1002 Kjeltec Manual

31
Copyright 2003 / All rights reserved FOSS Tecator AB, Box 70, SE-26321 Höganäs, Sweden Tel Int +46 42 361500, Fax +46 42 343150 Kjeltec 1002 System Distilling Unit User Manual 1000 1535 / Rev. 2.3 1002001A

Transcript of 1002 Kjeltec Manual

Page 1: 1002 Kjeltec Manual

Copyright 2003 / All rights reserved

FOSS Tecator AB, Box 70, SE-26321 Höganäs, Sweden

Tel Int +46 42 361500, Fax +46 42 343150

Kjeltec™ 1002 SystemDistilling UnitUser Manual

1000 1535 / Rev. 2.3

1002001A

Page 2: 1002 Kjeltec Manual
Page 3: 1002 Kjeltec Manual

Dansk1

Teksten med sikkerhedsinformation erskrevet i denne stil og oversat til delokale sprog (EU/EES). Informationenkan findes på de gule sider.

Deutsch1

Text über Sicherheitsinformationen istin diesem Stil geschrieben und inandere Sprachen (EU/EES) übersetzt. DieInformationen finden sich auf dengelben Seiten.

1English Text regarding safety information is

written in this style and translatedinto the local language (EU/EES). Theinformation will be found in the yellowpages.

1�������� ������� ��������� �� ��� s � ��� � �� ����

courier � � ��� � � ��� � ��� ����� �����

��������� �� ��������s ���������� � ��� X���

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1Íslenska Texti sem vidkemur upplysingum um

öryggi er skrifadur í pessum stíl ogpyddur á stadarmálid (EU/EES).Upplàsingarnar má finna á gulu sídunum.

1Español El texto relativo a la información de

seguridad está escrito en este estilo ytraducido al idioma local (EU/EES). Lainformación figura en las páginasamarillas.

1Français Le texte concernant les informations

sur la sécurité est rédigé dans cestyle et traduit dans les languesnationales (EUROPE, EEE). Cesinformations se trouvent dans les pagesjaunes.

1Italiano Il testo relativo alle informazioni di

sicurezza è scritto in questo stile etradotto nella lingua locale (EU/EES).Le informazioni si trovano sulle paginegialle.

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Nederlands1

De tekst inzakeveiligheidsvoorschriften is in hetopgesteld en wordt in het Nederlandsvertaald. De informatie staat in degouden gids.

1Norsk Tekst som gjelder sikkerhetsinformasjon

er skrevet med denne stilen og eroversatt til lokalt språk (EU/EES).Informasjonen finnes på de gule sidene.

1Português O texto sobre as informações de

segurança está escrito neste estilo etraduzido na língua local (EU/EES). Asinformações encontram-se nas páginasamarelas.

1Suomeksi Turvallisuuteen liittyvät tiedot on

kirjoitettu tällä tyylillä ja käännettypaikalliselle kielelle (EU/EES). Tiedotlöytyvät keltaisilta sivuilta.

1Svenska Text som har med säkerhet att göra är

skriven med denna stil och är översatttill lokalt språk (EU/EES).Informationen hittas på de gulasidorna.

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Table of Contents

1 SAFETY PRECAUTIONS AND PROCEDURES1.1 Intended Use .............................................................................................1

1.2 Safety Precautions .................................................................................1

2 INTRODUCTION2.1 Performance Data ..................................................................................3

3 FUNCTION3.1 Principle of Operation .........................................................................4

3.2 Steam Generation ..................................................................................5

3.3 Alkali System ............................................................................................5

4 PREPARATIONS FOR USE4.1 Unpacking and Checking....................................................................6

4.2 Installation .................................................................................................7

4.2.1 Installation Requirements ...........................................................................7

4.2.2 Fuses .................................................................................................................7

4.2.3 Installation Instructions................................................................................7

4.3 Functional Verification .......................................................................8

4.3.1 Testing Recovery ............................................................................................8

5 OPERATION5.1 Identification of Controls..................................................................9

5.2 Starting Up .................................................................................................9

5.3 Distillation ..................................................................................................9

5.4 Closing Down..........................................................................................10

6 MAINTENANCE6.1 Daily..............................................................................................................11

6.1.1 Cleaning Cycle ..............................................................................................11

6.1.2 Cleaning of Unit ..........................................................................................11

6.1.3 Rubber Adapter ...........................................................................................11

6.2 Weekly .......................................................................................................11

6.2.1 Reagent Tanks Inspection and Cleaning................................................11

6.2.2 Digestion Tubes Inspection .......................................................................11

6.2.3 Cleaning the Safety Door ..........................................................................12

6.3 Every One to Three Months............................................................12

6.3.1 Controlling the Rubber Adapter..............................................................12

6.3.2 Controlling the Alkali Volume .................................................................12

6.3.3 Cleaning the Alkali Pump..........................................................................13

6.3.4 Cleaning of the Splash Head ....................................................................13

6.3.5 Depending on Number of Analyses ........................................................13

6.3.6 Cleaning of the Steam Generator ...........................................................14

6.3.7 Every Year .....................................................................................................14

7 TROUBLE SHOOTING

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8 FOSS Tecator AB APPLICATION NOTES SYSTEM9 TECHNICAL SPECIFICATIONS9.1 Safety...........................................................................................................18

9.2 Environmental Conditions ..............................................................18

9.3 Storage and Transport ......................................................................19

9.3.1 Lifting Instructions 1002 ............................................................................19

10 ACCESSORIES AND SPARE PARTS10.1 Accessories ...............................................................................................20

10.2 Spare Parts................................................................................................20

10.3 Kjeltabs.......................................................................................................20

10.4 Manufacturer’s Name and Address .........................................21

11 SAFETY PRECAUTIONS AND PROCEDURES ..........23

12 SICHERHEITS- UND BETRIEBSVORSCHRIFTEN (DE)26

13 SIKKERHED - FORHOLDSREGLER OG PROCEDURER(DK) .............................................................................................................30

14 PRECAUCIONES Y PROCEDIMIENTOS DESEGURIDAD (ES) ..............................................................................33

15 VAROTOIMET JA MENETELMÄT (FIN) ..........................37

16 PRESCRIPTIONS ET PROCEDURES DE SECURITE (FR)40

17 ËÇØÇ ÌÅÔÑÙÍ ÁÓÖÁËÅÉÁÓ ÊÁÉ ÏÄÇÃÉÅÓ ×ÑÇÓÇÓ(GR)..............................................................................................................44

18 ÖRYGGISREGLUR OG AÐFERÐIR (IS) .........................48

19 NORME PRECAUZIONALI E PROCEDURE DISICUREZZA (IT) ...............................................................................51

20 VEILIGHEIDSMAATREGELEN EN PROCEDURES(NL)..............................................................................................................55

21 SIKKERHETSREGLER OG PROSEDYRER (NO) ......59

22 PRECAUÇÕES E MEDIDAS DE SEGURANÇA(PT) ..............................................................................................................62

23 SÄKERHETSFÖRESKRIFTER OCHTILLVÄGAGÅNGSSÄTT (SE) ...............................................66

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The Kjeltec Auto 1002 Analyzer is designedfor laboratory use analyzing parameters asspecified in FOSS Tecators Application Notes.

The responsible body shall be made awarethat, if the equipment is used in a manner notspecified by the manufacturer, the protectionprovided by the equipment may be impaired.

Please read these operating instructionscarefully and act accordingly.

For safety reasons people not familiar withthese operating instructions must not use theinstrument.

In order to find out the nature of thepotential hazard, please consult this manualin all cases where this symbol is used.

Careful handling of the solutions used in ananalysis is mandatory for laboratory safety.Refer to the appropriate material safety datasheet for reagent handling instructions.Eye protection should be worn at all timesand care should be taken when handling hotdigestion tubes.

This device is equipped with agrounding/earthing type power plug for yourprotection against electrical shock hazardand should only be attached to a properlygrounded/earthed receptacle.

Before replacing the fuses, disconnectincoming mains supply.

Covers or panel(s) should be removed byqualified personnel only.

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Terminals identified by the symbol, bring thevarious parts of a system to the samepotential e.g. ground potential, whenconnected together. Note that such a terminalmust not be used as a protective earth(ground) connection.

Modifications, alterations, rebuilding or useof safety parts not authorized by FOSSTecator AB violates the warranty. FOSSTecator AB has no responsibility for damages,material or personal, occuring as a result ofsuch actions.

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2 INTRODUCTION

The 1002 Distilling Unit is part of the Kjeltec System I. Togetherwith the 2006 Digestion System and a Titration Unit, officialdeterminations of nitrogen / protein according to the Kjeldahlmethod, can be performed.

The 1002 Distilling Unit is a convenient and safe instrument forrapid steam distillations. One of the main applications for the unitis the distillation of “Kjeldahl digests” where the alkali isconveniently added via a built in dispensing system. The distillateis collected in a Receiver flask for subsequent titration.

Many other distillations can be performed efficiently with the1002 Distilling unit. These include Sulphur dioxide, Cyanide,Phenol, Alkaline Direct Distillation and Alcohol. Ask your FOSSTecator AB representative for a copy of our extensive applicationlist.

2.1 Performance Data

Distilling time 4-5 min

Distillation capacity Approximately 10 samples perhour

Measuring range 1-160 mg

Reproducibility � 1 % relative

Recovery 99,5-100,5 %

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1002003A

Fig. 1 A complete Kjeldahl system.

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3 FUNCTION

3.1 Principle of Operation

A typical Kjeldahl distillation is described. Other reagents mightbe used in other analyses. Use figure 2 to identify the parts. A testtube (Pos. 2) with digested sample, diluted with 75 ml distilled ordeionised water, is connected to the splash head (Pos. 3). Alkali ispumped (Pos. 1) into the test tube when the alkali handle on thefront panel is pulled down. The distillation is started by openingthe steam valve (Pos 7), pushing the steam control handle on thefront panel, marked STEAM, in the OPEN (down) position. Theliberated Ammonia goes, together with steam, through the splashhead (Pos.3) and is cooled in the condenser (Pos. 10) andcollected in the receiver flask (Pos. 11).

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WASTE

ALKALI

TANK

COOLING WATER

INLETSTEAMGEN

DRAINVALID FROM SERIAL NO 5400

1002014A

Fig. 2 1. Alkali pump 2. Test tube 3. Splash head 4. Steam generator 5. Level pins 6. Over heat protector 7. Steam valve8. Double valve for cooling water and water for steam production 9. Drain valve (steam generator)

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3.2 Steam Generation

By opening the steam valve on the front panel, power is connectedto the heater in the steam generator (Pos.4), the cooling waterinlet valve opens, and the distillation starts. The steam generatormust contain a certain volume of water to operate. The correctwater level in the steam generator is automatically controlled bylevel pins (Pos. 5).

When the steam valve is closed, boiling continues for about 10seconds in the steam generator. The excess steam goes to drain viathe waste tubing. At the same time the cooling water is switchedoff automatically. No overpressure can develop. The generator iseither connected to the test tube or to drain. In addition there is asafety valve on the steam generator if for any reason the steamoutlet is blocked.

3.3 Alkali System

Make sure that the test tube is empty and in its proper position.Pull down the handle for dispensing alkali (Fig. 8) several times,until alkali flows into the test tube. Then press the handle rapidlyall the way down 3 - 4 times to remove all the air from the system.Always let the handle return to its upper position by itself. Onestroke will give approximately 50 ml of alkali. See themaintenance section, how to change the volume.

In some applications other reagents may be added usingthe alkali system. e.g. H2SO4, H3PO4.

Note: The flowscheme shows a system using tap water feedfor the steam generator. The water supply should beammonia free to keep blank values at a minimum. If distilledor deionised water is used a direct feed water system mustbe fitted. (Contact your FOSS Tecator AB representative).

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4 PREPARATIONS FOR USE

4.1 Unpacking and Checking

Unpack the 1002 Distilling Unit and its accessories with care.Remove all packing material.

Remove the plastic caps covering the outlets on the rear of theinstrument. Use a pair of pliers if necessary.

Use the parts list, packed together with the instrument and checkthat you have received all parts. Use Fig. 3 and 4 to identify thedifferent parts. If any parts are missing, contact your FOSSTecator AB representative.

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7956

1002004A

Fig. 3 1. Distilling unit 2. Alkali tank 3. PVC Tubing for drain 4. Handle 5. Tubing clamps for water tubing 6. Tubingclamps for alkali tubing 7. Reinforced PVC Tubing for alkali 8. Nipple 9. Reinforced tubing for water(with integralconnectors)

1002005A

1

2

3

4

5

6

7

Fig. 4 1. Manual 2. Dispensing stops 3. Rubber adapter, semi-micro 4. Rubber adapter, macro 5. Digestion tube 250 ml6. Reciever flask (set of 8) 7. Funnel

Page 13: 1002 Kjeltec Manual

4.2 Installation

4.2.1 Installation Requirements

Power supply 220-240 V, 50-60 Hz

Power consumption 1900 W

Water supply 1 l/min tap water at 20° C

Water pressure (max) 5 bar

Dimensions LxDxH 30x36x80 cm

Weight 25 kg

4.2.2 Fuses

External: One fuse T 10 A

Internal: One fuse F 125 mA andone fuse T 500 mA

4.2.3 Installation Instructions

Place the 1002 Distilling Unit close to a coldwater tap and appropriate power supply whichshould be grounded.The connections are: brown wire-line, bluewire-neutral and green/yellow-protectiveearth.

a)Place the alkali tank on the floor besidethe distilling unit.

b)Direct the waste tubing into the sink. Makesure that the outlet is not below the waterlevel in the sink.

c)Connect the alkali tubing from the alkalitank to the nipple labelled “ALKALI”(Fig.5). Secure with tubing clamps (Fig.6).Fill the alkali tank with sodium hydroxideprepared as described in the ApplicationNote AN 300.

d)Screw the black plastic nipple suppliedinto the DRAIN outlet, put a piece of tubingon the nipple and direct it into the sink.

e)Connect the reinforced tubing with integralconnectors to the cooling water inlet (Fig.7) and to the water tap using threadsealing tape if necessary. If you do nothave a threaded tap, cut the metal connectoroff one end of the tubing and secure thetubing to the tap with the tubing clampprovided.

f)Connect the distilling unit to the powersupply.

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1002006A

6 7543

21

Fig. 5 Connections left to right.1. Steam waste tubing 2. Cooling waterinlet 3. Steam generator drain 4. Water tank(for direct feed water systems only)5. Alkali inlet 6. Electric power cable7. Equipotential connector

1002006B

Fig. 6 Use tubing clamps to securetubings.

1002006C

Fig. 7 Water connection.

Page 14: 1002 Kjeltec Manual

g)Do the start up procedure according to 5.2and check that the temperature of thecondensate is below 25 - 30°C. If not,increase the flow of the cooling waterstepwise.Mark the cooling water tap in order to givethe same flow at all times.

4.3 Functional Verification

4.3.1 Testing Recovery

Please refer to Application Note 300 suppliedwith your system, section chemical check.

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5 OPERATION

5.1 Identification of ControlsThese are identified in Figure 8.1. Power switch2. Timer3. Steam control

UP CLOSEDDOWN OPEN

4. Alkali handle5. Safety door

5.2 Starting Upa)Check the level of alkali in the tank. Fill

up if necessary.

b)Make sure that a test tube and a receiverflask are placed in their proper positionsand that the safety door is closed.

c)Switch on the power.

d)Turn on the cold water tap

Note: The water for the condenser and steam generator willnot flow until the steam valve is in the open position withthe power on. It will stop automatically when the valve isclosed.

e)Open the valve for steam by pushing thesteam control handle on the front panel indown position (Fig. 9).

After a couple of minutes steam isgenerated. Let the distillation continueuntil some water is collected in thereceiver flask. The system is then heatedup.

g)If the platform with the receiver flask isin the upper position (Fig. 10), move it tothe lower position. Close the steam valve onthe front panel.

5.3 Distillationa)Remove the test tube and the receiver flask.

b)Place the tube with the first diluted Sampleto be distilled in its position and placethe receiver flask with the receiversolution on the platform. To avoidcontamination don’t touch the glass outlettube with your fingers. Hold it by itsplastic tubing if necessary.

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1002007A

1 2 3 4

5

Fig. 8 1. Power switch; 2. Timer;3. Steam control; 4. Alkali handle; 5. Safetydoor.

1002007B

Fig. 9

1002007C

Fig. 10

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c)Close the safety door.

d)Move the platform for the receiver flask toits upper position.

e)Gently pull the alkali handle all the waydown to dispense about 50 ml of alkali (Fig8).

f)Open the steam control and set the timer tothe appropriate distilling time (around 4minutes).

g)Lower the platform for the receiver flaskand continue distillation for a few moreseconds to rinse the outlet tip.Close the steam control.

h)Replace the test tube and the receiver flaskwith the next set and continue in the samemanner with all the samples. When removing atube, the teflon pipe through which thesteam enters the sample, should be placed inthe slot of the plastic holder (Fig. 11).This makes it possible to replace a tubewithout touching the teflon pipe which willhave traces of alkali on it.

5.4 Closing Downa)Do the daily maintenance according to

chapter 6.

b)Pull out the drain collector (Fig. 12) underthe tube holder and the platform for thereceiver flask and clean it with water.Wipe the instrument clean from anyspillage.

c)Switch off the power and close the watertap.

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1002008A

Fig. 11 Resting position for the teflontube

1002013A

Fig. 12

Page 17: 1002 Kjeltec Manual

6 MAINTENANCE

This text is also avaliable as an instruction 10006458 whichincludes Maintenance Record Charts to facilitate a record of youractions.

6.1 DailyTo avoid start up problems and to prolong thelifetime of your system the proceduresdescribed in this chapter should be performedevery day the unit is used.

6.1.1 Cleaning Cycle

Connect a test tube half filled with distilledwater and a receiver flask into theirpositions. Open the valve for steam and distilfor 3 minutes, in order to avoid chemicalresidues to remain in the lower part of thesplash head.

6.1.2 Cleaning of Unit

Clean the whole unit from any spillage with adamp cloth or sponge.

6.1.3 Rubber Adapter

Clean the adapter from all remaining residueswith a damp cloth or sponge, use warm water.Also clean the splash shield from residues.

6.2 WeeklyIn addition to the daily routines outlinedabove, the following procedures should beperformed on a weekly basis, or as the needarises. Use the Weekly Maintenance RecordChart provided to keep a record of theseoperations.

6.2.1 Reagent Tanks Inspection and Cleaning

Check the tanks for: Signs of cracks orsplitting. Replace the tank if damaged.Crystals blocking the air holes in the screwcap. To remove any crystals wash the screw capin clean warm water until the crystals aredissolved, dry and replace.

6.2.2 Digestion Tubes Inspection

Check the rims of the digestion tubes foruneven surface,cracks and chips. This type ofdamage can cause leakage between the tube andthe rubber adapter leading to loss of recoveryduring analysis. Look for scratches and starfractures on the base of the tubes. These canlead to untimely and unexpected breakages

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creating a safety hazard to you and yourcolleagues and potential damage to yourdigestion or distillation unit.

Discard all damaged tubes in the interest ofsafety.

After some digestions the base of the tubesmay take on an off-white to greyishcoloration. This is quite normal and does notrequire the tubes to be replaced.

6.2.3 Cleaning the Safety Door

Clean the safety door from any spillage witha damp cloth or sponge.

6.3 Every One to Three MonthsIn addition to the routines outlined above thefollowing procedures should be performedevery one to three months, or as the needarises, depending on usage. Use theMaintenance Record Chart provided with theinstruction to keep a record of theseoperations.

Important!

If the rear panel is removed, there is a grounding cable(yellow/green) connected inside between the rear panel andthe main cabinet (lower right corner). Be sure to reconnectwhen replacing the panel.

6.3.1 Controlling the Rubber Adapter

Remove the rubber adapter from the unit andinspect it for scratches and cracks. Note alsoif the rubber of the adapter has started tolose it softness. If the adapter show signs ofscratches, cracks or that the rubber hasstarted to lose its softness the adapter hasto be changed.

6.3.2 Controlling the Alkali Volume

� Connect an empty test tube to the unit.Mark the wanted volume with a pen on thetube. Alternatively, the content can bepoured in a measuring cylinder.

� Close the safety door.

� Switch on power.

� Gently pull the handle all the way down todispense the alkali.

� Check the volume a couple of times. Theamount of alkali is set to about 50 ml fromthe factory. This volume can be reduced by

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Fig. 13

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putting dispensing stops in the slot belowthe alkali dispensing handle. Turn them 90°to fix them in position fig.13.

� After any adjustment, check the volumeagain.

6.3.3 Cleaning the Alkali Pump.

Put approximately two litres of warm, 40°C,distilled water in a beaker and connect it tothe system.Pump about half a litre of thewater through the alkali pump by pressing thealkali handle. This procedure requires thatthe tube is emptied when about 200 ml has beendispensed. Replace the tube and continue theflushing.

6.3.4 Cleaning of the Splash Head

Pour about 25 ml of water and the same amountof concentrated acetic acid into a test tubeand distil for 5 to 10 minutes. Replace thetube with a clean tube and continue to distilfor another 5 minutes. Repeat this at leastthree times so no acid residues will interferewith the analysis.

6.3.5 Depending on Number of Analyses

The frequency with which you should carry outthe procedures in this chapter depends upon anumber of factors which are outside FOSSTecator AB’s control and are thereforedifficult to predict. In simple terms you willhave to judge the required frequency byphysically checking the situation in eachcase. To a large extent the frequency willdepend on two major points.

1.The quality of the water used for steamgeneration. For example tap water willcreate more or less salt deposits dependingon its hardness. If deionised water isused,cleaning will rarely be necessary, butplease remember that a certain level ofconductivity is required for correctoperation of the level pins (See troubleshooting)

2.How well you have followed the guidelines inthe first three chapters of this text.Regular and immediate cleaning of splashesand spillage will create less problems.Routine checking of connectors when thereagents are replaced will limit thelikelihood of leakages.

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6.3.6 Cleaning of the Steam Generator

Disconnect the power supply. Open the drainvalve for the generator. When empty, fill upthe generator with a solution of 100 g citricacid in 800 ml water, preferable hot, byconnecting the funnel to the steam generatordrain. Suspend the funnel so that is in higherposition than the steam generator. Close thedrain valve, whilst the funnel is stillsuspended above the steam generator.

Alternative 1.Leave the solution in the steamgenerator overnight, or until the generatorvessel is free from deposits.

Alternative 2.Connect the power supply. Placea distillation tube and a receiver flask intheir positions and close the safety door.Switch on power and open the steam valve. Letthe citric acid solution boil for about fiveminutes. Close the steam valve and disconnectthe power supply.

CautionIf Alternative 2 has been chosen the solution will beextremely hot!

Open the drain valve and empty the steamgenerator.Rinse the generator thoroughly with waterusing the funnel again. When the vessel isclean and rinsed, close the drain valve.Remove the funnel and put the drain tubingoutlet back to its normal position.

6.3.7 Every Year

Your local distributor offers ServiceAgreements in order to make your instrumentreliable in performance and safety.

As a minimum of care all tubings andconnectors should be inspected. Exchange ifvisible damages can be seen.

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7 TROUBLE SHOOTING

FAULT PROBABLECAUSE

CORRECTIVEMEASURE

A. Lamp in mainswitch does not litup.

No current to theunit.

Faulty lamp and/orswitch.

Check power supply.

Call service.

B. Alkali is notdispensed.

Alkali tank is empty.

Crystals on sealingvalves.

Fill up the tank.

Read Maintenacesection Clean Alkalipump.

C. No cooling water. No cooling water on.

Sieve in the coolingwater inlet clogged.

Double valve faulty.

No water in thesteam generator.

Turn on the watertap.

Rinse the sieve.

Call service.

See below.

D. No water in thesteam generator.

No cooling water on.

Sieve in the coolingwater inlet clogged.

Double valve faulty.

Turn on the watertap.

Rinse the sieve.

Call service.

E. No steam isgenerated.

Not enough water inthe steamgenerator.

Steam valve faulty ifsteam comes troughthe waste tubing,when steam is on.

No current toheater.

Check that the drainvalve is closed.Check level pinposition.

Call service.

Check the overheatprotector. Reset ifneccessary accordingto fig 14. If this isnot solving theproblem call service.

F. Steam generatoris overfilling.

(Direct Feed WaterSystems only.)

Non return valve forsteam or drainfaulty.

No conductivity inthe waterpreventingactivation of levelpins if distilledwater is used.

Call service.

Add 0,5 g Na2SO4 towater tank. Do notuse Borax or SodiumSulphate as this maycause foaming.

G. Temperature ofthe distillate above30°C

Too low water flowthrough condenser,or too high watertemperature.

Adjust water flow oruse water suppliedvia a chilling unit.

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Fig. 14 To reset the overheat protectorinsert a screwdriver in the hole and pressuntil you hear a clicking sound

Page 22: 1002 Kjeltec Manual

FAULT PROBABLECAUSE

CORRECTIVEMEASURE

H. Incorrectanalytical results (too high or too low)

Sample preparation

Titrantconcentration

Leakage.

Alkali volume toolow.

Distillatetemperature toohigh.

Water for steamproduction containsexcessive or variableamounts ofammonia.

Check weighing andthe whole digestionprocedure.

Standarise titrant.Check distillation &titration cycle bydistilling knownamounts ofammonium salts. Seetesting recovery.

Check tubings andthe rubber adapter.Test recovery.

Read maintenancesection.

See G above.

Use distilled ordeionized water.*

I. Other undefinedor unspecifiedproblems

Chemistry/application. Over 95% ofproblems are relatedto the chemistry ofcustomers specificapplications.

Systemsmalfunctions notmentioned above.

Contact your FOSSTecator ABrepresentative.

Contact your FOSSTecator ABrepresentative.

* This requires the fitting of a direct Feed Water System and mustbe carried out at the factory or by a certified FOSS Tecator ABservice engineer in your laboratory.

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8 FOSS Tecator ABAPPLICATION NOTESSYSTEM

For information about preparation of chemicals and the Kjeldahlmethod please see the Application Note AN 300 supplied withyour system.

In FOSS Tecator ABs extensive list of Application Sub Notes youwill find information on how to analyse the sample of yourchoice. Please contact your FOSS Tecator AB representative formore details.

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9 TECHNICALSPECIFICATIONS

9.1 SafetyThe insulation of external, inaccessiblecircuits is reinforced.

9.2 Environmental ConditionsThe equipment is designed to be safe at leastunder the following conditions:

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Page 25: 1002 Kjeltec Manual

� Indoor use

� Altitude up to 2000 m.

� Temperature 5°C to 40°C.

� Maximum relative humidity 80% fortemperatures up to 31°C decreasing linearlyto 50% relative humidity at 40°C.

� Mains supply voltage fluctuations notexeeding � 10% of the rated voltage.

� Transient overvoltage is according tocategory II, which is normal for this typeof equipment.

� Pollution degree 2

9.3 Storage and Transport

9.3.1 Lifting Instructions 1002

This instrument is not equipped with handlesor grips. Two persons are needed to lift theinstrument, following the instructions below:

1. Tilt the instrument slightly backwards,and lift and support the instrument asshown in fig.16 to simplify and ensure asafe lift.

2. Weight 25 kg.

CautionAvoid getting your fingers pinched!

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Fig. 16

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10 ACCESSORIES ANDSPARE PARTS

10.1 Accessories

1000 0164 Receiver Flasks, 250 ml (set of 8)1000 0427 Basket for handling of 12 receiver flasks1002-020 Titration Unit, complete, DIGITRATE 50 ml

capacity1000 0347 Kjeltec DD KIT Comprising:

2ea 1000-0787 Distilling Tubes 750 1 (set of 6)1ea 1000-2049 Stand for 12 DD tubes2ea 1000-0439 Receiver flasks set of 61ea 1000-0427 Basket for 12 Flask1ea Application Note

10.2 Spare Parts

1000 0299 Condenser with insulation1000 0725 Splash Head, complete1000 0056 Adapter for test tubes 250 ml1000 0487 Adapter for test tubes 100 ml1000 0593 Alkali Tank1582 0002 Tubing for steam ¢ 8/12 m m, per m1582 0004 Tubing for drain, ¢ 8/11 mm, per m1569 0010 Tubing Strip1577 0007 Set of 2 Valves for alkali reagent dispenser1579 0005 Timer1000 2720 Glass Vessel for steam generator1000 2762 Rubbler Seal for steam generator1000 3504 Printed Circuit Board Complete1000 3505 Heater Coil including cover for steam generator,

230 V / 1600 W1000 3743 Steam valve complete

1575 0025 Double Solenoid Valve for coolingwater, 230V1564 0082 Fuse F 125 mA1564 0043 Fuse T 500 mA1564 0006 Fuse T10 A

1582 0066 Water tubing with integral connectors1563 0117 Reed relay switch1582 0011 Tubing for alkali 8/13-5 reinforced

10.3 Kjeltabs

Mercury tablets are delivered in boxes of 500, all other types inboxes of 1000.

15270001 Selenium, tablets with 1,5 g K2SO4 + 7,5 mg Se

15270002 Selenium, tablets with 5 g K2SO4 + 5 mg Se

15270003 Selenium, tablets with 3,5 g K2SO4 + 3,5 mg Se

15270004 Mercury, tablets with 3,5 g K2SO4 + 175 mg HgO

15270010 CT, tablets with 5 g K2SO4 + 0,15 g CuSO4 x 5 H2O +0,15 g TiO2

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Page 27: 1002 Kjeltec Manual

15270018 Copper, tablets with 3,5 g K2SO4 + 400 mg CuSO4 x 5H20

15270020 CT, tablets with 3,5 g K2SO4 + 0,105 g CuSO4 x 5 H2O +0,105 g TiO2

15270033 Mercury, tablets with 1,5 g K2SO4 + 7.5 mg HgO

15270034 Copper, tablets with 1,5 g K2SO4 + 150 mg CuSO4 x 5H20

15270048 Mercury, tablets with 3,5 g K2SO4 + 175 mg HgO

15270056 NAS, tablets with 1 g Na2SO4 + 0,05 g Se

15270057 KPC, tablets with 4,5 g K2SO4 + 0,5 g CuSO4 x 5 H2O

15270058 Special (AB24), tablets with 1,65 g K2SO4 + 0,33 gCuSO4 x 5 H2O + 0,0165 g Se

15270059 Special (AB22), tablets with 4,75 g K2SO4 + 0,075 gCuSO4 x 5 H2O + 0,10 g Se

15270060 Antifoam (AA00), tablets with 0,966 g Na2SO4 + 0,029g silicon + 0,005g Si

15270061 Auto CT (AA22), tablets with 1,5 g K2SO4 + 0,045 gCuSO4 x 5 H2O + 0,045 g TiO2

15270062 Special (AB64), tablets with 5,0 g K2SO4 + 0,06 g Se

15270063 KS (AA47), tablets with 4,95 g K2SO4 + 0,05 g Se

15270065 K/5 (AA23), tablets with 5 g K2SO4

Other types are available upon request. However, those listedabove represent more than 90% of the catalyst tablets usedworldwide.

10.4 Manufacturer’s Name and Address

FOSS Tecator ABBox 70SE-263 21 HöganäsSweden

Int phone. +46 42 361500Int fax. +46 42 340349

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Page 30: 1002 Kjeltec Manual

c) Switch on the power.

d) Turn on the cold water tap

Note: The water for the condenser andsteam generator will not flow until thesteam valve is in the open positionwith the power on. It will stopautomatically when the valve is closed.

e) Open the valve for steam by pushing thesteam control handle on the front panel indown position (Fig. 9).

After a couple of minutes steam isgenerated. Let the distillation continue untilsome water is collected in the receiver flask.The system is then heated up.

g) If the platform with the receiver flask is inthe upper position (Fig. 10), move it to thelower position. Close the steam valve on thefront panel.

11.4.3 Distillation

a) Remove the test tube and the receiver flask.

b) Place the tube with the first diluted Sampleto be distilled in its position and place thereceiver flask with the receiver solution onthe platform. To avoid contamination don’ttouch the glass outlet tube with your fingers.Hold it by its plastic tubing if necessary.

c) Close the safety door.

d) Move the platform for the receiver flask toits upper position.

e) Gently pull the alkali handle all the waydown to dispense about 50 ml of alkali (Fig8).

f) Open the steam control and set the timer tothe appropriate distilling time (around 4minutes).

g) Lower the platform for the receiver flaskand continue distillation for a few moreseconds to rinse the outlet tip.Close the steam control.

h) Replace the test tube and the receiver flaskwith the next set and continue in the samemanner with all the samples. Whenremoving a tube, the teflon pipe through

which the steam enters the sample, shouldbe placed in the slot of the plastic holder(Fig. 11). This makes it possible to replace atube without touching the teflon pipe whichwill have traces of alkali on it.

11.4.4 Closing down

a) Do the daily maintenance according tochapter 11.5.

b) Pull out the drain collector (Fig. 12) underthe tube holder and the platform for thereceiver flask and clean it with water. Wipethe instrument clean from any spillage.

c) Switch off the power and close the watertap.

11.5 Maintenance

This text is also avaliable as an instruction10006458 which includes Maintenance RecordCharts to facilitate a record of your actions.

11.5.1 Daily

To avoid start up problems and to prolong thelifetime of your system the procedures describedin this chapter should be performed every daythe unit is used.

11.5.1.1 Cleaning cycle

Connect a test tube half filled with distilledwater and a receiver flask into their positions.Open the valve for steam and distil for 3minutes, in order to avoid chemical residues toremain in the lower part of the splash head.

11.5.1.2 Cleaning of unit

Clean the whole unit from any spillage with adamp cloth or sponge.

11.5.1.3 Rubber adapter

Clean the adapter from all remaining residueswith a damp cloth or sponge, use warm water.Also clean the splash shield from residues.

11.5.2 Weekly

In addition to the daily routines outlined above,the following procedures should be performedon a weekly basis, or as the need arises. Use theWeekly Maintenance Record Chart provided tokeep a record of these operations.

11.5.2.1 Reagent tanks inspectionand cleaning

Check the tanks for: Signs of cracks or splitting.Replace the tank if damaged. Crystals blockingthe air holes in the screw cap. To remove anycrystals wash the screw cap in clean warm wateruntil the crystals are dissolved, dry and replace.

11.5.2.2 Digestion tubes inspection

Check the rims of the digestion tubes for unevensurface,cracks and chips. This type of damagecan cause leakage between the tube and therubber adapter leading to loss of recovery duringanalysis. Look for scratches and star fractures onthe base of the tubes. These can lead to untimelyand unexpected breakages creating a safetyhazard to you and your colleagues and potentialdamage to your digestion or distillation unit.

Discard all damaged tubes in the interest ofsafety.

After some digestions the base of the tubes maytake on an off-white to greyish coloration. Thisis quite normal and does not require the tubes tobe replaced.

11.5.2.3 Cleaning the safety door

Clean the safety door from any spillage with adamp cloth or sponge.

11.5.3 Every one to three months

In addition to the routines outlined above thefollowing procedures should be performed everyone to three months, or as the need arises,

depending on usage. Use the MaintenanceRecord Chart provided with the instruction tokeep a record of these operations.

Important!

If the rear panel is removed, there is agrounding cable (yellow/green)connected inside between the rearpanel and the main cabinet (lowerright corner). Be sure to reconnectwhen replacing the panel.

11.5.3.1 Controlling the rubberadapter

Remove the rubber adapter from the unit andinspect it for scratches and cracks. Note also ifthe rubber of the adapter has started to lose itsoftness. If the adapter show signs of scratches,cracks or that the rubber has started to lose itssoftness the adapter has to be changed.

11.5.3.2 Controlling the alkalivolume

� Connect an empty test tube to the unit.Mark the wanted volume with a pen on thetube. Alternatively, the content can bepoured in a measuring cylinder.

� Close the safety door.

� Switch on power.

� Gently pull the handle all the way down todispense the alkali.

� Check the volume a couple of times. Theamount of alkali is set to about 50 ml fromthe factory. This volume can be reduced byputting dispensing stops in the slot belowthe alkali dispensing handle. Turn them 90°to fix them in position fig. 13.

� After any adjustment, check the volumeagain.

1002 Kjeltec� System, User Manual, Rev. 2.3, Part no 1000 1535, FOSS Tecator AB, Sweden 24

Page 31: 1002 Kjeltec Manual

11.5.3.3 Cleaning the alkali pump.

Put approximately two litres of warm, 40°C,distilled water in a beaker and connect it to thesystem.Pump about half a litre of the waterthrough the alkali pump by pressing the alkalihandle. This procedure requires that the tube isemptied when about 200 ml has been dispensed.Replace the tube and continue the flushing.

11.5.3.4 Cleaning of the splashhead

Pour about 25 ml of water and the same amountof concentrated acetic acid into a test tube anddistil for 5 to 10 minutes. Replace the tube witha clean tube and continue to distil for another 5minutes. Repeat this at least three times so noacid residues will interfere with the analysis.

11.5.4 Depending on number ofanalyses

The frequency with which you should carry outthe procedures in this chapter depends upon anumber of factors which are outside FOSSTecator AB’s control and are therefore difficultto predict. In simple terms you will have tojudge the required frequency by physicallychecking the situation in each case. To a largeextent the frequency will depend on two majorpoints.

1. The quality of the water used for steamgeneration. For example tap water willcreate more or less salt deposits dependingon its hardness. If deionised water isused,cleaning will rarely be necessary, butplease remember that a certain level ofconductivity is required for correctoperation of the level pins (See troubleshooting)

2. How well you have followed the guidelinesin the first three chapters of this text.Regular and immediate cleaning of splashesand spillage will create less problems.Routine checking of connectors when thereagents are replaced will limit thelikelihood of leakages.

11.5.4.1 Cleaning of the steamgenerator

Disconnect the power supply. Open the drainvalve for the generator. When empty, fill up thegenerator with a solution of 100 g citric acid in800 ml water, preferable hot, by connecting thefunnel to the steam generator drain. Suspend thefunnel so that is in higher position than thesteam generator. Close the drain valve, whilstthe funnel is still suspended above the steamgenerator.

Alternative 1.Leave the solution in the steamgenerator overnight, or until the generator vesselis free from deposits.

Alternative 2.Connect the power supply. Place adistillation tube and a receiver flask in theirpositions and close the safety door. Switch onpower and open the steam valve. Let the citricacid solution boil for about five minutes. Closethe steam valve and disconnect the powersupply.

CautionIf Alternative 2 has been chosen thesolution will be extremely hot!

Open the drain valve and empty the steamgenerator.Rinse the generator thoroughly with water usingthe funnel again. When the vessel is clean andrinsed, close the drain valve. Remove the funneland put the drain tubing outlet back to its normalposition.

11.5.5 Every Year

Your local distributor offers Service Agreementsin order to make your instrument reliable inperformance and safety.

As a minimum of care all tubings and connectorsshould be inspected. Exchange if visibledamages can be seen.

� TROUBLE SHOOTING* This requires thefitting of a direct Feed Water System andmust be carried out at the factory or by acertified FOSS Tecator AB service engineerin your laboratory.

For information about preparation of chemicalsand the Kjeldahl method please see theApplication Note AN 300 supplied with yoursystem.

In FOSS Tecator ABs extensive list ofApplication Sub Notes you will find informationon how to analyse the sample of your choice.Please contact your FOSS Tecator ABrepresentative for more details.

11.6 Technicalspecifications

11.6.1 Safety

The insulation of external, inaccessible circuitsis reinforced.

11.6.2 Environmental conditions

The equipment is designed to be safe at leastunder the following conditions:

� Indoor use

� Altitude up to 2000 m.

� Temperature 5°C to 40°C.

� Maximum relative humidity 80% fortemperatures up to 31°C decreasing linearlyto 50% relative humidity at 40°C.

� Mains supply voltage fluctuations notexeeding � 10% of the rated voltage.

� Transient overvoltage is according tocategory II, which is normal for this type ofequipment.

� Pollution degree 2

11.7 Storage & transport

11.7.1 Lifting instructions 1002

This instrument is not equipped with handles orgrips. Two persons are needed to lift theinstrument, following the instructions below:

1. Tilt the instrument slightly backwards, andlift and support the instrument as shown infig.16 to simplify and ensure a safe lift.

2. Weight 25 kg.

Caution!Avoid getting your fingers pinched!

11.8 Explanations toillustrations

Fig 5Connections left to right.1. Steam waste tubing2. Cooling water inlet3. Steam generator drain4. Water tank (for direct feed water systemsonly)5. Alkali inlet6. Electric power cable7. Equipotential connector

Fig 6Use tubing clamps to secure tubings.

Fig 7Water connection.

Fig 81. Power switch2. Timer3. Steam control4. Alkali handle5. Safety door.

Fig 11Resting position for the teflon tube.

1002 Kjeltec� System, User Manual, Rev. 2.3, Part no 1000 1535, FOSS Tecator AB, Sweden 25