1002 Kjeltec Manual

™

Kjeltec 1002 System Distilling Unit User Manual 1000 1535 / Rev. 2.3

1002001A

Copyright 2003 / All rights reserved FOSS Tecator AB, Box 70, SE-26321 Höganäs, Sweden Tel Int +46 42 361500, Fax +46 42 343150

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

Dansk

1

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Deutsch

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English

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

Nederlands

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

Table of Contents 1

SAFETY PRECAUTIONS AND PROCEDURES

1.1 1.2

Intended Use .............................................................................................1 Safety Precautions .................................................................................1

2

INTRODUCTION

2.1

Performance Data ..................................................................................3

3

FUNCTION

3.1 3.2 3.3

Principle of Operation .........................................................................4 Steam Generation ..................................................................................5 Alkali System ............................................................................................5

4

PREPARATIONS FOR USE

4.1 4.2 4.2.1 4.2.2 4.2.3 4.3 4.3.1

Unpacking and Checking....................................................................6 Installation .................................................................................................7 Installation Requirements ...........................................................................7 Fuses .................................................................................................................7 Installation Instructions................................................................................7

5

OPERATION

5.1 5.2 5.3 5.4

Identification of Controls ..................................................................9 Starting Up .................................................................................................9 Distillation ..................................................................................................9 Closing Down ..........................................................................................10

6

MAINTENANCE

6.1 6.1.1 6.1.2 6.1.3 6.2 6.2.1 6.2.2 6.2.3 6.3 6.3.1 6.3.2 6.3.3 6.3.4 6.3.5 6.3.6 6.3.7

Daily..............................................................................................................11

7

Functional Verification .......................................................................8 Testing Recovery............................................................................................8

Cleaning Cycle ..............................................................................................11 Cleaning of Unit ..........................................................................................11 Rubber Adapter ...........................................................................................11

Weekly .......................................................................................................11 Reagent Tanks Inspection and Cleaning................................................11 Digestion Tubes Inspection .......................................................................11 Cleaning the Safety Door ..........................................................................12 Every One to Three Months............................................................12 Controlling the Rubber Adapter..............................................................12 Controlling the Alkali Volume .................................................................12 Cleaning the Alkali Pump..........................................................................13 Cleaning of the Splash Head ....................................................................13 Depending on Number of Analyses ........................................................13 Cleaning of the Steam Generator ...........................................................14 Every Year .....................................................................................................14

TROUBLE SHOOTING

8 9

FOSS Tecator AB APPLICATION NOTES SYSTEM TECHNICAL SPECIFICATIONS

9.1 9.2 9.3 9.3.1

Safety...........................................................................................................18 Environmental Conditions ..............................................................18 Storage and Transport ......................................................................19 Lifting Instructions 1002 ............................................................................19

10

ACCESSORIES AND SPARE PARTS

10.1 10.2 10.3 10.4

Accessories ...............................................................................................20 Spare Parts................................................................................................20 Kjeltabs .......................................................................................................20 Manufacturer’s Name and Address .........................................21

11 12

SAFETY PRECAUTIONS AND PROCEDURES ..........23 SICHERHEITS- UND BETRIEBSVORSCHRIFTEN (DE) 26

13 14 15 16

SIKKERHED - FORHOLDSREGLER OG PROCEDURER (DK) .............................................................................................................30 PRECAUCIONES Y PROCEDIMIENTOS DE SEGURIDAD (ES) ..............................................................................33 VAROTOIMET JA MENETELMÄT (FIN) ..........................37 PRESCRIPTIONS ET PROCEDURES DE SECURITE (FR)

17 18 19 20 21 22 23

ËÇØÇ ÌÅÔÑÙÍ ÁÓÖÁËÅÉÁÓ ÊÁÉ ÏÄÇÃÉÅÓ ×ÑÇÓÇÓ (GR) ..............................................................................................................44 ÖRYGGISREGLUR OG AÐFERÐIR (IS) .........................48 NORME PRECAUZIONALI E PROCEDURE DI SICUREZZA (IT) ...............................................................................51 VEILIGHEIDSMAATREGELEN EN PROCEDURES (NL) ..............................................................................................................55 SIKKERHETSREGLER OG PROSEDYRER (NO) ......59 PRECAUÇÕES E MEDIDAS DE SEGURANÇA (PT) ..............................................................................................................62 SÄKERHETSFÖRESKRIFTER OCH TILLVÄGAGÅNGSSÄTT (SE) ...............................................66

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

40

The Kjeltec Auto 1002 Analyzer is designed for laboratory use analyzing parameters as specified in FOSS Tecators Application Notes.

The responsible body shall be made aware that, if the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired.

Please read these operating instructions carefully and act accordingly. For safety reasons people not familiar with these operating instructions must not use the instrument.

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

Careful handling of the solutions used in an analysis is mandatory for laboratory safety. Refer to the appropriate material safety data sheet for reagent handling instructions. Eye protection should be worn at all times and care should be taken when handling hot digestion tubes.

This device is equipped with a grounding/earthing type power plug for your protection against electrical shock hazard and should only be attached to a properly grounded/earthed receptacle.

Before replacing the fuses, disconnect incoming mains supply.

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

Terminals identified by the symbol, bring the various parts of a system to the same potential e.g. ground potential, when connected together. Note that such a terminal must not be used as a protective earth (ground) connection.

Modifications, alterations, rebuilding or use of safety parts not authorized by FOSS Tecator AB violates the warranty. FOSS Tecator AB has no responsibility for damages, material or personal, occuring as a result of such actions.

2

INTRODUCTION

The 1002 Distilling Unit is part of the Kjeltec System I. Together with the 2006 Digestion System and a Titration Unit, official determinations of nitrogen / protein according to the Kjeldahl method, can be performed. The 1002 Distilling Unit is a convenient and safe instrument for rapid steam distillations. One of the main applications for the unit is the distillation of “Kjeldahl digests” where the alkali is conveniently added via a built in dispensing system. The distillate is collected in a Receiver flask for subsequent titration. Many other distillations can be performed efficiently with the 1002 Distilling unit. These include Sulphur dioxide, Cyanide, Phenol, Alkaline Direct Distillation and Alcohol. Ask your FOSS Tecator AB representative for a copy of our extensive application list.

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

2.1

Performance Data

Distilling time

4-5 min

Distillation capacity

Approximately 10 samples per hour

Measuring range

1-160 mg

Reproducibility

± 1 % relative

Recovery

99,5-100,5 %

1002003A

Fig. 1

A complete Kjeldahl system.

3

3

FUNCTION

3.1

Principle of Operation

A typical Kjeldahl distillation is described. Other reagents might be used in other analyses. Use figure 2 to identify the parts. A test tube (Pos. 2) with digested sample, diluted with 75 ml distilled or deionised water, is connected to the splash head (Pos. 3). Alkali is pumped (Pos. 1) into the test tube when the alkali handle on the front panel is pulled down. The distillation is started by opening the steam valve (Pos 7), pushing the steam control handle on the front panel, marked STEAM, in the OPEN (down) position. The liberated Ammonia goes, together with steam, through the splash head (Pos.3) and is cooled in the condenser (Pos. 10) and collected in the receiver flask (Pos. 11).

12

3

13 10 7

2 11

5

6

4

9 8 WASTE

COOLING WATER INLET

STEAMGEN DRAIN

ALKALI TANK

1002014A

VALID FROM SERIAL NO 5400

Fig. 2 1. Alkali pump 2. Test tube 3. Splash head 4. Steam generator 5. Level pins 6. Over heat protector 7. Steam valve 8. Double valve for cooling water and water for steam production 9. Drain valve (steam generator)

4

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

1

3.2

Steam Generation

By opening the steam valve on the front panel, power is connected to the heater in the steam generator (Pos.4), the cooling water inlet valve opens, and the distillation starts. The steam generator must contain a certain volume of water to operate. The correct water level in the steam generator is automatically controlled by level pins (Pos. 5). When the steam valve is closed, boiling continues for about 10 seconds in the steam generator. The excess steam goes to drain via the waste tubing. At the same time the cooling water is switched off automatically. No overpressure can develop. The generator is either connected to the test tube or to drain. In addition there is a safety valve on the steam generator if for any reason the steam outlet 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 rapidly all 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. One stroke will give approximately 50 ml of alkali. See the maintenance section, how to change the volume. In some applications other reagents may be added using the alkali system. e.g. H2SO4, H3PO4.

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

Note: The flowscheme shows a system using tap water feed for the steam generator. The water supply should be ammonia free to keep blank values at a minimum. If distilled or deionised water is used a direct feed water system must be fitted. (Contact your FOSS Tecator AB representative).

5

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 the instrument. Use a pair of pliers if necessary. Use the parts list, packed together with the instrument and check that you have received all parts. Use Fig. 3 and 4 to identify the different parts. If any parts are missing, contact your FOSS Tecator AB representative.

2

1

4 8

6

5

3

7

9

1002004A

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

5

1

2

6 4

3 1002005A

Fig. 4 1. Manual 2. Dispensing stops 3. Rubber adapter, semi-micro 4. Rubber adapter, macro 5. Digestion tube 250 ml 6. Reciever flask (set of 8) 7. Funnel

6

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

7

3 4 1

5 6 7

2

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

1002006A

Fig. 5 Connections left to right. 1. Steam waste tubing 2. Cooling water inlet 3. Steam generator drain 4. Water tank (for direct feed water systems only) 5. Alkali inlet 6. Electric power cable 7. Equipotential connector

4.2.2

Fuses

External: One fuse T 10 A Internal: One fuse F 125 mA and one fuse T 500 mA 4.2.3

Installation Instructions

Place the 1002 Distilling Unit close to a cold water tap and appropriate power supply which should be grounded. The connections are: brown wire-line, blue wire-neutral and green/yellow-protective earth. a)Place the alkali tank on the floor beside the distilling unit. b)Direct the waste tubing into the sink. Make sure that the outlet is not below the water level in the sink.

1002006B

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

Fig. 6 tubings.

Use tubing clamps to secure

c)Connect the alkali tubing from the alkali tank to the nipple labelled “ALKALI” (Fig.5). Secure with tubing clamps (Fig.6). Fill the alkali tank with sodium hydroxide prepared as described in the Application Note AN 300. d)Screw the black plastic nipple supplied into the DRAIN outlet, put a piece of tubing on the nipple and direct it into the sink.

1002006C

Fig. 7

Water connection.

e)Connect the reinforced tubing with integral connectors to the cooling water inlet ( Fig.7) and to the water tap using thread sealing tape if necessary. If you do not have a threaded tap, cut the metal connector off one end of the tubing and secure the tubing to the tap with the tubing clamp provided. f)Connect the distilling unit to the power supply.

7

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

4.3

Functional Verification

4.3.1

Testing Recovery

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

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

8

1

2

3

5

4

5.1

5 1002007A

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

OPERATION Identification of Controls

These are identified in Figure 8. 1. Power switch 2. Timer 3. Steam control UP CLOSED DOWN OPEN 4. Alkali handle 5. Safety door

5.2

Starting Up

a)Check the level of alkali in the tank. Fill up if necessary. b)Make sure that a test tube and a receiver flask are placed in their proper positions and 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 will not flow until the steam valve is in the open position with the power on. It will stop automatically when the valve is closed.

1002007B

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

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

Fig. 9

After a couple of minutes steam is generated. Let the distillation continue until some water is collected in the receiver flask. The system is then heated up. g)If the platform with the receiver flask is in the upper position (Fig. 10), move it to the lower position. Close the steam valve on the front panel.

5.3

Distillation

a)Remove the test tube and the receiver flask. 1002007C

Fig. 10

b)Place the tube with the first diluted Sample to be distilled in its position and place the receiver flask with the receiver solution on the platform. To avoid contamination don’t touch the glass outlet tube with your fingers. Hold it by its plastic tubing if necessary.

9

c)Close the safety door. d)Move the platform for the receiver flask to its upper position. e)Gently pull the alkali handle all the way down to dispense about 50 ml of alkali (Fig 8). f)Open the steam control and set the timer to the appropriate distilling time (around 4 minutes). g)Lower the platform for the receiver flask and continue distillation for a few more seconds to rinse the outlet tip. Close the steam control.

1002008A

Fig. 11

Resting position for the teflon

h)Replace the test tube and the receiver flask tube with the next set and continue in the same manner with all the samples. When removing a tube, the teflon pipe through which the steam enters the sample, should be placed in the slot of the plastic holder (Fig. 11). This makes it possible to replace a tube without touching the teflon pipe which will have traces of alkali on it.

5.4

Closing Down

a)Do the daily maintenance according to chapter 6. b)Pull out the drain collector (Fig. 12) under the tube holder and the platform for the receiver flask and clean it with water. Fig. 12 Wipe the instrument clean from any spillage.

1002013A

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

c)Switch off the power and close the water tap.

10

6

MAINTENANCE

This text is also avaliable as an instruction 10006458 which includes Maintenance Record Charts to facilitate a record of your actions.

6.1

Daily

To avoid start up problems and to prolong the lifetime of your system the procedures described in this chapter should be performed every day the unit is used. 6.1.1

Cleaning Cycle

Connect a test tube half filled with distilled water and a receiver flask into their positions. Open the valve for steam and distil for 3 minutes, in order to avoid chemical residues to remain in the lower part of the splash head. 6.1.2

Cleaning of Unit

Clean the whole unit from any spillage with a damp cloth or sponge. 6.1.3

Rubber Adapter

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

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

6.2

Weekly

In addition to the daily routines outlined above, the following procedures should be performed on a weekly basis, or as the need arises. Use the Weekly Maintenance Record Chart provided to keep a record of these operations. 6.2.1

Reagent Tanks Inspection and Cleaning

Check the tanks for: Signs of cracks or splitting. Replace the tank if damaged. Crystals blocking the air holes in the screw cap. To remove any crystals wash the screw cap in clean warm water until the crystals are dissolved, dry and replace. 6.2.2

Digestion Tubes Inspection

Check the rims of the digestion tubes for uneven surface,cracks and chips. This type of damage can cause leakage between the tube and the rubber adapter leading to loss of recovery during analysis. Look for scratches and star fractures on the base of the tubes. These can lead to untimely and unexpected breakages

11

creating a safety hazard to you and your colleagues and potential damage to your digestion or distillation unit. Discard all damaged tubes in the interest of safety. After some digestions the base of the tubes may take on an off-white to greyish coloration. This is quite normal and does not require the tubes to be replaced. 6.2.3

Cleaning the Safety Door

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

6.3

Every One to Three Months

In addition to the routines outlined above the following procedures should be performed every one to three months, or as the need arises, depending on usage. Use the Maintenance Record Chart provided with the instruction to keep a record of these operations. Important! If the rear panel is removed, there is a grounding cable (yellow/green) connected inside between the rear panel and the main cabinet (lower right corner). Be sure to reconnect when replacing the panel.

Controlling the Rubber Adapter

Remove the rubber adapter from the unit and inspect it for scratches and cracks. Note also if the rubber of the adapter has started to lose it softness. If the adapter show signs of scratches, cracks or that the rubber has started to lose its softness the adapter has to 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 the tube. Alternatively, the content can be poured in a measuring cylinder. Close the safety door. Switch on power. Gently pull the handle all the way down to dispense the alkali. Check the volume a couple of times. The amount of alkali is set to about 50 ml from the factory. This volume can be reduced by Fig. 13

12

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

6.3.1

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

·

After any adjustment, check the volume again.

6.3.3

Cleaning the Alkali Pump.

Put approximately two litres of warm, 40°C, distilled water in a beaker and connect it to the system.Pump about half a litre of the water through the alkali pump by pressing the alkali handle. This procedure requires that the tube is emptied when about 200 ml has been dispensed. Replace the tube and continue the flushing. 6.3.4

Cleaning of the Splash Head

Pour about 25 ml of water and the same amount of concentrated acetic acid into a test tube and distil for 5 to 10 minutes. Replace the tube with a clean tube and continue to distil for another 5 minutes. Repeat this at least three times so no acid residues will interfere with the analysis. 6.3.5

Depending on Number of Analyses

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

The frequency with which you should carry out the procedures in this chapter depends upon a number of factors which are outside FOSS Tecator AB’s control and are therefore difficult to predict. In simple terms you will have to judge the required frequency by physically checking the situation in each case. To a large extent the frequency will depend on two major points. 1.The quality of the water used for steam generation. For example tap water will create more or less salt deposits depending on its hardness. If deionised water is used,cleaning will rarely be necessary, but please remember that a certain level of conductivity is required for correct operation of the level pins (See trouble shooting) 2.How well you have followed the guidelines in the first three chapters of this text. Regular and immediate cleaning of splashes and spillage will create less problems. Routine checking of connectors when the reagents are replaced will limit the likelihood of leakages.

13

6.3.6

Cleaning of the Steam Generator

Disconnect the power supply. Open the drain valve for the generator. When empty, fill up the generator with a solution of 100 g citric acid in 800 ml water, preferable hot, by connecting the funnel to the steam generator drain. Suspend the funnel so that is in higher position than the steam generator. Close the drain valve, whilst the funnel is still suspended above the steam generator. Alternative 1.Leave the solution in the steam generator overnight, or until the generator vessel is free from deposits. Alternative 2.Connect the power supply. Place a distillation tube and a receiver flask in their positions and close the safety door. Switch on power and open the steam valve. Let the citric acid solution boil for about five minutes. Close the steam valve and disconnect the power supply.

Caution If Alternative 2 has been chosen the solution will be extremely hot! Open the drain valve and empty the steam generator. Rinse the generator thoroughly with water using the funnel again. When the vessel is clean and rinsed, close the drain valve. Remove the funnel and put the drain tubing outlet back to its normal position.

Every Year

Your local distributor offers Service Agreements in order to make your instrument reliable in performance and safety. As a minimum of care all tubings and connectors should be inspected. Exchange if visible damages can be seen.

14

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

6.3.7

7

TROUBLE SHOOTING

FAULT

PROBABLE CAUSE

CORRECTIVE MEASURE

A. Lamp in main switch does not lit up.

No current to the unit.

Check power supply. Call service.

Faulty lamp and/or switch. B. Alkali is not dispensed.

C. No cooling water.

Alkali tank is empty.

Fill up the tank.

Crystals on sealing valves.

Read Maintenace section Clean Alkali pump.

No cooling water on.

Turn on the water tap.

Sieve in the cooling water inlet clogged.

Rinse the sieve.

Double valve faulty. Call service. No water in the steam generator. D. No water in the steam generator.

Sieve in the cooling water inlet clogged.

1002018A

Fig. 14 To reset the overheat protector insert a screwdriver in the hole and press until you hear a clicking sound

Turn on the water tap. Rinse the sieve.

Double valve faulty. Call service. E. No steam is generated.

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

No cooling water on.

See below.

F. Steam generator is overfilling. (Direct Feed Water Systems only.)

G. Temperature of the distillate above 30°C

Not enough water in the steam generator.

Check that the drain valve is closed. Check level pin position.

Steam valve faulty if steam comes trough the waste tubing, when steam is on.

Call service.

No current to heater.

Check the overheat protector. Reset if neccessary according to fig 14. If this is not solving the problem call service.

Non return valve for steam or drain faulty.

Call service.

No conductivity in the water preventing activation of level pins if distilled water is used. Too low water flow through condenser, or too high water temperature.

Add 0,5 g Na 2 SO 4 to water tank. Do not use Borax or Sodium Sulphate as this may cause foaming.

Adjust water flow or use water supplied via a chilling unit.

15

FAULT

PROBABLE CAUSE

CORRECTIVE MEASURE

H. Incorrect analytical results ( too high or too low)

Sample preparation

Check weighing and the whole digestion procedure.

Titrant concentration

Standarise titrant. Check distillation & titration cycle by distilling known amounts of ammonium salts. See testing recovery.

Leakage.

Alkali volume too low.

Check tubings and the rubber adapter. Test recovery. Read maintenance section. See G above.

Distillate temperature too high.

Use distilled or deionized water.*

Water for steam production contains excessive or variable amounts of ammonia. I. Other undefined or unspecified problems

Chemistry/applicatio n. Over 95% of problems are related to the chemistry of customers specific applications.

Contact your FOSS Tecator AB representative.

Systems malfunctions not mentioned above.

Contact your FOSS Tecator AB representative.

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

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

16

8

FOSS Tecator AB APPLICATION NOTES SYSTEM

For information about preparation of chemicals and the Kjeldahl method please see the Application Note AN 300 supplied with your system.

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

In FOSS Tecator ABs extensive list of Application Sub Notes you will find information on how to analyse the sample of your choice. Please contact your FOSS Tecator AB representative for more details.

17

9 9.1

TECHNICAL SPECIFICATIONS Safety

The insulation of external, inaccessible circuits is reinforced.

9.2

Environmental Conditions

Fig. 15

18

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

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

· · · · · · ·

Indoor use Altitude up to 2000 m. Temperature 5°C to 40°C. Maximum relative humidity 80% for temperatures up to 31°C decreasing linearly to 50% relative humidity at 40°C. Mains supply voltage fluctuations not exeeding ± 10% of the rated voltage. Transient overvoltage is according to category II, which is normal for this type of equipment. Pollution degree 2

9.3

Storage and Transport

9.3.1

Lifting Instructions 1002

This instrument is not equipped with handles or grips. Two persons are needed to lift the instrument, following the instructions below: 1.

Tilt the instrument slightly backwards, and lift and support the instrument as shown in fig.16 to simplify and ensure a safe lift.

2.

Weight 25 kg.

Caution Avoid getting your fingers pinched!

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

1002017A

Fig. 16

19

ACCESSORIES AND SPARE PARTS

10.1

Accessories

1000 0164 1000 0427 1002-020

Receiver Flasks, 250 ml (set of 8) Basket for handling of 12 receiver flasks Titration Unit, complete, DIGITRATE 50 ml capacity Kjeltec DD KIT Comprising: 2ea 1000-0787 Distilling Tubes 750 1 (set of 6) 1ea 1000-2049 Stand for 12 DD tubes 2ea 1000-0439 Receiver flasks set of 6 1ea 1000-0427 Basket for 12 Flask 1ea Application Note

1000 0347

10.2

Spare Parts

1000 0299 1000 0725 1000 0056 1000 0487 1000 0593 1582 0002 1582 0004 1569 0010 1577 0007 1579 0005 1000 2720 1000 2762 1000 3504 1000 3505 1000 3743

Condenser with insulation Splash Head, complete Adapter for test tubes 250 ml Adapter for test tubes 100 ml Alkali Tank Tubing for steam ¢ 8/12 m m, per m Tubing for drain, ¢ 8/11 mm, per m Tubing Strip Set of 2 Valves for alkali reagent dispenser Timer Glass Vessel for steam generator Rubbler Seal for steam generator Printed Circuit Board Complete Heater Coil including cover for steam generator, 230 V / 1600 W Steam valve complete

1575 0025 1564 0082 1564 0043 1564 0006

Double Solenoid Valve for coolingwater, 230V Fuse F 125 mA Fuse T 500 mA Fuse T10 A

1582 0066 1563 0117 1582 0011

Water tubing with integral connectors Reed relay switch Tubing for alkali 8/13-5 reinforced

10.3

Kjeltabs

Mercury tablets are delivered in boxes of 500, all other types in boxes of 1000. 15270001

Selenium, tablets with 1,5 g K 2 SO 4 + 7,5 mg Se

15270002

Selenium, tablets with 5 g K 2 SO 4 + 5 mg Se

15270003

Selenium, tablets with 3,5 g K 2 SO 4 + 3,5 mg Se

15270004

Mercury, tablets with 3,5 g K 2 SO 4 + 175 mg HgO

15270010

CT, tablets with 5 g K 2 SO 4 + 0,15 g CuSO 4 x 5 H 2 O + 0,15 g TiO 2

20

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

10

15270018

Copper, tablets with 3,5 g K 2 SO 4 + 400 mg CuSO 4 x 5 H20

15270020

CT, tablets with 3,5 g K 2 SO 4 + 0,105 g CuSO 4 x 5 H 2 O + 0,105 g TiO 2

15270033

Mercury, tablets with 1,5 g K 2 SO 4 + 7.5 mg HgO

15270034

Copper, tablets with 1,5 g K 2 SO 4 + 150 mg CuSO 4 x 5 H20

15270048

Mercury, tablets with 3,5 g K 2 SO 4 + 175 mg HgO

15270056

NAS, tablets with 1 g Na 2 SO 4 + 0,05 g Se

15270057

KPC, tablets with 4,5 g K 2 SO 4 + 0,5 g CuSO 4 x 5 H 2 O

15270058

Special (AB24), tablets with 1,65 g K 2 SO 4 + 0,33 g CuSO 4 x 5 H 2 O + 0,0165 g Se

15270059

Special (AB22), tablets with 4,75 g K 2 SO 4 + 0,075 g CuSO 4 x 5 H 2 O + 0,10 g Se

15270060

Antifoam (AA00), tablets with 0,966 g Na 2 SO 4 + 0,029 g silicon + 0,005g Si

15270061

Auto CT (AA22), tablets with 1,5 g K 2 SO 4 + 0,045 g CuSO 4 x 5 H 2 O + 0,045 g TiO 2

15270062

Special (AB64), tablets with 5,0 g K 2 SO 4 + 0,06 g Se

15270063

KS (AA47), tablets with 4,95 g K 2 SO 4 + 0,05 g Se

15270065

K/5 (AA23), tablets with 5 g K 2 SO 4

Other types are available upon request. However, those listed above represent more than 90% of the catalyst tablets used worldwide.

10.4

Manufacturer’s Name and Address

FOSS Tecator AB Box 70 SE-263 21 Höganäs Sweden +46 42 361500 +46 42 340349

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

Int phone. Int fax.

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

This page is intentionally not used.

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c) Switch on the power. d) Turn on the cold water tap Note: The water for the condenser and steam generator will not flow until the steam valve is in the open position with the power on. It will stop automatically when the valve is closed. e) Open the valve for steam by pushing the steam control handle on the front panel in down position (Fig. 9). After a couple of minutes steam is generated. Let the distillation continue until some water is collected in the receiver flask. The system is then heated up. g) If the platform with the receiver flask is in the upper position (Fig. 10), move it to the lower position. Close the steam valve on the front panel.

11.4.3

Distillation

which the steam enters the sample, should be placed in the slot of the plastic holder (Fig. 11). This makes it possible to replace a tube without touching the teflon pipe which will have traces of alkali on it.

11.4.4

Closing down

a) Do the daily maintenance according to chapter 11.5. b) Pull out the drain collector (Fig. 12) under the tube holder and the platform for the receiver flask and clean it with water. Wipe the instrument clean from any spillage. c) Switch off the power and close the water tap.

11.5

This text is also avaliable as an instruction 10006458 which includes Maintenance Record Charts to facilitate a record of your actions.

11.5.1

b) Place the tube with the first diluted Sample to be distilled in its position and place the receiver flask with the receiver solution on the platform. To avoid contamination don’t touch the glass outlet tube with your fingers. Hold it by its plastic tubing if necessary.

To avoid start up problems and to prolong the lifetime of your system the procedures described in this chapter should be performed every day the unit is used.

d) Move the platform for the receiver flask to its upper position. e) Gently pull the alkali handle all the way down to dispense about 50 ml of alkali (Fig 8). f) Open the steam control and set the timer to the appropriate distilling time (around 4 minutes). g) Lower the platform for the receiver flask and continue distillation for a few more seconds to rinse the outlet tip. Close the steam control. h) Replace the test tube and the receiver flask with the next set and continue in the same manner with all the samples. When removing a tube, the teflon pipe through

11.5.1.1

Daily

Cleaning cycle

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

11.5.1.2

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

11.5.2.1

Reagent tanks inspection and cleaning

Rubber adapter

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

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

depending on usage. Use the Maintenance Record Chart provided with the instruction to keep a record of these operations. Important! If the rear panel is removed, there is a grounding cable (yellow/green) connected inside between the rear panel and the main cabinet (lower right corner). Be sure to reconnect when replacing the panel.

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

11.5.3.1

11.5.2.2

Remove the rubber adapter from the unit and inspect it for scratches and cracks. Note also if the rubber of the adapter has started to lose it softness. If the adapter show signs of scratches, cracks or that the rubber has started to lose its softness the adapter has to be changed.

Digestion tubes inspection

Check the rims of the digestion tubes for uneven surface,cracks and chips. This type of damage can cause leakage between the tube and the rubber adapter leading to loss of recovery during analysis. Look for scratches and star fractures on the base of the tubes. These can lead to untimely and unexpected breakages creating a safety hazard to you and your colleagues and potential damage to your digestion or distillation unit. Discard all damaged tubes in the interest of safety. After some digestions the base of the tubes may take on an off-white to greyish coloration. This is quite normal and does not require the tubes to be replaced.

Cleaning of unit

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

11.5.1.3

Weekly

Maintenance

a) Remove the test tube and the receiver flask.

c) Close the safety door.

11.5.2

11.5.2.3

11.5.3.2

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

· · ·

Close the safety door.

·

Check the volume a couple of times. The amount of alkali is set to about 50 ml from the factory. This volume can be reduced by putting dispensing stops in the slot below the alkali dispensing handle. Turn them 90° to fix them in position fig. 13.

·

After any adjustment, check the volume again.

Cleaning the safety door

Every one to three months

Controlling the alkali volume

·

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

11.5.3

Controlling the rubber adapter

Switch on power. Gently pull the handle all the way down to dispense the alkali.

In addition to the routines outlined above the following procedures should be performed every one to three months, or as the need arises, 24

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 the system.Pump about half a litre of the water through the alkali pump by pressing the alkali handle. This procedure requires that the tube is emptied when about 200 ml has been dispensed. Replace the tube and continue the flushing.

11.5.3.4

Cleaning of the splash head

Pour about 25 ml of water and the same amount of concentrated acetic acid into a test tube and distil for 5 to 10 minutes. Replace the tube with a clean tube and continue to distil for another 5 minutes. Repeat this at least three times so no acid residues will interfere with the analysis.

11.5.4

Depending on number of analyses

The frequency with which you should carry out the procedures in this chapter depends upon a number of factors which are outside FOSS Tecator AB’s control and are therefore difficult to predict. In simple terms you will have to judge the required frequency by physically checking the situation in each case. To a large extent the frequency will depend on two major points. 1. The quality of the water used for steam generation. For example tap water will create more or less salt deposits depending on its hardness. If deionised water is used,cleaning will rarely be necessary, but please remember that a certain level of conductivity is required for correct operation of the level pins (See trouble shooting) 2. How well you have followed the guidelines in the first three chapters of this text. Regular and immediate cleaning of splashes and spillage will create less problems. Routine checking of connectors when the reagents are replaced will limit the likelihood of leakages.

11.5.4.1

Cleaning of the steam generator

Disconnect the power supply. Open the drain valve for the generator. When empty, fill up the generator with a solution of 100 g citric acid in 800 ml water, preferable hot, by connecting the funnel to the steam generator drain. Suspend the funnel so that is in higher position than the steam generator. Close the drain valve, whilst the funnel is still suspended above the steam generator. Alternative 1.Leave the solution in the steam generator overnight, or until the generator vessel is free from deposits. Alternative 2.Connect the power supply. Place a distillation tube and a receiver flask in their positions and close the safety door. Switch on power and open the steam valve. Let the citric acid solution boil for about five minutes. Close the steam valve and disconnect the power supply.

Caution If Alternative 2 has been chosen the solution will be extremely hot! Open the drain valve and empty the steam generator. Rinse the generator thoroughly with water using the funnel again. When the vessel is clean and rinsed, close the drain valve. Remove the funnel and put the drain tubing outlet back to its normal position.

11.5.5

Every Year

Your local distributor offers Service Agreements in order to make your instrument reliable in performance and safety. As a minimum of care all tubings and connectors should be inspected. Exchange if visible damages can be seen.

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

·

TROUBLE SHOOTING* This requires the fitting of a direct Feed Water System and must be carried out at the factory or by a certified FOSS Tecator AB service engineer in your laboratory.

For information about preparation of chemicals and the Kjeldahl method please see the Application Note AN 300 supplied with your system. In FOSS Tecator ABs extensive list of Application Sub Notes you will find information on how to analyse the sample of your choice. Please contact your FOSS Tecator AB representative for more details.

11.6 11.6.1

Technical specifications Safety

The insulation of external, inaccessible circuits is reinforced.

11.6.2

Environmental conditions

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

· · · ·

Indoor use

·

Mains supply voltage fluctuations not exeeding ± 10% of the rated voltage.

·

Transient overvoltage is according to category II, which is normal for this type of equipment.

·

Pollution degree 2

11.7

Storage & transport

11.7.1

Lifting instructions 1002

This instrument is not equipped with handles or grips. Two persons are needed to lift the instrument, following the instructions below: 1. Tilt the instrument slightly backwards, and lift and support the instrument as shown in fig.16 to simplify and ensure a safe lift. 2. Weight 25 kg.

Caution! Avoid getting your fingers pinched!

11.8

Explanations to illustrations

Fig 5 Connections left to right. 1. Steam waste tubing 2. Cooling water inlet 3. Steam generator drain 4. Water tank (for direct feed water systems only) 5. Alkali inlet 6. Electric power cable 7. Equipotential connector

Altitude up to 2000 m. Temperature 5°C to 40°C. Maximum relative humidity 80% for temperatures up to 31°C decreasing linearly to 50% relative humidity at 40°C.

Fig 6 Use tubing clamps to secure tubings. Fig 7 Water connection. Fig 8 1. Power switch 2. Timer 3. Steam control 4. Alkali handle 5. Safety door. Fig 11 Resting position for the teflon tube.

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