Operation Manual

Distillation Unit
K�­355

93036 en
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 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 competi-
tive 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.

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 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

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 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

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 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 safety-
related 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-vola-
tile substances.

2.3 Improper use

Applications not mentioned above are improper. Also, applications which do not comply with the tech-
nical 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.

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 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

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.

2.5.1 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.

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 2 Safety

2.5.2 Other hazards

WARNING
Certain solvents in or in the vicinity of the instrument can form peroxides and/or are highly inflam-
mable.
• A
 lways 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.

2.5.3 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:

• P rotective 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.

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 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 autho-
rized 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 modifi-
cations.

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 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 Order number

Distillation Unit K-355 Standard with 43505

glass splash protector, 230 V, 50/60 Hz
Distillation Unit K-355 with splash 43419
protector made of fiber glass reinforced
polypropylene, 230 V, 50/60 Hz
Distillation Unit K-355 Standard with 43070
glass splash protector and SO2 determi-
nation kit

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 3 Technical data

3.1.2 Standard accessories

Table 3-2: Standard accessories

Product Order number

a 1 mains cable of the following types

1 2 Type CH 10010
Type Schuko 10016
Type GB 17835
Type AUS 17836
Type USA 33763
Type Japan 10016
b 1 pair of glass tongs 02004
c 1 hose cooling water drain, silicone, 43439
L = 1.8 m, Ø 10/14 mm
6
4 5
3 d 1 hose chemical supply, solaflex, 43555
7 L = 3.5, Ø 10/5 mm
8
9 e 1 hose tygon, L = 530 mm 43029
11 10
f 3 suction tubes to tanks, FEP, 43407
L = 580 mm
g 1 hose connector PP 43565
h 1 Y hose coupling 11043
i 2 clamps Ø 7.6 43571
i 6 clamps Ø 11.9 43841
j 1 hose viton (acid resistant) L = 2 m 20344
k 1 cooling water hose complete: G ¾", 37780
½", L = 1.5 m
l 3 tanks 10 l, without caps 43410
m 1 cap for 10 l tanks, large 25869
n 3 tank labels 43434
o 1 cap for 10 l and 20 l tanks, small 43477
12

13 14

15

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 3 Technical data

3.1.3 Optional accessories

Table 3-3: Optional accessories K-355

Product Order number

a 1 sample tube 500 ml 26128

1 2 3 4 sample tubes 500 ml 43982
b 4 sample tubes 300 ml 37377
c Condenser cover, complete 43484

d 20 l tank for chemicals 43469

e 10 l tank for chemicals 43468

f Holder for 4 sample tubes, 500 ml 16951

g Holder for 6 sample tubes, 300 ml 43039

h Holder for 12 sample tubes, 300 ml 43041

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 3 Technical data

Table 3-3: Optional accessories K-355 (cont.)

Product Order number

 plash protector for Devarda method

S 43335
K-350/K-355/K-360/K-370

Constricted distillate outlet tube Ø 5 mm 43096

Sample tubes graduated, 300 ml, set of 4 43049

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 3 Technical data

Table 3-3: Optional accessories K-355 (cont.)

Product Order number

Universal adapter for K-350, K-355, 43115

K-360, K-370

SO2 accessory 48680

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 3 Technical data

3.2 Technical data

Table 3-4: Technical data K-355

Distillation Unit K-355

Power consumption max. 2.2 kW

Connection voltage 230 V ± 10% / 200 V ± 10%
Frequency 50/60 Hz
Current consumption (230 V) 8.5 A
Mains connection 3-pole (P, N, E) via power cord
Recovery rate ≥ 99.5%
Reproducibility (RSD) ≤ 1%
Detection limit ≥ 0.1 mg Nitrogen
Environmental conditions for indoor use only
Temperature 5 - 35 °C
Altitude up to 2000 m
Humidity maximum relative humidity 80% for temperatures up to
31 °C decreasing linearly to 67% relative humidity at
35 °C
Installation category II
Pollution degree 2
Dimensions (W x H x D) 400 x 660 x 360 mm
Weight 17 kg

3.3 Materials used

Table 3-5: Materials used for the K-355

Component Material designation Material code

Housing Polyurethane PUR / UL V0

Glass parts Borosilicate glass 3.3 DIN/ISO 3585
Steam generator isolation Ceramic fiber Multitherm 550
Steam generator housing Stainless steel 1.4301
Protective door Polymethyl methacrylate PMMA
Condenser cover Polymethyl methacrylate PMMA
Connecting stopper Hypalon CSM
NaOH tube Ethylene Propylene Dimonomer EPDM

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 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

4
1

a Splash protector dC ondenser

b Sample tube eO perating panel
c Protective door f Service door
Fig. 4.1: Instrument overview

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 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, SO2, volatile acids).
a Sample tube
b Splash protector
c Condenser
d Distillate outlet tube
e Receiving vessel with receiver solution
3

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).

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 4 Description of function

4.3 Controls of the instrument

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
1
f UP: Increases time and steam up
g STEAM: Sets steam power
h DOWN: Decreases time and steam down
2 i REAGENT: Button that adds reagent (e.g.
water, sodium hydroxide solution)

6
5
4
8
7

Fig. 4.3: Controls of the instrument

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 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 immedia-
tely 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 instru-
ment.

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 H2O inlet (for steam generator) from tank

b Reagent 1 inlet (water or acid)
a c Reagent 2 inlet (NaOH)
d Cooling water inlet
e Cooling water outlet
f Drain to waste
b

Fig. 5.2: Reagent and water connections

All pumps are self-priming, no overpressure is necessary at the tanks.

5.3.1 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”.

5.3.2 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:

• C ut 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 “H2O” 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 H2O 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 „H2O steam“, the steam generator will be damaged.

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 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 Manual dosage

When pressing “REAGENT 1” or “REAGENT 2” the connected reagent is dosed as long as the switch
is pressed.

6.1.2 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.

6.1.3 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.

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 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

The program storage function can be used optionally. Up to 9 programs can be stored. In addition the
last used program is stored.

6.4.1 Storing a program

To store a program, proceed as follows:

• S elect 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.

6.4.2 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.

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 6 Operation

6.5 Steam generator status

6.5.1 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.

6.5.2 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 deter-
mine.
• 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:
• F ill 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

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 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.

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 7 Maintenance and repairs

7 Maintenance

This chapter gives instructions on all maintenance work to be performed in order to keep the instru-
ment in good working condition.
WARNING
Electrical hazard:
• P
 rior 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 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.

7.1.2 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.
• A
 s 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.

7.1.3 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.

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 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 Setting
Check distillate amount: Distillation and titration
Sample tube: empty
Water: 0 ml
NaOH: 0 ml
Distillation time: 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.

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 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 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.

7.5.2 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 applica-
tion problems, contact one of these offices.
The customer service offers the following:
• Spare part delivery
• Repairs
• Technical advice

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 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 Corrective measure
E 30 Service door open. Close service door.
E 31 Protective door open. Close protective door.
E 32 Sample tube missing. Insert a sample tube.
E 40 Steam generator overheat. Switch off the instrument
immediately and contact the Buchi
customer service.
E 40 - E 47 Electronic problem. Contact the Buchi customer service.
E 50 - E 56 Steam generator problem. Water feeding problem. Control the
water volume in the tank.
Control the tube connections.
E 61 Cooling water flow too low Increase the cooling water flow.
(< 0.5 l/min for > 30 seconds). Check the tightness of the cooling
water circulation.
E 70 - E 76 Keyboard problem. Switch off the instrument.
Signal sound in a 10 seconds interval Contact the Buchi customer service.
“H” in the STEAM display Steam generator is heating, not Heating takes approx. 3 minutes. A
ready for distillation. flashing colon (:) and no “H” in the
STEAM display indicates that the
steam generator is ready.
Decimal point flashing in the Cooling water flow too high Reduce the cooling water flow.
TIME display during distillation (> 2.5 l/min).
Decimal point stable in the Cooling water flow too low Increase the cooling water flow until
TIME display during distillation (< 0.5 l/min). the decimal point disappears
(reaction time approx. 5 seconds).
Check the tightness of the cooling
water circulation system.

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 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.
• A
 lways 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.

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 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

Table 10-1: Spare parts K-355

1 4 5 Product Order number
6
7 a Set of clamps Ø 7.6 / Ø 11.9 / Ø 9.6 / 43586
Ø 10.7 / Ø 12.8 (5 pieces each)
2 b SVL 22 screw cap 03577
3
8 c SVL 22 sealing 02073
9 10 d Outlet tube for distillate, PTFE 43569
e Set of hose connectors, bent EPDM 43129
sealing (4 pieces)
f Set of hose connectors, straight, FPM 40296
sealing (4 pieces)
g Set of sealings, FPM (10 pieces) 40040
h Gasket, complete (splash protector) 43068
Gasket with ring and without screw
nut (splash protector)
i Set of connectors cooling water outlet 43538
(1 piece of each)
j Hose connector, PP 43565
k Splash protector, glass 43332
l Condenser 43320
m Check valve, complete 43356
n Splash protector, polypropylene 43590
11 12
14

13

o Set of accessories for splash protector 43585

K-350 and K-355

15

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 10 Spare parts

Table 10-1: Spare parts K-355 (cont.)

Product Order number

p Drip tray 43302

16

4 sample tubes 300 ml 37377

Cap for 20 l tanks, large (1 piece) 43478

10.2 Hosing connection scheme

12
14

1
9 11

5 13

10

15
6
2

7
3

8
4

a Inlet i Cooler
b NaOH tank j Receiving vessel
c H2O tank k Splash protector
d Acid tank l Check valve
e Valve cooling water in m Ventilation
f Pump NaOH n Valve steam
g Pump H2O steam generator o Output
h Pump special
Fig. 10.1: Hosing connection scheme

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 10 Spare parts

Table 10-2: Tubes and components Distillation Unit K-355

Position Order number Pcs Description
1-2 43555 1 Solaflex tube Ø 10/5, L = 3500
3 43153 1 Unisil Ø 6 x 2, L = 640
4 43151 1 Unisil Ø 6 x 2, L = 370
5 43154 1 Unisil Ø 6 x 2, L = 920
6 43572 1 Viton tube Ø 9/6, L = 1200
7 43578 1 Viton tube Ø 10/7, L = 380
8 43574 1 Viton tube Ø 10/7, L = 190
9 43575 1 Viton tube Ø 10/7, L = 230
10 43574 1 Viton tube Ø 10/7, L = 190
12 43029 1 EPDM 6.35/1.58, L = 530
14 43573 1 Viton tube Ø 7/4, L = 120
15 43573 1 Viton tube Ø 7/4, L = 120
16 43572 1 Viton tube Ø 7/4, L = 1200
17 43574 1 Viton tube Ø 10/7, L = 190
18 43578 1 Viton tube Ø 10/7, L = 380
19 43574 1 Viton tube Ø 10/7, L = 190
20 43574 1 Viton tube Ø 10/7 L = 190
21 43574 1 Viton tube Ø 10/7, L = 190
22 43439 1 Silicone tube Ø 14/10, L = 1800
23 37780 1 Cooling water tube, complete, L = 1500
101 43139 3 Connectors GL-14, bent, EPDM
102 27738 11 Hose clamps Ø 9.6, black
103 43202 7 Hose clamps Ø 10.7, green
105 29646 1 CW flow sensor
106 43207 1 Tube spout
107 11043 3 Y-pieces PP
108 43565 1 Reduction piece PP
109 03562 7 Binders 2.5 x 98 mm
110 43139 1 Connector, bent, black
111 43542 1 Screw spout D4, G1/8”
112 43533 1 Screw spout, bent D4, G1/8”
113 43534 1 Screw spout D6, G1/8”
114 40297 1 Connector, bent, green

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 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 protec-
tion 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.

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11.2 Declaration of conformity

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 BÜCHI Labortechnik AG
CH-9230 Flawil 1 / Switzerland
T +41 71 394 63 63
F +41 71 394 65 65 093036

www.buchi.com Quality in your hands

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