = 380
1 Viton tube Ø 10/7, L = 190
43575
43574
43029
43573
43573
43572
43574
43578
43574
43574
1
1
1
1
1
1
1
Viton tube Ø 10/7, L = 230
Viton tube Ø 10/7, L = 190
EPDM 6.35/1.58, L = 530
Viton tube Ø 7/4, L = 120
Viton tube Ø 7/4, L = 120
1 Viton tube Ø 7/4, L = 1200
1 Viton tube Ø 10/7, L = 190
1 Viton tube Ø 10/7, L = 380
Viton tube Ø 10/7, L = 190
Viton tube Ø 10/7 L = 190
43574
43439
37780
43139
27738
43202
29646
43207
11043
43565
03562
43139
43542
43533
43534
40297
1 Viton tube Ø 10/7, L = 190
1 Silicone tube Ø 14/10, L = 1800
1 Cooling water tube, complete, L = 1500
3 Connectors GL-14, bent, EPDM
11 Hose clamps Ø 9.6, black
7 Hose clamps Ø 10.7, green
1 CW flow sensor
1 Tube spout
3 Y-pieces PP
1 Reduction piece PP
7 Binders 2.5 x 98 mm
1 Connector, bent, black
1 Screw spout D4, G1/8”
1 Screw spout, bent D4, G1/8”
1 Screw spout D6, G1/8”
1 Connector, bent, green
10 Spare parts
33 K-355 Operation Manual, Version G
11 Declarations and requirements
11 Declarations and requirements
11 .1 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, pursuant 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 likely 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 réglementations FCC ainsi qu’à la réglementation des interférences radio du Canadian Department of Communications. Ces limites sont destinées à fournir une protection adéquate contre les interférences néfastes lorsque l’appareil est utilisé dans un environnement commercial.
Cet appareil génère, utilise et peut irradier une énergie à fréquence radioélectrique, il est en outre susceptible d’engendrer des interférences 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 néfastes, auquel cas l’exploitant sera amené à prendre les dispositions utiles pour palier aux interférences à ses propres frais.
34 K-355 Operation Manual, Version G
11 .2 Declaration of conformity
11 Declarations and requirements
35 K-355 Operation Manual, Version G
BÜCHI Labortechnik AG
CH-9230 Flawil 1 / Switzerland
T +41 71 394 63 63
F +41 71 394 65 65
www .buchi .com
093036
Quality in your hands
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