Operation Manual Distillation Unit K�355 93036 en
Table of contents Table of contents 1 2 3 4 5 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.1 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 2.1 User qualification . . . . . . .
Table of contents 6 7 8 9 10 11 4 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 6.1 Addition of chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 6.1.1 Manual dosage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 6.1.2 Automatic dosage . . . . . . . . . . . . . . .
1 1 About this manual About this manual This manual describes the Distillation Unit K-355 and provides all information required for its safe operation and to maintain it in good working order. It is addressed to laboratory personnel in particular. NOTE The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in chapter 2. 1.
2 2 Safety Safety This chapter points out the safety concept of the instrument and contains general rules of behavior and warnings from hazards concerning the use of the product. The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual chapters are strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein. 2.
2 2.4 Safety Warning notices used in this manual WARNING Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life if the instructions are not followed. WARNING Hot surface. WARNING Electrical hazard. WARNING Caustic substances. ATTENTION With the general „Read this” symbol, ATTENTIONs indicate the possibility of equipment damage, malfunctions or incorrect process results, if instructions are not followed.
2 2.5.2 Safety Other hazards WARNING Certain solvents in or in the vicinity of the instrument can form peroxides and/or are highly inflammable. • A lways be aware of the explosion risk when working with hazardous substances or with substances of unknown composition. • Always provide a good ventilation within or in the vicinity of the system. 2.5.3 Safety measures WARNING Sodium hydroxide, acids and lye are used for applications according to Kjeldahl.
2 2.6 Safety General safety rules Responsibility of the operator The head of laboratory is responsible for training his personnel. The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed.
3 3 Technical data Technical data This chapter introduces the reader to the instrument specifications. It contains the scope of delivery, technical data, requirements and performance data. 3.1 Scope of delivery Check the scope of delivery according to the order number. NOTE For detailed information on the listed products see www.buchi.com or contact your local dealer. 3.1.
3 3.1.2 Technical data Standard accessories Table 3-2: Standard accessories Product Order number a 1 mains cable of the following types 1 2 6 5 4 3 7 8 11 9 10 Type CH 10010 Type Schuko 10016 Type GB 17835 Type AUS 17836 Type USA 33763 Type Japan 10016 b 1 pair of glass tongs 02004 c 1 hose cooling water drain, silicone, L = 1.8 m, Ø 10/14 mm 43439 d 1 hose chemical supply, solaflex, L = 3.
3 3.1.
3 Technical data Table 3-3: Optional accessories K-355 (cont.
3 Technical data Table 3-3: Optional accessories K-355 (cont.
3 3.2 Technical data Technical data Table 3-4: Technical data K-355 Distillation Unit K-355 3.3 Power consumption max. 2.2 kW Connection voltage 230 V ± 10% / 200 V ± 10% Frequency 50/60 Hz Current consumption (230 V) 8.5 A Mains connection 3-pole (P, N, E) via power cord Recovery rate ≥ 99.5% Reproducibility (RSD) ≤ 1% Detection limit ≥ 0.
4 4 Description of function Description of function This chapter explains the basic principle of the instrument, shows how it is structured and gives a functional description of the assemblies. 4.1 Instrument overview 5 4 1 6 2 3 a Splash protector b Sample tube c Protective door dC ondenser eO perating panel f Service door Fig. 4.
4 4.2 Description of function Function principle The Distillation Unit K-355 is suitable for determining nitrogen using the Kjeldahl (TKN; Total Kjeldahl Nitrogen) and Devarda methods as well as for other distillations of steam-volatile substances (e.g. of alcohol, SO2, volatile acids). a Sample tube b Splash protector c Condenser d Distillate outlet tube e Receiving vessel with receiver solution 3 2 4 1 5 Fig. 4.
4 4.3 Description of function Controls of the instrument a STOP: Stops a distillation or the addition of reagent b TIME display c STEAM power display d START: Starts a distillation e TIME: Sets time in min:sec f UP: Increases time and steam up g STEAM: Sets steam power h DOWN: Decreases time and steam down i REAGENT: Button that adds reagent (e.g. water, sodium hydroxide solution) 1 2 3 6 5 4 8 7 9 9 Fig. 4.
5 5 Putting into operation Putting into operation This chapter describes how the instrument is installed and gives instructions on initial startup. NOTE Inspect the instrument for damages during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company or transportation company. Keep the original packaging for future transportation. 5.
5 Putting into operation The instrument cable must be well attainable at all times. Make sure that no electric sparks form in the instrument or its surroundings as they might damage the instrument. 5.3 Reagent and water connections a a H2O inlet (for steam generator) from tank b Reagent 1 inlet (water or acid) c Reagent 2 inlet (NaOH) d Cooling water inlet e Cooling water outlet f Drain to waste b c d e f Fig. 5.
5 5.3.3 Putting into operation Storage tank connection To connect the storage tanks, proceed as follows: • C ut the solaflex tube into pieces of the appropriate length (use an acid resistant tube, if acid is dosed). • Insert a PTFE suction tube into the solaflex tube. • Push an EPDM sealing ring over the solaflex tube. • Now fasten the tubes to the tank with the red screw cover. • Connect the tubes at the appropriate connections at the instrument side and secure them with the clamps.
6 6 Operation Operation This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely. WARNING Risk of injury. • Never operate the instrument when glassware is damaged. WARNING Sodium hydroxide, acid and lye are used for applications according to Kjeldahl. For this reason, protective goggles must be worn at all times when using this instrument or working in its immediate proximity. NOTE Close unused connections with plug caps.
6 6.2 Operation Setting the distillation time To set the distillation time, proceed as follows: • Press “TIME”, the digit for minutes starts to flash. • Press “TIME” again, the digit for seconds starts to flash. • Set the distillation time by pressing “UP” and “DOWN”. • Start the distillation by pressing “START”. Digits stop flashing after a certain time or after starting the distillation. When pressing “UP” and “DOWN”, the time is first counted slowly, then faster.
6 6.5 Steam generator status 6.5.1 Heating Operation A constant colon (:) and an “H” in the STEAM-display indicates, that the steam generator is heating. A flashing colon (:) and a signal sound for 1 second indicates that the steam generator is ready. 6.5.2 Standby mode (after 30 minutes) The TIME display and STEAM display show (-----). Press “START” to cancel the standby mode. 6.
6 Operation solution. The volume of the added sodium hydroxide solution is measured on the scale behind the sample tube. The added volume selected must produce a clear shift in color to brown or blue. NOTE After distillation or after “STOP“, the last distillation time can be recalled by pressing “START“ or will automatically be recalled when exchanging the sample tube.
7 7 Maintenance and repairs Maintenance This chapter gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition. WARNING Electrical hazard: • P rior to all maintenance work on the instrument switch off the power supply and remove all sources of flammable vapor. WARNING All maintenance and repair work requiring the opening or removal of instrument covers may only be carried out by trained personnel and with the tools provided for this purpose.
7 7.1.4 Maintenance and repairs Preparing the instrument for a standstill overnight To prepare the instrument for a longer standstill (e.g. overnight), fill 50 ml distilled water into the receiving vessel and 30 ml of distilled water into the sample tube. 7.2 Weekly maintenance 7.2.1 Cleaning the splash protector and the rubber bung seal Unmount the splash protector and remove the rubber bung seal. Rinse the splash protector with water to remove sample residues.
7 7.4 Half-yearly maintenance 7.4.1 Replacing the NaOH tube Maintenance and repairs We recommend to replace the NaOH tube every six months. The other tubes need to be replaced as and when required. 7.5 Yearly maintenance 7.5.1 Replacing the rubber bung seal The seal is subject to wear and tear, thus you should check it regularly. We recommend to replace it once a year. 7.5.2 Replacing the NaOH pump We recommend to replace the NaOH pump once a year.
8 8 Troubleshooting Troubleshooting This chapter helps to resume operation after a minor problem has occurred with the instrument. It lists possible occurrences, their probable cause and suggests how to remedy the problem. The troubleshooting table below lists possible malfunctions and errors of the instrument. The operator is enabled to correct some of those problems or errors by him/herself. For this, appropriate corrective measures are listed in the column “Corrective measure”.
9 9 Shutdown, storage, transport and disposal Shutdown, storage, transport and disposal This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and specifies the storage and shipping conditions. 9.1 Preparing the instrument for transport Take out the power cord and remove all water/reagent tubing. Rinse the sodium hydroxide solution tube with distilled water. Clean the instrument thoroughly, so that all chemical residues are removed completely.
10 10 Spare parts Spare parts This chapter lists spare parts, accessories, and options including their ordering information. Order the spare parts from Buchi. Always state the product designation and the part number when ordering spare parts. Use only genuine Buchi consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer. 10.
10 Spare parts Table 10-1: Spare parts K-355 (cont.) Product Order number p Drip tray 43302 4 sample tubes 300 ml 37377 Cap for 20 l tanks, large (1 piece) 43478 16 10.2 Hosing connection scheme 12 1 9 14 11 13 5 10 15 6 2 7 3 8 4 a Inlet b NaOH tank c H2O tank d Acid tank e Valve cooling water in f Pump NaOH g Pump H2O steam generator h Pump special i Cooler j Receiving vessel k Splash protector l Check valve m Ventilation n Valve steam o Output Fig. 10.
10 Spare parts Table 10-2: Tubes and components Distillation Unit K-355 Position 33 Order number Pcs Description 1-2 43555 1 Solaflex tube Ø 10/5, L = 3500 3 43153 1 Unisil Ø 6 x 2, L = 640 4 43151 1 Unisil Ø 6 x 2, L = 370 5 43154 1 Unisil Ø 6 x 2, L = 920 6 43572 1 Viton tube Ø 9/6, L = 1200 7 43578 1 Viton tube Ø 10/7, L = 380 8 43574 1 Viton tube Ø 10/7, L = 190 9 43575 1 Viton tube Ø 10/7, L = 230 10 43574 1 Viton tube Ø 10/7, L = 190 12 43029 1 EPDM 6.
11 11 Declarations and requirements 11.1 FCC requirements (for USA and Canada) Declarations and requirements English: This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.
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BÜCHI Labortechnik AG CH-9230 Flawil 1 / Switzerland T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.
