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6 Operation

29

KjelFlex K-360

Operation Manual, Version D

6 Operation

This chapter gives examples of typical instrument applications and instructions on how to operate the
instrument properly and safely.

!

CAUTION

Risk of cuts by defective glassparts.
•  Handle glassparts with care.
•  Exchange defective glassparts directly.
•  Do not operate the instrument when glassparts are damaged.

!

WARNING

Serious chemical burnings by corrosives.
•  Observe supplementary data sheets of all used chemicals.
•  Wear protective goggles.
•  Wear protective gloves.
•  Wear protective clothing.

NOTE

Close unused connections with plug caps.

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Summary of Contents for KjelFlex K-360

Page 1: ...KjelFlex K 360 Operation Manual 093176D en...

Page 2: ...he right to make changes to the manual as deemed necessary in the light of experi ence especially in respect to structure illustrations and technical detail This manual is copyright Information from i...

Page 3: ...on principle 20 4 3 Kjeldahl applications 20 4 4 Non Kjeldahl applications 20 4 5 Operational elements of the instrument 22 Read this manual carefully before installing and running your system and not...

Page 4: ...1 Standard instrument configuration 34 6 3 2 Distillation methods 34 6 3 3 System preparation 34 6 3 4 Individual working method 35 6 4 Configuring the instrument 35 6 4 1 Pump calibration 36 6 4 2 Se...

Page 5: ...3 4 Glass parts 52 7 3 5 Replacing the hoses 52 7 4 Yearly maintenance 53 7 4 1 Customer service 53 7 4 2 Decalcification of the steam generator 53 8 Troubleshooting 54 8 1 Malfunctions and their rem...

Page 6: ...It is addressed to laboratory personnel in particular NOTE The symbols pertaining to safety messages are explained in chapter 2 1 1 Abbreviations EPDM Ethylene Propylene Dimonomer FCC Federal Communi...

Page 7: ...mpanied by the general safety sign For your safety it is important to read and fully understand the below table with the different signal words and their definitions Sign Signal word Definition Risk l...

Page 8: ...t machine parts hot surface Corrosive substances General warning sign General system damage Mandatory action symbols Meaning Wear safety gloves Wear protective goggles Additional user information Para...

Page 9: ...er The operator bears the sole risk for any damages caused by such improper use The following uses are expressly forbidden Use of the instrument in rooms which require ex protected instruments Use on...

Page 10: ...urns at the splash protector distillation area which is hot during distillation Protective door sensor Prevents the start of a distillation with the protective door open and stops a running distillati...

Page 11: ...ed in proper condition only and that maintenance service and repair jobs are performed with care and on schedule and by autho rized personnel only Spare parts to be used Use only genuine consumables a...

Page 12: ...0 Standard with splash protector made of fiber glass reinforced polypropylene 230 V 50 60 Hz 43601 KjelFlex K 360 with glass splash protector and acid resistant pump 230 V 50 60 Hz 43605 KjelFlex K 36...

Page 13: ...ain silicone L 1 8 m 14 10 mm 43439 d Weighing boats 40444 e Hose chemical supply Nylflex L 6 m 10 5 mm 43185 f 3 suction hoses to tanks FEP L 580 mm 43407 g Hose waste drain EPDM L 1 8 m 18 11 mm for...

Page 14: ...out level sensors including caps e 10 L chemicals 43468 e 10 L waste 43470 h 20 L chemicals 43469 h 20 L waste 43471 Tanks with level sensors including caps g 10 L chemicals 43472 g 10 L waste 43374 f...

Page 15: ...L each 16951 Holder for 6 sample tubes 300 mL 43039 Holder for 12 sample tubes 300 mL 43041 Titration set 43698 Splash protector for Devarda method 43335 Connection cable to Mettler DL15 22 titrator 4...

Page 16: ...sumption max 2 2 kW Connection voltage 220 240 VAC 10 Frequency 50 60 Hz Mains connection 3 pole P N E via power cord Recovery rate 99 5 Reproducibility RSD 1 Detection limit 0 1 mg Nitrogen Vapor out...

Page 17: ...0 1 mol L 5 71 mL 10 P 6 25 1 6 N 2 g H2 SO4 0 1 mol L 11 42 mL 10 P 6 25 1 6 N 2 g H2 SO4 0 25 mol L 4 57 mL 20 P 6 25 3 2 N 2 g H2 SO4 0 25 mol L 9 14 mL 50 P 6 25 8 0 N 2 g H2 SO4 0 5 mol L 11 42...

Page 18: ...UR UL V0 Glass parts Borosilicate glass 3 3 DIN ISO 3585 Steam generator isolation Ceramic fiber Multitherm 550 Steam generator housing Stainless steel 1 4301 Protective door Polymethyl methacrylate P...

Page 19: ...his 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 1 2 3 4 5 6 a Splash protector b Samp...

Page 20: ...nser e Distillate outlet tube f Receiving vessel with receiver solution Fig 4 2 Function principle Steam is introduced into the sample solution in sample tube a to drive out volatile components such a...

Page 21: ...wnwards position To carry out a non Kjeldahl application the stop cock must be in horizontal position CAUTION Risk of burnings by hot machine parts and water steam Let the system cool down before perf...

Page 22: ...display 4 5 Operational elements of the instrument 1 2 3 6 7 8 5 3 3 3 4 9 a Stop button to stop a process b Display c Functional buttons to operate the software d Navigation buttons to navigate withi...

Page 23: ...he tanks for chemicals beside the instrument not higher and not more than 1 m lower Notice Reduced instrument safety and lifetime due to improper handling and installation location Do not place any ob...

Page 24: ...necessary at the tanks 5 3 1 Cooling water connection The water pressure should be at a maximum of 4 bar The built in valve reduces the water flow to 1 2 liters per minute The flanged screw coupling f...

Page 25: ...k flow the hose may be placed maximum 10 cm into the tank 5 3 4 Storage tank connection To connect the storage tanks proceed as follows Cut the Nylflex hose into pieces of the appropriate length use a...

Page 26: ...vel sensor for the waste tank must be set active at Configuration Settings Level Sensor Waste This is not necessary for the other sensors Fig 5 4 Adapting the length of the level sensor Adapt the leng...

Page 27: ...rresponding manual The following printers have been tested together with the K 360 HP Color LaserJet 3700DN HP Deskjet 1280c Brother mfc 8820d Lexmark E120 Lexmark E240 HP OfficeJet Pro K550 Brother H...

Page 28: ...sulfuric acid solution or hy drochloric acid solution It is recommended to use boric acid solution 4 adjusted to pH 4 65 and standardized sulfuric acid solution The K 360 includes all necessary hardwa...

Page 29: ...afely CAUTION Risk of cuts by defective glassparts Handle glassparts with care Exchange defective glassparts directly Do not operate the instrument when glassparts are damaged WARNING Serious chemical...

Page 30: ...e List 2 Preheating 3 Priming Priming Method H2 O NaOH H3 BO3 Reagent volumes Reaction Time Steam Power Distillation Time Titration Start Titr Type Stirrer Speed Aspiration Sample Receiver 4 Cleaning...

Page 31: ...aOH H3 BO3 Reagent Pump 2 Set Date and Time Date Time Details 3 Settings Language Display Contrast Demo Mode Endless Mode Level Sensor Waste Rec Vessel Present Reagent Pump 4 Titrator Print Data Titra...

Page 32: ...Unit Titrator Dispenser Battery 2 Test Sensor Cooling Water Flow Tube Shield Switch Tube Present Check Switch Service Door Switch Steam Unit Level Sensors Titrator Dispenser Voltage Temperature 3 Tes...

Page 33: ...d on a report Add 10 mL of H2 O Add 10 mL of H3 BO3 Add 10 mL of NaOH Add 10 mL of reagent Go to the method screen to view define or edit a method Go to the Method List screen Print Switch from Standb...

Page 34: ...tandard instrument configuration This configuration consists of typical settings which have to be defined before the instrument is used for the first time As long as the instrument is not updated or e...

Page 35: ...ented analysis Here all sample names and the corresponding weight is entered prior to determination The volume consumption of the titrant solution is stored together with the sample name see also chap...

Page 36: ...the dosed volume and enter the measured volume Press Cal to calibrate the pump When the calibration is finished a corresponding calibration factor appears NOTE Repeat this procedure until the entered...

Page 37: ...Mode Endless Mode Level Sensor Waste Receiving Vessel present Reagent pump present Enter the desired settings via arrow buttons and press Save to store them These settings have to be defined before th...

Page 38: ...tware Mettler Toledo DL 15 22 Txx Schott TitroLine Easy Metrohm Titrino DMP 785 719 702 848 Plus To assure a correct signal transfer the respective titrator has to be configurated according to the B c...

Page 39: ...l Standardized sulfuric acid Titrant Standardized sodium hydroxide solution Defining the K 360 settings for back titration The following setting at the K 360 is a prerequisite for working with a dispe...

Page 40: ...the corresponding user is indicated on the result printout list When a password is forgotten the determination can be started with the Buchi default login User name buchi password buchi01 When the Buc...

Page 41: ...6 11 Method A method consists of the following settings Name User Amount of chemicals to be dosed H2 O NaOH H3 BO3 Reagent Reaction time Titration type Stirrer speed Distillation Titration aspiration...

Page 42: ...to analysis Use a clean and empty sample tube for this processing It is recommended to perform a preheating when the glass splash protector has cooled down The preheating time is predefined 6 7 2 Pri...

Page 43: ...hes depending on how you prefer to work Single sample analyses Rack oriented analyses 6 8 1 Single sample analysis For single sample analyses no predefined sample list is needed for identification To...

Page 44: ...ress Save The newly created entry now appears in the list Repeat this step for all provided samples To start distillation of a sample enter Determination in the main menu select an entry and press the...

Page 45: ...or is connected no Result screen is displayed 6 8 5 Result list To view the list of results measured go to Results in the main menu and press Enter or just press 6 The Result List opens Fig 6 18 Resul...

Page 46: ...checklist To switch on and preheat the instrument proceed as follows Check the filling level of the supply tanks Open the main water tap Switch on the instrument and wait until the steam generator is...

Page 47: ...and remove the power cord Do not bring any electrical component into contact with fluids Do not operate the instrument when enclosure is open or removed CAUTION Risk of burnings by hot machine parts...

Page 48: ...a damp cloth NOTICE Risk of housing damage by solvents and acids Do not clean the housing with solvents Wipe off any acid drops immediately Open the service door and perform a visual check of all part...

Page 49: ...stillation Sample tube empty Water 0 mL NaOH 0 mL Distillation time 5 00 Measure the distillate amount by means of a measuring flask With the above parameters it should be minimum 130 mL 7 3 Maintenan...

Page 50: ...Replace the Splash protector after approximately 5000 determinations 7 3 3 Replacing the rubber bung seals and the splash protector We recommend to replace the parts listed below depending on the ins...

Page 51: ...ews with black head to remove the metal holder at the front side Carefully remove the bracket Now unscrew the black plastic screw with a polygrip Make sure to do this gently as you might break the gla...

Page 52: ...shown on the first picture of chapter 7 3 3 Put back the replaced parts in the reverse order and make sure to tighten the screw on top of the splash protector very carefully with the Polygrip 7 3 4 G...

Page 53: ...generator To decalcify the steam generator proceed as follows 1 Make sure that the steam generator is cooled down switch off the unit and let it cool down for at least 30 minutes 2 Remove the water of...

Page 54: ...vice 8 Injection Valve Y8 on malfunction Contact the Buchi customer service 9 Water Valve Y9 on malfunction Contact the Buchi customer service 11 Steam Valve Y1 off malfunction Contact the Buchi custo...

Page 55: ...for steam generator Fill water tank check H2 O pump 46 Titrator not ready or not configured Configure titrator in Configuration menu 47 Dispenser not ready or not configured Configure dispenser in Con...

Page 56: ...delete some methods Delete some methods and add new methods 64 Restart from Watchdog No corrective measure needed 65 You changed between the demo and the normal mode Restart the system to activate th...

Page 57: ...Open the tube shield When the sensor is working properly Open will be indicated on the display Close the tube shield Now Close has to be indicated on the display NOTE The button Actors enables to swi...

Page 58: ...ment and remove the power cord Do not bring any electrical component into contact with fluids Do not operate the instrument when enclosure is open or removed CAUTION Risk of burnings by hot machine pa...

Page 59: ...ow with a screw driver and completely empty the steam generator Close the stop cock with a screw driver 1 a Drain with screw Fig 9 1 Emptying the steam generator 9 2 Storage and transport Store and tr...

Page 60: ...eliability Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer 10 1 Spare parts K 360 1 2 3 Table 10 1 Spare parts K 360 Product Order numb...

Page 61: ...in silicone L 1 8 m 14 10 mm 43439 h Weighing boat 40444 i Hose chemical supply Nylflex L 6 m 10 5 mm 43185 j 3 suction hoses to tanks FEP L 580 mm 43407 k Hose waste drain EPDM L 1 8 m 18 11 mm 43457...

Page 62: ...7 8 9 10 11 12 13 14 a Boric acid tank b H2 O tank c NaOH tank d Cooling water valve in e Boric acid pump f H2 O steam generator pump g NaOH pump h Condenser i Receiving vessel j Splash protector k Sa...

Page 63: ...Boric acid tank b H2 O tank c NaOH tank d Cooling water valve in e Boric acid pump f H2 O steam generator pump g NaOH pump h Condenser i Receiving vessel Titration set j Splash protector k Sample tube...

Page 64: ...ank c NaOH tank d Storage bottle for reagent e Cooling water valve in f Boric acid pump g H2 O steam generator pump h NaOH pump i Reagent pump j Condenser k Receiving vessel l Splash protector m Sampl...

Page 65: ...H tank d Storage bottle for reagent e Cooling water valve in f Boric acid pump g H2 O steam generator pump h NaOH pump i Reagent pump j Condenser k Receiving vessel Titration set l Splash protector m...

Page 66: ...8 L 530 1 1 19 43692 EPDM 6 2 8 L 820 1 1 20 43438 EPDM 18 2 11 L 340 1 1 1 1 21 43457 EPDM 18 2 11 L 1800 1 1 1 1 22 43366 FEP 6 4 L 40 1 1 23 43439 Silicone 14 10 L 1800 1 1 1 1 24 43184 Spiral ban...

Page 67: ...to cause harmful interference in which case the user will be required to correct the interference at his own expense Fran ais Cet appareil a t test et s est av r conforme aux limites pr vues pour les...

Page 68: ...oling water 24 external keyboard 27 peripheral devices 26 printer 27 storage tank 25 Controls of the instrument 22 Converter cock 21 Customer service 53 D Date and time 36 Diagnostics 56 Disposal 59 D...

Page 69: ...M Maintenance daily 48 monthly 49 Materials used 18 Modes 42 Modifications 11 N Non Kjeldahl applications 20 O Operating Hours 57 Operational Tests 56 P Password settings 39 Preheating 42 Preparation...

Page 70: ...2 Service Test 57 Settings 37 titrator 37 Single sample analysis 35 Software structure 30 Spare parts to be used 11 Storage 59 System preparation aspiration 42 cleaning 42 preheating 42 priming 42 T T...

Page 71: ......

Page 72: ...w buchi com cn India BUCHI India Private Ltd IN Mumbai 400 055 T 91 22 667 75400 F 91 22 667 18986 india buchi com www buchi in Indonesia PT BUCHI Indonesia ID Tangerang 15321 T 62 21 537 62 16 F 62 2...

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