Read these instructions thoroughly before you use the BÜCHI
Distillation Unit K-314. 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.
Chapter 2 contains important safety information. Knowledge
of this is imperative for the safe operation of the Distillation
unit.
1 Sample tube 500 mL26128
1 Rack for 4 sample tubes 500 mL16951
1 Special rubber bung for16890
Tecator/Gerhardt glasses
1 Handle with cam for26109
Tecator/Gerhardt glasses
1 Indicator acc.Sher, 100 ml03512
Table 3: Accessories
Page 3
BÜCHI Distillation Unit K-314
2 Safety
2Safety
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.
2.1Symbols
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.
2.2Requirements 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.
Personnel without this training or persons who are in training
require thorough instruction. These operating instructions
are the basis.
2.3Regulation use
The unit is conceived and built as a piece of laboratory
equipment. Its regulation use is the distillation of steam
volatile substances.
2.4Non-regulation use
Any use other than those 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
Page 4
2 Safety5BÜCHI Distillation Unit K-314
BÜCHI Distillation Unit K-314
2.5General hazards
General hazards arise from:
• Hot acids and bases
• 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!
2.6Safety measures
The distillation unit K-314 is equipped with a protective
door, which must be closed during operation.
The wearing of personal safety equipment such as safetyglasses, gloves and
As a necessary part of the distillation unit K-314, 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.
The fusion processing glass must only be removed with
pliers because of danger beeing burnt.
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.
ll
laboratory coats is necessary.
ll
4
Page 5
2 Safety
It is to be assumed that a safe operation is not possible
any more
• if the unit is visibly damaged,
• If the unit is not functioning any more
• after long storage under anfavourable conditions,
• 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.
Page 6
3 Function
햳
햴
BÜCHI Distillation Unit K-314
3Function
The distillation unit K-314 is suitable for determining nitrogen
using the Kjeldahl and Devarda methods
distillations (e.g., of alcohol) can also be carried out easily.
3.1 Principle of operation
햲 Sample tube
햳 Splash protection
햴 Cooler
햵 Distillate outlet tube
햶 Receiving vessel
. .
. Other steam
. .
햲
Fig. 3: Principle of operation K-314
햵
햶
6
Page 7
BÜCHI Distillation Unit K-314
4 Putting into operation
4Putting into operation
4.1Setup location
The distillation 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 distillation unit.
4.2Unpacking
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.
Fig. 4: Standard sleeve nut (premounted)
Fig. 5: K-314 rear
햲
햳
4.3Water supply
The distillation unit K-314 is delivered with 3 Nyflex highpressure hoses intended for the following connections:
• cooling water inlet
•H
O supply tank
2
• NaOH supply tank
Connect the cooling water connector to the mains water tap.
The standard sleeve nut has an R 1/2” thread (Fig. 4).
Shorten the Nyflex hose to the optimum length, connect it
to the water connector, and secure it with a hose clamp.
Connect the other end of the hose to the cooling water
inlet nipple.
Cooling water outlet (2):
Shorten the silicone hose [9/6 mm] to the optimum length
and connect it to the cooling water oulet nipple (OUT
nipple). Direct the open end into the drain.
Check
The cooling water must flow through the cooling unit from
the bottom to the top.
Make sure that the hose drains freely. No kinks! No airtraps
in the hose!
7
Page 8
4 Putting into operation
BÜCHI Distillation Unit K-314
4.4Drain hose (3)
Make sure that the hose drains freely. No kinks! No airtraps
in the hose!
Fig. 6: Drain hose arrangement
004113
026058
026660
026411
ca. 456
Fig. 7: Connection supply tanks
4.5Connection of the supply tanks
• Connect the Nyflex hose to the flow-through tube
• Unscrew the small tank cap and stick it on the flowthrough tube
• Insert the flow-through tube with the tank cap on into
the tank until it reaches the stop
• Tighten the tank cap
• Connect the hose from the water tank to the K-314
(H
O nipple)
2
• Connect the hose from the sodium hydroxide tank to
the K-314 (NaOH nipple
• Fix the hose nozzle in place on the large tank cap.
The supply tanks must not be any higher than the unit
itself, nor any lower than 1 meter below it.
8
Page 9
BÜCHI Distillation Unit K-314
5 Operation
5Operation
5.1Control elements
햶
햷
햵
햻
Fig. 8: Arrangement and designation of the control and display elements
햽
헂헁
Fig. 9: Arrangement and designation of the connection nipples
헀
햾
햿
햲
햳
햴
햸
햹
햺
햲 Main switch
햳 Pressure switch for adding the sodium hydroxide
solution
햴 Steam tap
햵 Digestion tube
햶 Rubber bung with PTFE hose
햷 Sample tube holder
햸 Distillate outlet tube with PTFE hose
햹 Receiver plate
햺 Drip tray
햻 Protective door
햽 Connection nipple for cooling water inlet hose (IN)
햾 Connection nipple for cooling water outlet hose (OUT)
햿 Connection nipple for sodium hydroxide solution
(NaOH)
헀 Connection nipple for water (H
O)
2
헁 Connection nipple for drain
헂 Mains connector with 2 fuses 20x5,10 AT
Fig. 10: Control elements and their function
I/O
NaOH
Steam
5.2Control elements and their function
I / OAfter switching on the distillation unit, it takes
about 90 seconds before the unit is ready for
operation.
Before switching on, check that the supply tanks
and/or the hoses are filled with reagents.
NaOHSodium hydroxide adding switch.
The alkali is dosed in as long as the switch is
pressed.
SteamSteam on / off.
Switching the distillation on and off manually.
9
Page 10
5 Operation
BÜCHI Distillation Unit K-314
5.3Start-up checklist
The first time that the distillation unit is started up, there is
a penetrating odor. This smell, however, is of no importance.
It occurs when the heater pipe and the isolation become
warm. No overheating of the steam generator is possible.
5.4Supply tanks
Fill the supply tanks. This can be done, for example, using
a bent funnel (Item No. 16662) or a footpump. The reagents
are forwarded within the K-314 unit by suction.
To ensure optimum long-time operation, the steam generator
must only be operated on distillated or deionized water!
Advantages:
1.No cleaning of the steam generator is necessary
2.The blank values can be kept under control.
Never supply the steam generator from a building distilled
water distribution pipe!
5.5Rubber bung and PTFE hose
Check that the rubber bung and the PTFE hose are still properly
fitted, especially after they have been subjected to stresses
during transport or otherwise.
Mounting instruction:
If the PTFE hose has become loose, hold it with a piece of
sandpaper and refit it without kinking.
10
Page 11
BÜCHI Distillation Unit K-314
햲
5 Operation
5.6Sample tube holder
The sample tube holder has been correctly adjusted in the
factory.
Check whether the holder is still correctly positioned;
• Push the quick-locking clamp all the way up (1)
• Insert the test tube as shown on the figure (2)
• Now push the quick-locking clamp all the way down (3)
• The sample tube is now positioned.
The tube should not be too loose (possible
leakage) or too tight (deformation of the
rubber bung).
햳
Loosen the holders Phillips-head screws (4)
and adjust the holder according to the
position of the sample tube.(4).
햴
Fig. 11: Inserting the sample tube
햵
11
Page 12
5 Operation
BÜCHI Distillation Unit K-314
5.7Distillation outlet tube
Fit the distillate outlet tube onto the cooler outlet using the
coupling ring and inserted gasket. Slide the PTFE hose,
top down, as far to the bottom of the receiving vessel as
possible.
The distillate outlet tube has an aeration valve (patented
by Büchi) that keeps the receiving solution from being
sucked back.
5.8Connection to the mains
Before switching the distillation machine K-314 on for the
first time, make certain that the power system voltage is
the same as that indicated on the unit's nameplate.
Then connect the distillation unit cable to the mains.
5.9Adjusting the cooling water flow
• Open the cooling water tap until the flow of water at the
outlet hose is 1 l/min.
The distillate must leave the cooler cooled!.
5.10 Switching the K-314 ON/OFF checklist
Switching on and preheating the distillation unit K-314
• Check the filling of the supply tanks,
• Open the main water tap, regulate the water flow,
• Switch on the distillation unit K-314 and wait until the
steam generator is ready,
• Insert an empty sample tube and an empty receiving
vessel,
• Close the protective door,
• Turn steam tap to ON (2 minutes),
• The unit is now ready for the distillation.
12
Page 13
BÜCHI Distillation Unit K-3146 Bedienung
5.11 Carrying out the Kjeldahl distillation
• Switch the unit on and preheat,
• Wear goggles!
• Insert the digestion tube containing the specimen diluted
in water
Dilution with water prevents too violent a reaction when
subsequently adding the hydroxide solution.
The specimen must be diluted in a ratio of approximatly
1 part of acid to 2 parts of water.
• Prepare a conical flask or a similar receptacle (250 ml)
as the receiving vessel, dilute with 60 ml boric acid
(2%) and 2-3 drops of Sher indicator (Item No. 03512).
Alternative: Choose a suitable indicator for the back
titration.
Fig. 13: K-314 in operation
• Add sodium hydroxide solution:
Recommeded alkali concentration: 32%
Add alkali to the specimen in a ratio of about 1 part
acid to 3 parts sodium hydroxide solution. The volume
of the added sodium hydroxide solution is measured
on the scale (behind the distillation glass).
The added volume selected must produce a clear shift
in color to brown or blue.
• Distillation
Steam tap to ON
A distillation time of approximately 3 minutes is required
to get a volume of 100 ml.
• After the completion of the distillation turn the steam
tap back to OFF.
5.12 Cleaning the unit
Clean the unit by distilling 100 ml distilled water for a period
of 2 minutes.
13
Page 14
BÜCHI Distillation Unit K-3145 Operation
5.13 Malfunctions
MalfunctionPossible causeRemedy
No steam production,1. Water tank is empty1. Fill water tank
other functions OK2. Water pump does not suck any2. Fill water tank
water, hoses remain empty
3. Steam generator or steam3. Replace the defective part
valve defective
Distillate receiving solution is suckedDrain tube with ventilationClean the ventilation valve
into the coolervalve obstructedthoroughly
Resultats too low1. Screwed fitting between the cooler1. Tighten the screwed fitting
and splash protection is
2. Distillation time too short2. Extend distillation time
3. Unit not preheated3. Preheat the unit
4. Fusion processing time too short4. Extend fusion processing time
Sodium hydroxide not fed in1. Tank empty1. Fill the tank
2. The pump is not sucking2. Check electrical connections
3. The pump is blocked3. Clean the pump
4. The pump is faulty4. Exchange the pump
Steam escapin from the housing1. Hose connection leaking1. Check hose connection
Distillate too warm1. Main water tap closed1. Open main water tap
2. Too little cooling water2. Increase cooling water flow
Unit does not work1. Mains fuse(s) defective1. Replace the fuse(s)
Green check lamp not lit.
14
Page 15
BÜCHI Distillation Unit K-314
6 Maintenance
6Maintenance
6.1General information and Preparations
The distillation unit K-314 casing has a plastic coating. The
wet domain also has a plastic jacketing.
In order to avoid damage to these plastic coverings, wipe
off any acid or alkaline splashes immediately with a wet
cloth.
6.2Maintenance: daily, weekly
Daily:
• Check for damage on glass parts
After stand still overnight, or after long periods of non-use:
• Insert a sample tube containing approximatively 30 ml
destillated water,
• Fill the receiving vessel with destillated water so that
the PTFE hose is just barely immersed.
Weekly:
• Remove the rubber bung and clean it with water.
• Also clean the exposed glass nozzle on the splash
protection.
The glass parts are cleaned.
6.3Rubber bung and PTFE hose
During the life duration of the rubber bung it is advantageous
to remove it periodically, approximately after 100 distillations,
and to clean it with water without any cleaning product or
solvent.
• Remove the rubber bung by turning it downwards and
clean it carefully with water,
• Clean also the liberated glass nozzle of the splash
protection with a wet cloth.
15
Page 16
6 Maintenance
BÜCHI Distillation Unit K-314
6.4Cleaning the feeding pump
Proceed as follows when the sodium hydroxide feed pump
no longer functions correctly:
• Prepare approximately 1 liter water,
• Open the small cover of the supply tank,
• Carefully take out the flow-through tube and place it in
the water vessel,
• Press the NaOH switch until the sample tube is filled,
• Remove the sample tube and empty it,
• If necessary, repeat the process.
6.5Changing glass parts
The glass parts are held in place with a quick-locking
fastening device.
• Close the water tap,
• Switch off the unit
• Pull the mains plug
• Loosen the screw cap connecting the splash protection
and the cooler and carefully take the splash protection
out of the cooler. Release the holding springs by simply
pressing them down by hand.
• Slowly pull the splash protection out forward and pull
the distributor off the glass part (if necessary, replace
the distributor as well).
Proceed in the reverse order for reassembly.
After the first distilllation, check that the screw cap is
correctly positioned. If necessary, tighten it.
6.6Customer 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.
16
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.
Page 17
BÜCHI Distillation Unit K-314
햲
6 Maintenance
Büchi’s customer service offers the following services:
• Replacement part service
• Repair service
• Maintenance service
• Technical consultation.
6.7Main fuses
Please change the main fuses as follows::
• Pull out mains cables
• Pull out fuse holders 햲
• Replace the defective mains fuse by a new one with same
performance 햳:
- 230V:T 10A L 250V
Fig. 14: Device plug, inserted
• Insert again fuse holders
햳
6.8Checking the unit
In order to check that the unit is functioning properly, do a
nitrogen analysis using ammonia salt. For a standard
application, we recommend the following parameters:
Standard substance: Ammonium dihydrogen phosphate
p.A.
Molecular weight:115.03
Nitrogen content:12.17%
Originally weighed in:400 to 500 mg
H2O:20 ml
NaOH:20 ml
Distillation time:4 min
Titration:Sulphuric acid 0.5 N
Consumption:approx. 7-10 mL
Table 7: Checking th unit parameters
17
Page 18
7 Taking out of service
BÜCHI Distillation Unit K-314
7Taking out of service
Remove all dangerous substances and clean the unit
thoroughly.
This avoids any risk that individuals could come into contact
with dangerous substances.
7.1Storage/Transport
The unit has to be cleaned and repacked in its original
packaging when it is being stored or transported.
7.2Disposal
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.
18
Page 19
BÜCHI Distillation Unit K-314
8 Replacement parts
8Replacement parts
Only original Büchi accessories and replacement parts
guarantee safe operation and a proper functioning of the
unit. The use of replacement parts and accessories other
than those recommended by Büchi is permissible only with
prior approval from the manufacturer. The replacements
parts cited herein may be used only for purposes of
disassembly and reassembly as described in Chap. 6 of
this Instruction Manual. It is strictly forbidden to disclose
this manual or its contents to third parties. No production
of parts based on the information contained herein is
permissible.
8.1Replacement parts
1Fuses 10*10 AT16952
1Splash protection36900
1Cooler26004
1Distillate outlet tube, complete26302
1Set of sample tubes 300 mL (4 pieces)37377
1PTFE hose to digestion tube19010
1PTFE hose to distillate outlet tube26300
1Rubber bung03907
1Connector (Hypalon)19002
1Seal ø 22 mm02073
1Seal ø 15 mm03574
1Screw cap nut ø 22 mm03577
1Screw cap nut ø 15 mm03549
1Sample tube 500 mL26128
1Drip tray26290
1Silicone hose D 9/604133
1Silicone hose D 14/1004134
1Nyflex hose D 14/804113
1Water connection10992
1Tank 10 L NaOH, complete26112
1Tank 10 L H2O, complete26113
1Gasket for tank26411
1Flow-through tube D 8/6 mm26058
1Screw cap26660
1Tank plug25869
Table 5: Replacement parts
19
Page 20
BÜCHI Distillation Unit K-3149 Appendix
9Appendix
9.1Technical data
Dimensions (Width x Height x Depth)245 x 420 x 220 mm
Nominal voltage230 V, 50/60 Hz
Mains voltage tolerance+10 % / -15 %
Power rating1800 Watt
Power consumptionapprox. 8 Ampère
Volume supply tank10 L
Volume sample tubes300 ml (Standard)
500 ml (Special)
Weight (netto)approx. 16 kg
Dimensions320 x 695 x 320 mm
Ambient temperatureOperation:+10 to +40° C
Storage:- 40 bis +70° C *
Steam or distillate flow capacityapprox. 30ml/min
Overvoltage CategoryII
Pollution degree2
*Note:If being stored at temperatures below +5° C, remove all liquid from the unit.
Due to the danger of frost, the steam generator, cooler, hoses etc. must all be emptied !
Caution:The steam generator may only be emptied by authorized service personnel.
Housing steam generatorPolysulphones with 20% fiberglassPSU/20% GF
Rubber bungHypalonCSM
DistributorEthylene-propylene rubberEPDM
MetalsX5CrNi18101.4301
X10CrNiS1891.4305
HosesPolytetrafluorethyleenPTFE
Silicone
Table 7: Materials used
20
Page 21
BÜCHI Distillation Unit K-314
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.
9 Appendix
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.
21
Page 22
9 Appendix
We
declare under our sole responsibility that the product:
to which this declaration relates is in conformity with the following standards:
BÜCHI Distillation Unit K-314
9.4Declaration of conformity
BÜCHI Labortechnik AG
Postfach, CH-9230 Flawil
Switzerland
BÜCHI Distillation Unit K-314
EN 61010-1:1993 (~ IEC 1010-1, VDE 0411-1)
Safety requirements for electrical equipment for measurement, control an laboratory use: General requirements
EN 55011:1991/B (~ VDE 0875/B, VDE 0871/B)
Maximum permissible values and measurement technique for radio interference by industrial, scientific and medical
high-frequency devices
EN 61000-3-2: 1995/1996
Limits for harmonic current emissions
EN 61000-3-3: 1995
Limitation of voltage fluctuations and flicker
In accordance with the regulations of the EU guidelines:
73/23/EWG (Electrical special tools/low voltage guidelines)
89/336/EWG (electromagnetic compatibility)
Flawil, 19th December 2000
BÜCHI Labortechnik AG
Meierseggstrasse 40
9230 Flawil
Schweiz