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4 Description of function

K-375 / K-376 / K-377

Operation Manual, Version E

36

4.5 Distillation and titration

4 5 1

Distillation and Titration Options

Titration

type

Titration

mode

Distallation

mode

Measuring mode

Titration

algorithm

Boric acid

Back titration

Standar

d

Online

IntelliDist

Fixed time

Endpoint pH

Startpoint pH

Setpoint mV

Optimal

Normal

Potentiometric

x

x

x

x

x

x

x

x

x

x

Colorimetric

x

x

x

x

x

x

x

4 5 2

Distillation Mode

Automatic – IntelliDist

This mode eliminates errors caused by a cooled instrument. The countdown of the set distillation time
only starts after operating temperature is attained. With single samples or sample list measurements
this mode guarantees result accuracy from the very first run.

Fixed Time

The countdown of the set distillation time starts immediately with the start of the distillation process.
This setting is recommended when a sample changer is used for the analysis of samples in a rack (or
sequence).

4 5 3

Titration Type

The built-in titrator is fully controlled via the K-375 software. It is not possible to use the titrator without
the KjelMaster K-375. It can be used for boric acid or back titration. The measuring mode can be
determined as endpoint or startpoint titration by defining the method in the K-375. The software of the
K-375 allows to choose between standard and online titratio

n.

Boric Acid Titration

Boric acid adjusted to a pH of 4.65 is used as receiving solution to capture the nitrogen carried over
as ammonia during the steam distillation. The subsequent endpoint titration (pH 4.65) is performed
with an acid titration solution. This titration type does not require an accurate dosage of the boric
acid.

Back Titration

The receiving solution is a standardized acid (e.g. H

2

SO

4

) of which an accurate volume is dispensed

into the receiving vessel. After collecting the ammonia the excess acid is titrated with a basic titration
solution (NaOH) at pH 7.00. If the use of boric acid has to be avoided the back titration is the proce-
dure of choice.

4 5 4

Sensor Type

Potentiometric

Potentiometric pH measurement is

commonly used and allows

both boric acid and back titrations.

They need regular calibration with buffers.

Colorimetric

Colorimetric titration is based on colour change at the equivalence point and is used in situations
where an official standard requires it. For sound measurements and reproducible results the conden-
sate outlet with air bubble trap must be fitted. The condensate outlet prevents air bubbles interfering

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Содержание KjelMaster K-375

Страница 1: ...KjelMaster K 375 with KjelSampler K 376 K 377 Operation Manual 11593514E en ...

Страница 2: ... BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience espe cially in respect to structure illustrations and technical detail This manual is copyright Information from it may not be reproduced distributed or used for competitive purpos es nor made available to third parties The manufacture of any component with the aid of this manual without prior wr...

Страница 3: ...G Initial version B 16 JUL 2013 NAGG First revised version C 17 NOV 2014 HILS BRUS Second revised version update colorimetric titration D 28 APR 2016 HILS Removal of Declaration of Conformity E 12 DEC 2018 HOES Third revised version update colorimetric titration ...

Страница 4: ...evice without the prior written agreement of BUCHI Unauthorized modifications may affect the system safety or result in accidents This manual is copyright Information from it may not be reproduced distributed or used for competitive purposes nor made available to third parties The manufacture of any component with the aid of this manual without prior written agreement is also prohibited If you nee...

Страница 5: ...ories for K 376 K 377 21 3 1 4 Operation Manuals for K 375 22 3 1 5 Optional accessories K 375 23 3 1 6 Optional accessories K 376 K 377 25 3 2 Technical data overview 26 3 2 1 Technical data KjelMaster K 375 and KjelSampler K 376 K 377 26 3 2 2 Technical data titrator 27 3 3 Determination parameters 28 3 4 Information on type plate 29 3 4 1 Titrator module and dosing unit 29 3 4 2 Material on the...

Страница 6: ...75 46 5 3 1 Connecting the K 376 to the K 375 46 5 3 2 Connecting the transfer hoses of the K 377 48 5 4 Reagent water and waste connections 49 5 5 Buret unit for titrant 51 5 6 Positioning of the dosing tip 53 5 7 Storage tank connection 53 5 8 Level sensors 54 5 9 Installation of the titration sensor 56 5 9 1 Potentiometric sensor 56 5 9 2 Colorimetric sensor 56 5 10 Connections to peripheral de...

Страница 7: ... 118 6 9 4 Logout 119 7 Maintenance 119 7 1 Daily maintenance 120 7 1 1 Before sample determination potentiometry 120 7 1 2 Before sample determination colorimetry 121 7 1 3 After sample determination 122 7 1 4 pH electrode 122 7 1 5 Filling boric acid into receiving vessel after last sample of rack was determined potentiometry only 123 7 1 6 Sample tube cleaning 124 7 2 Weekly maintenance 125 7 2...

Страница 8: ... 7 2 Cleaning the pH electrode 141 7 7 3 Replacing the buret 142 7 7 4 Cleaning the splash protector and the rubber seal 142 7 7 5 Glass parts 142 7 7 6 Troubleshooting the dosing unit 143 7 7 7 Adjusting the sample tube holder 143 7 8 Customer service 144 8 Troubleshooting 145 8 1 Problems that may occur 145 8 2 Error messages on the display of the K 375 149 8 3 Eliminating errors of the KjelSamp...

Страница 9: ...NGER CAUTION and WARNING are explained in chapter 2 1 1 Trademarks DURAN is a registered trademark of the SCHOTT AG Nylflex is a registered trademark of the Pedex Co GmbH 1 2 Abbreviations CSM Chopped Strand Mat ETFE Polytetrafluorethylene FEP Fluorinated Ethylene Propylene KCI Potassium chloride PCTFE Polychlorotrifluoroethylene PMMA Polymethyl methacrylate POM Polyoxymethylene PP Polypropylene P...

Страница 10: ... training or persons who are currently being trained require careful instruction The present Operation Manual serves as the basis for this 2 2 Proper use The device has been designed and built for laboratories It serves for nitrogen determination according to Kjeldahl The KjelMaster K 375 as stand alone device may also be used for distillations of steam volatile substances 2 3 Improper use Applica...

Страница 11: ...in serious injury or death CAUTION Indicates a hazardous situation which if not avoided may result in minor or moderate injury NOTICE Indicates possible material damage but no prac tices related to personal injury Supplementary safety information symbols may be placed in a rectangular panel on the left to the signal word and the supplementary text see example below Space for supplemen tary safety ...

Страница 12: ... accordance with current state of the art technology Neverthe less risks to users property and the environment can arise when the device is used carelessly or improperly The manufacturer has determined residual dangers emanating from the instrument if the device is operated by insufficiently trained personnel if the device is not operated according to its proper use Appropriate warnings in this ma...

Страница 13: ... the device or its components Do not drop the device or its components Keep external vibrations away from the instrument 2 5 2 Instrument related hazards CAUTION Risk of injury Never touch the surface of the touch screen with pointed or sharp objects Otherwise the screen might get damaged and splinter CAUTION Risk of burns by hot surface Surface temperature exceeds 60 C Do not touch hot surfaces o...

Страница 14: ...inity of the instrument damaged glass parts insufficient distance between the device and the wall see chapter 5 1 Installation site burns caused by contact with hot glass parts burns caused by contact with steam at the waste outlet defective transfer tube escape of steam and or sulfuric acid 2 5 4 Personal protective equipment Always wear personal protective equipment such as protective eye goggle...

Страница 15: ...ly not in use can be opened K 375 Protective door Safety appliance to protect users from burns at the splash protector distillation area which is hot during distillation Protective door sensors Prevents to start a distillation with the protective doors open and stops the distillation as soon as a protective door is opened during the process Sample tube sensor Prevents to start a distillation witho...

Страница 16: ...e for the proper condition of instrument This includes maintenance service and repair jobs that are performed on schedule by authorized personnel only Spare parts to be used Use only genuine consumables and spare parts for maintenance to assure good system perfor mance reliability and safety Any modifications of spare parts or assemblies are only allowed with the prior written permission of the ma...

Страница 17: ...ctor and potentiometric sensor 220 240 V 50 60 Hz 113751700 KjelMaster K 375 with glass splash protector and colorimetric sensor 220 240 V 50 60 Hz 113752700 KjelMaster K 375 with plastic splash protector and potentiometric sensor 220 240 V 50 60 Hz 113753700 KjelMaster K 375 with plastic splash protector and colorimetric sensor 220 240 V 50 60 Hz 113754700 KjelSampler K 376 Order number KjelSampl...

Страница 18: ...376 K 375 with plastic splash protector and colorimetric sensor K 375 220 240 V 50 60 Hz K 376 K 377 100 240 V 50 60 Hz 113754710 KjelMaster System K 375 K 377 Order number KjelMaster System K 375 K 377 K 375 with glass splash protector and potentiometric sensor K 375 220 240 V 50 60 Hz K 376 K 377 100 240 V 50 60 Hz 113751720 KjelMaster System K 375 K 377 K 375 with glass splash protector and col...

Страница 19: ...Sher 100 mL if device version with colori metric sensor is shipped 003512 5 Buffer set pH 4 and pH 7 3 x 20 mL each if device version with potentiometric sensor is shipped 043188 KCI electrolyte sat 250 mL if device version with potentiometric sensor is shipped 11059759 6 Connection grommet for Chiller 049151 7 Hose connector in line 11 13 for waste tank 043178 Hose chemical supply Nylflex length ...

Страница 20: ...st gauge sample tube holder 11059802 12 Tank 10 L 043410 13 Cap for 10 L tank large 025869 14 Cap for 10 L and 20 L tank small 043477 15 Tank labels 043434 Tank 20 L 043408 16 Cap for 20 L tank large 043478 17 Distance holder for dosing tip 043203 18 Mini gender changer 043108 Weighing boats 20 pcs 11060522 EPDM sealing for tanks 043048 Open end spanner 11058252 19 Tool SVL 22 11057779 20 CD KjelL...

Страница 21: ...le tube 500 mL 026128 2 Clamp ring 043238 3 Hose clamp 022352 4 Fastener for transfer tube K 376 only 043482 Sample tubes set of 4 300 mL 037377 5 Express rack 4 places K 376 only 11057711 6 Rack 20 places 11059831 7 Mains cable of the following types Type CH Type Schuko Japan Type GB Type AUS Type USA 10010 10016 17835 17836 33763 Test gauge for sample tubes 11058240 8 1 6 3 4 2 7 8 5 ...

Страница 22: ... Operation Manuals for K 375 Description Order number English 11593514 German 11593515 French 11593516 Italian 11593517 Spanish 11593518 Chinese 11593519 Japanese 11593520 Russian 11593653 KjelMaster K 375 Network Connection 11593539 KjelMaster K 375 Data Export 11593558 ...

Страница 23: ...9676 11 O ring level sensor 20 L tank 11058241 12 Buffer solution pH 4 250 mL 11064974 Buffer solution pH 7 250 mL 11064975 Temperature sensor for titrator 11056851 13 2 boric acid with Sher indicator 11064972 4 boric acid with Sher indicator 11064973 4 boric acid with bromocresol green methyl red indicator 11064976 Dosing unit for back titration 11056836 14 Driving motor for dosing unit 11056835 ...

Страница 24: ...3 Technical data K 375 K 376 K 377 Operation Manual Version E 24 2 7 15 17 16 18 13 14 8 10 9 3 4 5 11 12 1 6 19 20 ...

Страница 25: ...k for 12 sample tubes 500 mL 043970 2 Retainer plate holds tubes firmly in rack for machine washing 038559 3 Set of 10 boiling rods for digestion of samples with tendency of boiling retardation alternative for boiling chips 043087 4 Dip tube with cross slot for soil stone containing samples 047845 5 Glassfinger for sample tubes for soil samples 048638 6 1 4 5 6 2 3 ...

Страница 26: ...00 240 VAC 10 Frequency 50 60 Hz 50 60 Hz 50 60 Hz Power consumption max 2 2 kW max 150 W max 150 W Current consumption 230 V 9 5 A 650 mA 650 mA Weight 32 kg 40 kg without rack and sample tubes 64 kg without rack and sample tubes Dimensions W x H x D 458 x 670 x 431 mm 505 x 750 x 655 1000 mm height required to allow free movement of the sampler arm 1015 x 750 x 655 1250 mm height required to all...

Страница 27: ...ata titrator The following sensors can be connected to the titrator combined pH glass electrode optical sensor temperature measuring sensor for Resistance Thermometer Pt 1000 connection 2x4 mm sockets and 1 x 2 mm socket Dosing accuracy According to DIN EN ISO 8655 Part 3 or better Typical accuracy Fulfills ISO DIN 8655 3 regulation Measuring input pH mV input with 12 bit transducer for accurate r...

Страница 28: ...Protein factor 6 25 Sample size Boric acid concen tration Titrant concen tration Titrant volume 0 02 mg 20 ppm 1 0 g 2 3 g KCl L 0 005 N 2 mL 0 1 mg 100 ppm 1 0 g 2 0 005 N 3 mL 1 mg 0 2 1 0 2 g 2 0 01 N 8 mL 5 mg 1 6 0 5 g 2 0 1 N 4 mL 10 mg 1 6 1 0 g 4 0 1 N 8 mL 20 mg 2 13 1 0 g 4 0 1 N 14 mL 50 mg 5 31 0 4 g 4 0 1 N 14 mL 100 mg 10 63 1 0 g 4 0 5 N 14 mL 100 mg 20 0 5 g 4 0 5 N 14 mL 200 mg 20...

Страница 29: ... Material designation Housing sheet steel Note For the materials of the Dosing Unit please refer to its manual which is delivered together with dosing unit 3 4 2 Material on the K 375 Part Material Material code Housing Polyurethane PUR UL VO Glass parts Borosilicate glass 3 3 DIN ISO 3585 Insulation steam generator Ceramic fiber Multitherm 550 Steam generator housing Stainless steel 1 4301 Protec...

Страница 30: ...ainless steel 1 4301 L 314 Housing top cover Alu sheet AlMgSi1 Guide express rack PP PP Coating Polyester Epoxy PEP 31 Protective shield Polymethyl methacrylate Alu PMMA Alu Drip tray Polypropylene PP Housing y axle Alu sheet AlMgSi1 End cap y axle POM POM Dip tube PVDF PVDF Sealing cap EPDM EPDM Transfer hose linear PTFE PTFE Steam tube Silicone polyester MQ PU Protective hose PP PP Hose chain PA...

Страница 31: ...titration Automation of Kjeldahl determination is possible with the KjelSampler K 376 K 377 4 1 Device overview 1 KjelMaster K 375 2 KjelSampler K 376 3 Protective shield 4 Rack with sample tubes 5 Handle for protective shield 6 Transfer hose 7 Splash protector 8 Sample tube bracket 9 Sample tube 10 Protective door 11 Condenser 12 Receiving vessel 13 Touch screen with display 14 pH electrode or op...

Страница 32: ...ured with a sensor switch Electrical power is disconnected immediately when the service door is opened thus preventing electrical shock during maintenance To open the the service door for maintenance proceed as follows To open the service door pull the door lock 1 upwards open the door 2 Fig 4 2 Opening the service door ...

Страница 33: ...le tube in the K 376 K 377 via the steam hose The steam presses the sample into the dip tube so that the sample is transferred into the sample tube in the K 375 via the transfer hose Water and sodium hydroxide is dosed into the sample tube in the K 375 Then steam is introduced to drive out ammonia The ammonia evaporates into the splash protector and condensates in the condenser Boric acid is dosed...

Страница 34: ...4 Description of function K 375 K 376 K 377 Operation Manual Version E 34 Fig 4 4 Sample transfer principle Fig 4 5 Steam transfer during distillation ...

Страница 35: ...ting when the glass splash protector has cooled down The preheating time is predefined and can not be adapted 4 4 2 Priming Priming is used to prepare the entire system This preparation procedure includes distillation and titration with a clean and empty sample tube It is recommended to perform a priming at least once a day before starting analysis The priming method can be modified 4 4 3 Cleaning...

Страница 36: ...ation The measuring mode can be determined as endpoint or startpoint titration by defining the method in the K 375 The software of the K 375 allows to choose between standard and online titration Boric Acid Titration Boric acid adjusted to a pH of 4 65 is used as receiving solution to capture the nitrogen carried over as ammonia during the steam distillation The subsequent endpoint titration pH 4 ...

Страница 37: ... pH 4 65 before starting sample measurements This mode is more accurate and yields the highest accuracy Setpoint mV colorimetric The setpoint must be determined daily before the blank values and samples are colorimetrically tested and in addition if the distillation time the boric acid the indicator or the titrant is changed The setpoint determined is then used as the end point for the subsequent ...

Страница 38: ...rmination sample and reference substance Control blanks are performed to check the determination process for cross contaminations and are not used for calculation The determination and the definition of blank values is described in chapter 6 Operation 4 7 1 Blanks It is recommended to run blank values with exactly the same method as the subsequent samples The blank values may vary depending on the...

Страница 39: ...blank 4 8 Reference substances Reference substances are substances with known nitrogen content and serve to check the perfor mance of the system and the application It is recommended to analyze reference substances regularly For information on reference substances see table A check of the K 375 without digestion is done with a standardized ammonium salt e g ammonium di hydrogen phosphate In order ...

Страница 40: ...c titration an indicator must be added to the boric acid For optimal performance the Sher mixed indicator is recommended The point of inflection is depending on the indicator type as well as on the added indicator amount The Sher indicator shows best performance in terms of endpoint detection speed and reliability In boric acid the color changes from green pH 7 6 to blue 7 4 to 4 8 and finally to ...

Страница 41: ...quick method This fact permits an experimental determination of the ratio of total nitrogen or protein to ammonia nitrogen which is released by boiling in an alkaline solution Once the resulting conversion factor is determined a series of analysis can be carried out for control purposes without the time consuming digestion step The overall analysis is reduced to the following steps Sample addition...

Страница 42: ... content are obtained by dilution with distilled water Calculation Calculation of the protein content after factor determination g protein 100 mL Vsample Vblank xConv Fact Reg Fact Vsample Volume Titrant for sample determination in mL Vblank Volume Titrant for blank determination in mL Conv Fact Conversion factor for direct distillation Reg Fact Regression factor for direct distillation ...

Страница 43: ...be set up on a stable clean and level surface For safety reasons the distance between the back of the device and the wall or to another object must be at least 30 cm No containers chemicals or other objects must be located behind the instru ment The KjelSampler K 376 or K 377 is set up on the left side of the KjelMaster K 375 with a space of approximate 10 cm Make sure that the back of the KjelSam...

Страница 44: ...ic sensor Ind and Pwr Col or pH electrode Ind only m Connectors for temperature sensor Fig 5 1 Electrical connections of the K 375 NOTICE Risk of device damage by wrong voltage Make sure that the voltage on the socket corresponds to the voltage given on the type plate of the instrument Always connect the device to an earthed socket External connections and extension cables must be provided with an...

Страница 45: ...ear side of the housing 1 Power switch K 376 K 377 2 Power connection K 376 K 377 3 Fuses 2 x 3A 4 RS232 connection to K 375 5 Toggle switch see chapter 8 3 Fig 5 2 Electrical connections of the K 376 K 377 NOTICE Risk of device damage by wrong voltage Make sure that the voltage on the socket corresponds to the voltage given on the type plate of the instrument Always connect the device to an earth...

Страница 46: ...es premounted to the device WARNING Serious chemical burns by corrosives Risk of burns by hot steam Never operate the K 375 together with a sampler while the sample transfer and steam hoses are missing defective or incorrectly mounted Make sure there is always enough room for a free movement of the sampler arm if the sampler arm collides with any object during movement the transfer hose and or the...

Страница 47: ...on of the valve 1 attention 2 parts and take out the cutting ring 2 Slide the screw cap over the white hose 4 Slide the cutting ring over the hose Plug the hose on the valve and fix it by screwing the screw cap on the valve Fixing the steam hose to the K 375 Mount the red steam hose on the steam valve of the K 375 top right corner Slide the red hose on the connector and secure it with a hose clamp...

Страница 48: ...ng position is on the rear right side of the tray For the K 376 this is the fixed position to the right of the express rack The K 377 provides two washing positions one on the rear right side of each tray 5 3 2 Connecting the transfer hoses of the K 377 K 377 Connect the transfer hose and the steam hose to the two fittings on top of the sealing cap on the sampler arm Secure both connections with h...

Страница 49: ...ight on top Mount the white transfer hose on the valve using the provided screw connection 3 Mount the red steam hose on the steam valve and secure it with a hose clamp 4 5 4 Reagent water and waste connections NOTICE Risk of device damage by exceeding the maximum permissible pressure for the cooling water inlet Make sure never to exceed the maximum permissible pressure of 6 bar for the cooling wa...

Страница 50: ...ed in the standard delivery can be used to merge both tubes Cooling water connection Screw the cooling water hose to the cooling water inlet on the device side and connect it to the water supply The water pressure should not exceed 4 bar and the cooling water temperature should not exceed 25 C The flanged screw coupling for the water connection has a standard screw thread of G 3 4 Drain cooling wa...

Страница 51: ...the waste outlets and secure them with clamps The hose must be cut to appropriate length The drain hose is then connected to the tank by means of the straight connector and the screw cap including the sealing Alternatively the waste hose can also be guided into the sink Fig 5 7 Connection of the drain hose using the straight connector WARNING Risks and hazards for humans animals and the environmen...

Страница 52: ... is guided through a cut out in the housing at the rear side of the K 375 and must be connected to port Acid see chapter 5 2 1 Fig 5 10 Guidance of the cable through the cut out Fig 5 11 Connection of the cable of the driving motor The cable of an additional dosing unit for back titration can also be guided through the same cut outs in the housing NOTE In case the buret gets blocked refer to chapt...

Страница 53: ...h the bottom of the receiving vessel as this would block the outlet 5 7 Storage tank connection To connect the storage tanks proceed as follows Cut the Nylflex tube into pieces to the appropriate length Insert a PTFE suction tube into the Nylflex tube Push a EPDM sealing ring over the Nylflex tube Now fasten the tubes to the tank with the red screw cover The storage tanks should not be positioned ...

Страница 54: ...le tube or receiver waste Additional level sensors are available as optional equipment Each individual sensor is connected to the corresponding socket on the rear side of the device see section 5 2 1 The sensitivity of the capacitive level sensors can be adjusted to safely detect the liquid level if neces sary Assemble the level sensors according to the following picture Fig 5 14 Assembly of the l...

Страница 55: ... with the small adjustment screw of the sensor see 2 in figure 5 9 Front view Rear view The crosshair marks the sensitive area Status LED Adjustment screw b Fig 5 15 Fixing the level sensors NOTE The sensor detects a liquid when the red LED is off The level sensor for the waste tank must be set active within the Settings Peripherals screen See chapter 6 9 1 Settings This is not necessary for the o...

Страница 56: ...e bottom of the receiving vessel Risk of sensor damage by wrong storage Always store the pH electrode in the storage cap in saturated KCl solution 4 2 mol L A pH elec trode should not be stored dry as this would destroy the diaphragm If a pH electrode has been stored dry let it regenerate in saturated KCl for 24 hours or at least overnight prior to further use 5 9 2 Colorimetric sensor Fig 5 17 Co...

Страница 57: ... on the printer first followed by the K 375 5 10 2 Connecting a network cable Instead of storing data locally on the instrument it can also be stored on a network place A network cable can be connected to the device on the LAN port on the rear side For adapting the network settings refer to chapter 6 9 1 Settings Network More details regarding the network connection can be found in the document Kj...

Страница 58: ...laced in any other position 5 11 Preparing the system 5 11 1 Preparing the software In general it is recommended to check and adapt all device settings located under HOME Settings previous to the first use of the instrument Following a selection of the most common settings to be adapted is provided Define regional settings HOME Settings Regional settings Choose device language keyboard layout and ...

Страница 59: ...ose volume e g 50 mL Press START to start the calibration procedure Measure the actually dosed volume and enter it as calibration volume in the displayed screen Repeat the calibration procedure until the measured and the dosed volume correspond An acceptable difference at 50 mL is 5 mL NOTE H2O and NaOH can be dosed into the sample tube and then poured for measurement into a gradu ated cylinder Th...

Страница 60: ...perated via the touch screen To select a button or an input element in the dialog window you simply touch the screen using a soft blunt object or a fingertip CAUTION Risk of injury Never touch the surface of the touchscreen with pointed or sharp objects Otherwise the screen might get damaged and splinter 6 2 The home screen The central element of the user interface is the home screen Fig 6 1 The h...

Страница 61: ...selection Result Groups Create and view groups for the storage of your results Last Results View print or export the results of the last sample determinations Blank Correction Calculate mean blanks enter manual blanks or adapt the settings for the correction of blanks Determination Parameters All tasks related to the methods and the used solutions and substances Methods Create import edit and mana...

Страница 62: ...exception the START button will be switched to a PAUSE button during a running sequence Fig 6 3 Bottom bar 1 HOME this button will bring you back to the home screen from any other screen 2 SHOW HIDE STATUS shows or hides the Status view 3 READY STANDBY toggles the system mode between standby and ready In standby mode the steam generator is powered off for energy saving reasons 4 START PAUSE starts...

Страница 63: ...ssible via the button SHOW HIDE STATUS in the bottom bar 6 3 User concept The software distinguishes between three user types with differing access permissions Administrator no restrictions Operator limited permissions Lab Manager limited permissions Find the detailed user rights in the KjelMaster K 375 Compliance guide Pharma package available on the BUCHI website NOTE In case you forgot the pass...

Страница 64: ... of a small padlock NOTE Sample lists and sequences can be locked and unlocked by users with administrator rights therefore the check mark in front of the list or sequence has to be checked and the LOCK button has to be pressed Fig 6 5 Listed item 1 Check box for selecting an item 2 Padlock indicates items that can not be deleted 3 Arrow symbol indicates further screens belonging to the same item ...

Страница 65: ...ed amount per click can be adapted by a user with administrator rights under HOME u SETTINGS u Dosage volume in status view 2 Buttons for switching between RESULT CHART and INFO display 3 Status field indicates the system status and shows the active step of the running task 4 Progress indication for the running task remaining time titrated volume and measured pH 5 Information area shows last resul...

Страница 66: ... Orange the system is in standby mode The steam generator is powered off Blue the system is busy preparative task periodic task or sample determination running Red the system has an error or a system component is not ready 6 5 1 RESULT display The RESULT display of the Status view shows the last 3 results and the currently active blank together with its type and value ...

Страница 67: ...ual data export Each result that is exported automati cally will always contain the charts 6 5 3 INFO display The INFO display of the Status view shows all system and error messages 6 6 Determination In general there are three different ways for a sample determination with the KjelMaster K 375 Determination of single samples one by one without a sampler Determination of a predefined sample list on...

Страница 68: ...e 3 Enter data for the second sample 4 Determine the second sample 5 1 Enter data for all samples 2 Determine the first sample 3 Determine the second sample 4 1 Enter data for all samples 2 Determine the first sample 3 Determine the second sample 4 Descrip tion Without sampler Without sampler With KjelSampler K 376 K 377 NOTE Pressing the red STOP key on the touchscreen stops all processes immedia...

Страница 69: ...nd performed In addition periodic tasks like elec trode or pump calibration and certain manual tasks related to burets a sampler or pH measurement can be performed Preparative Tasks The System Preparation dialog is subdivided in two sections Preparative Tasks Preheating Priming Cleaning Aspiration Periodic Tasks Calibration pH electrode Setpoint colorimetric sensor Buret functions Pump calibration...

Страница 70: ...ntary sheet We recommend replacing the electrode if it does not fulfill the following criteria at 25 C room temper ature anymore Slope 95 105 Zero point pH 6 4 7 6 For pH electrodes other than the ones supplied by BUCHI additional criteria might be important NOTE It is recommended to use buffer solutions pH 4 00 and 7 00 For a 3 point calibration in addition the buffer solution for pH 9 21 is reco...

Страница 71: ...hod The selected method for Setpoint determination must be identical to the method used for sample determina tion The Setpoint should fulfill the following criteria Deviation between the last two Setpoints should not be more than 20 mV If Sher indicator is used you should work with a wavelength of 610nm in which case the setpoint is in the range of 300 500mV If bromocresol green methyl red indicat...

Страница 72: ...sage on the status view will inform the user if preheating is required If an auto sampler is configured under Settings select either Unit only or Via Sampler for Preheating cycle For Unit only only the glassware and tubing of the K 375 device is heated up With the option Via Sampler also glassware and tubing of a connected sampler can be included for the heat up procedure The duration of the prehe...

Страница 73: ... Priming cycle to Via sampler if the priming procedure should be performed via a present sampler Only visible if a sampler has been config ured under Settings The other parameter sets Distillation Parameters Titration Parameters and Aspiration Param eters are just the same like within a method A detailed explanation can be found in the section 6 8 1 Method Press START to start the priming procedur...

Страница 74: ...nit only to via sampler in this case the hoses from and to the sampler are also cleaned Press START to start the cleaning procedure Press FACTORY DEFAULTS to reset the settings of this screen NOTE If only one cleaning run is selected and no aspira tion no aspiration will be done at all If more than one cleaning run is selected and no aspiration the sample tube and the receiving vessel will be aspi...

Страница 75: ...matically during power on of the instrument Pump calibration Select the pump to be calibrated H2O NaOH or H3BO3 Enter the target Dose volume e g 50 mL Press START to start the calibration procedure Measure the actually dosed volume and enter it as calibration volume in the displayed screen Repeat the calibration procedure until the measured and the dosed volume correspond An acceptable difference ...

Страница 76: ...y positioned in For a 2 tray sampler it is also possible to move the arm of the sampler with Move to tray A from tray B to the zero position of tray A and vice versa Press START to move the arm to the selected posi tion Measuring pH or mV Using this functionality a direct measurement can be performed with the potentiometric or colorimetric sensor Select either potentiometric or colorimetric for th...

Страница 77: ... thought for a small amount of samples to be measured without a sampler present First of all the sample type has to be selected Blank Sample Reference substance or Control blank According to the selected type of sample different parameters are available For samples of type Blank press Name and enter a name for the blank result Press Method and select the method to be used for the determination of ...

Страница 78: ...he available result groups It is also possible to create a new result group using the New Group button For samples of type Reference Substance press Name and enter a name for the result of the reference substance determination Press Reference substance and select the refer ence substance from the list Press Sample weight and enter the weight of the sample in g or mL Press Method and select the met...

Страница 79: ... For samples in addition the weight and the protein factor have to be specified If a compatible balance is connected to the instrument the weight of each sample can be automatically taken over from this balance NOTE For each new sample the entries of the previously entered item are used as default values the default value for the name depends on the type of the sample in this case the name of the ...

Страница 80: ... User with administrator rights can also lock and unlock sample lists NOTE Locked sample lists can not be edited and the contained samples can not be determined but they can be used as template by copying them Within each sample list all contained samples are listed together with name type method and weight except blanks where no weight is needed Samples are added to the list with the NEW button A...

Страница 81: ...ons PREVIOUS NEXT POSITION it is possible to navigate from one set of sample parameters to the parameters of the previous or following sample in the list The first parameter for each sample is the sample type Blank Sample Reference substance or Control blank Press NEW to enter a sample of the selected type on the next position without leaving the screen With OK the sample is added to the actual po...

Страница 82: ...ailable result groups It is also possible to create a new result group using the New Group button For samples of type Sample press Name and enter a name for the sample result Press Sample weight and enter the weight of the sample in g or mL Press Protein factor and enter the protein factor for the determination of the results Press Method and select the method to be used for the sample determinati...

Страница 83: ...he list of the available methods Press Group and select a result group for the storage of the result from the list of the available result groups It is also possible to create a new result group using the New Group button For samples of type Control Blank press Name and enter a name for the control blank result Press Method and select the method to be used for the determination of the control blan...

Страница 84: ...nd configured under Device Settings Peripherals Sampler present If the sampler has been installed and prepared properly a sample series to be determined with a one or two tray sampler can be defined and pre programmed via a sequence A sequence contains a number of steps defining the samples itself and the necessary system tasks like preheating priming aspiration etc The following types of steps ma...

Страница 85: ...de This step cannot be changed NOTE The order of the steps can not be changed once they have been added to the sequence but steps can always be deleted and added again in a different order The tasks Preheating Priming and Cleaning are always performed via sampler if used within a sequence Even if those tasks are set to unit only within the area System Preparation this setting will be omitted Once ...

Страница 86: ...W NOTE Since the order of the steps can not be changed afterwards make sure to add the steps in a reason able order To change the order of steps within a sequence you have to delete selected steps and to add them again in a reasonable order NOTE Except the steps Rack 4 Rack 12 and Rack 20 none of the steps can be changed from within the sequence See the table at the beginning of this chapter for d...

Страница 87: ...ce to eliminate a faulty blank determination from the calculation before any sample determinations are corrected with the calculated blank The third setting is only available for 2 tray samplers Use tray in sampler A B Define the position of the rack in the K 377 sampler The step will be marked with A or B The positions of the rack can be filled one by one with samples by clicking on each position...

Страница 88: ...tion and the sample list is displayed again According to the selected type of sample a different set of parameters is offered For samples of type Blank press Name and enter a name for the blank result Press Method and select the method to be used for the determination of the blank from the list of the available methods Press Group and select a result group for the storage of the result from the li...

Страница 89: ...methods Press Group and select a result group for the storage of the result from the list of the available result groups It is also possible to create a new result group using the New Group button For samples of type Reference Substance press Name and enter a name for the result of the reference substance determination Press Reference substance and select the refer ence substance from the list Pre...

Страница 90: ...trol blank result Press Method and select the method to be used for the determination of the control blank from the list of the available methods Press Group and select a result group for the storage of the result from the list of the available result groups It is also possible to create a new result group using the New Group button ...

Страница 91: ... the balance mode is automatically left If certain samples of a rack that is already in prog ress have to be determined immediately this can be done using the Split Rack functionality Press PAUSE to stop the determination of the sequence Select the samples to be determined immediately and press SPLIT RACK The selected samples will be deleted from the sequence and will be inserted into the rack ste...

Страница 92: ...named and deleted by users with administrator rights User with operator rights are only allowed to create new result groups Using the FILTER button the list of the Result groups can be filtered with respect to the name and the creation date of the group Set the Group filter to On to filter the list of result groups Select Yes for Filter between dates if you wish to filter the list with respect to ...

Страница 93: ...n be filtered Enter a sample group to set the sample filter Press FILTER to set the sample filter Set the Sample filter to On to filter the list of displayed results Select Yes for Filter between dates if you wish to filter the list with respect to the creation date and specify a time period using begin and end date The list of displayed results can be restricted to one or more certain types of re...

Страница 94: ...e sample report of selected results can be printed either detailed or short Results can be exported to a USB stick or a network place NOTE The last results are shown regardless of the result group they are assigned to Clicking on a single result opens the detailed sample report With PREVIOUS SAMPLE and NEXT SAMPLE you can navigate back and forth within the sample reports of the stored samples ...

Страница 95: ... maximum number of 90 blanks can be listed In general four different possibilities for the determination of the active blank value for the automatic correction of results are available Blank values can be measured type measured Blank values can be entered manually type manual Blank values can be calculated as mean value of freely selectable measured blanks type mean Blank values can be determined ...

Страница 96: ...n in the list of blanks in the Blank Correction screen Manually entered blanks are listed in the blank list with type manual NOTE If you select Yes for Use last measured blank the next measured value for a sample of Type Blank will be used for the correction of all subsequent sample determinations All sample determinations up to the next blank determination will still be corrected using the curren...

Страница 97: ...ll be used for the calculation of the mean value Confirm your selection with OK The calculated mean blank value is now automatically selected and shown in the list of blanks in the Blank Correction screen Averaged blanks are listed in the blank list with type mean NOTE If you select Yes for Use last measured blank the next measured blank value will be used for the correction of all subsequent samp...

Страница 98: ...RESULT display of the status view NOTE If you select Yes for Use last measured blank the next measured blank value will be used for the correction of all subsequent sample determinations All sample determinations up to the next blank determination will still be corrected using the currently selected blank value Monitoring the blank limits If the function Monitor blank limits is switched on a toler...

Страница 99: ...or single samples or sample lists those tasks have to be performed manually previous to a sample determination See chapter 6 6 1 System Preparation For sequences automated determina tion of sample racks with a sampler the system preparation tasks can be defined within the Sample Sequence previous to or after the determination of a complete rack see chapter 6 6 4 Sequences Within the Methods screen...

Страница 100: ...ersion E 100 The different areas of the method are separated from each other by the corresponding heading The Method Information section at the bottom of each method provides information about the last modifi cation date and the creator of the method ...

Страница 101: ...ralization Parameters for Step 3 Steam distillation For the mode of the steam distillation either Auto matic IntelliDist or Fixed time can be selected Automatic potentiometry only The countdown of the specified distillation time is not started until the first amount of nitrogen reaches the receiver vessel indicated by an increase of the pH value The variable heat up time is excluded from the disti...

Страница 102: ...lication either a back titration or a boric acid titration can be performed BUCHI recommends the use of the boric acid titration If no titration at all shall be performed None can be selected for the parameter Titration type The boric acid titration can be performed either with a potentiometric or a colorimetric sensor for the back titration only the potentiometric sensor can be used Select None f...

Страница 103: ...lutions The exact amount of the provided receiving solution can be entered using the Receiving solution volume parameter In addition the stirrer speed for the titration and a titration start volume can be specified The speci fied titration start volume is dosed into the receiving vessel previous to the titration The sensor type cannot be changed for the back titration With the parameter Titration ...

Страница 104: ...lay of 90 seconds Standard The titration is started sequential after the distillation is finished Furthermore the stirrer speed for the titration and a titration start volume can be specified The speci fied titration start volume is dosed into the receiving vessel at the beginning of the titration when samples are analyzed With the parameter Titration algorithm one of two available algorithms for ...

Страница 105: ...an be determined Startpoint the endpoint pH value is determined by a measurement of the boric acid in the receiving vessel previous to the distillation process Endpoint the endpoint pH value can be entered as number using the parameter Endpoint pH Furthermore the stirrer speed for the titration and a titration start volume can be specified The speci fied titration start volume is dosed into the re...

Страница 106: ...ard for a determination with a previous digestion or Direct distillation for a determination without previous digestion For a direct distillation an additional factor and regression factor can be specified for result calcula tion NOTE The result for a direct distillation is calculated following the linear equation y a x b where a is given by the direct distillation factor and b by the regression f...

Страница 107: ...the sample tube Click on Aspiration receiving vessel and select Yes to switch on the automatic aspiration of the receiving vessel NOTE If you select the automatic aspiration of the sample tube and or the receiving vessel and the waste is collected we recommend the use of level detectors for the corresponding waste container s The level sensors can be configured within the Settings Peripherals scre...

Страница 108: ... be referenced and used from within a method Create a new volumetric solution using a unique name or delete or rename an existing one NOTE Volumetric solutions marked with a small padlock are predefined and cannot be deleted Only the Titer can be adapted for those solutions For each solution molarity valence factor and titer or normality and titer can be specified for latter one Type Based on norm...

Страница 109: ...r information on reference substances see table in chapter 4 8 Reference substances In the following the steps necessary for defining reference substances are described Create a new reference substance with a unique name or delete or rename an existing one NOTE Reference substances marked with a small padlock are predefined and cannot be deleted or changed For each reference substance a theoretica...

Страница 110: ...ettings Adapt Language Keyboard layout and Time and Date format Date and time Set system Date Time and Time zone Display and sound Adapt Display and Sound settings Result units Select or define the Result units Dosage volume in status view Define the increments for direct dosing in the status view for H2O NaOH and H3BO3 Peripherals Configure the present Peripherals like Level sensors Sampler Balan...

Страница 111: ...e Date format can be switched to Month Day Year Day Month Year or Year Month Day with a slash dot or hyphen as separator The time can be displayed either in 12 hour or in 24 hour format Date and Time Set Date and Time and select your Time zone Display and sound Adapt the brightness of the display and set the switch off time screen saver Set the sound volume and select if there should be an acousti...

Страница 112: ...Enter a correction factor and or correction offset if necessary and select the preferred number of decimal places The results are calculated following the linear equa tion y a x b where a is given by the correction factor and b by the correction offset Dosage volume in status view Set the increment in mL click for the direct dosing of H2O NaOH and H3BO3 within the status view Per click on the corr...

Страница 113: ... is strictly necessary to select Yes for Chiller used in order to have the cooling water valve permanently opened If a sampler is connected to the instrument select the type 1 tray for K 376 2 trays for the K 377 and enable or disable the auto cleaning functionality of the sampler after each sample measurement If a balance is connected to the instrument specify the communication settings for the b...

Страница 114: ...twork or USB printer the paper format and the color mode monochrome CMY or CMYK For a network printer in addition the IP address has to be specified NOTE If no printer is available you may select Adobe PDF as printer type the data is then stored as a pdf file on a USB stick Network If connected to a network you can assign a device name for the device to be recognized within the network The IP addr...

Страница 115: ...using xml format Most LIM systems are able to handle this format If more details regarding the data format are required refer to the document Manual Data export K 375 which can be obtained from any authorized BUCHI representative User administration Create delete or rename users Assign user rights to each user NOTE The first created user has to be of type Adminis trator After different users have ...

Страница 116: ...played indicating the necessity of an equipment service The criteria next service date number of performed determinations between two services or both can be determined under Notification options within the same dialog If a specified criterion is fulfilled a notification message is displayed on the Info display of the Status view See also section 6 5 The Status view If both criteria are selected t...

Страница 117: ...se USB backup device and or YES for a Use network backup share Specify the path to the USB and or network directory For the network share the IP address name domain and User name and password have to be specified NOTE For the network settings configuration the help of an IT specialist of the company may be required Lab timer Create or delete a timer and define the count down time Start or Stop the...

Страница 118: ...cked Each item is displayed in a list and if currently active a green dot is displayed in front of it With the button SERVICE MODE one can switch to the service mode to actively set each system component into operation and check it for proper functioning NOTE The diagnostics dialogs are only accessible for user with administrator rights For users with operator rights the diagnostics area is read o...

Страница 119: ...ath or serious injuries by contact with high voltage All maintenance and repair work requiring the opening or removal of device covers may only be carried out by trained personnel and with the tools provided for this purpose Prior to all maintenance work on the device switch off the power supply and remove all sources of flammable vapor Only open the housing of the product while the device is swit...

Страница 120: ...mes obvious the maintenance work must be carried out immediately 7 1 Daily maintenance 7 1 1 Before sample determination potentiometry Remove the electrode from the storage cap the cap can be fixed to the electrode holder on the front side of the housing and place it into the receiving vessel Rinse the titration hoses Path System Preparation Buret functions Buret function Dose Calibrate the pH ele...

Страница 121: ...minations as described in chapter 6 6 1 System Preparation Path System Preparation Setpoint colorimetric sensor Prime the system Path System Preparation Priming see also chapter 6 6 1 System Prepara tion Submerge the sensor into the measuring medium at least up to the measuring cell NOTE All glass parts must be warm before the analysis begins Therefore a preheating of the system is necessary if mo...

Страница 122: ...volume of water in System Preparation Cleaning H2O volume 7 1 3 2 Cleaning of the pH electrode Rinse off the pH electrode with distilled water do not wipe it off but carefully sponge off excess droplets Place the pH electrode into the storage cap the pH electrode must be stored in saturated KCl solution 4 2 mol L 7 1 4 pH electrode Storage The pH electrode must be stored in saturated KCl solution ...

Страница 123: ...meters to your needs press START and follow the SOP given by the software Details about all available parameters can be found in chapter 6 6 1 System preparation 7 1 5 Filling boric acid into receiving vessel after last sample of rack was determined potentiometry only By default the pH electrode has to be stored in saturated KCl solution Keeping the electrode for a long time in air reduces its lif...

Страница 124: ...ng button provided in the status view refer to 6 5 The status view 7 1 6 Sample tube cleaning NOTICE Risk of sample tube damage Sample tubes can break due to mechanical or temperature shocks 1 Do not cool down sample tubes with cold water 2 Do not place hot sample tubes and the rack on a cold surface Single tube Place the sample tube into the dishwasher to prevent any damage Make sure the sample t...

Страница 125: ...stains 7 2 2 Cleaning the titrator Clean the housing of the titration unit with a moist piece of cloth with normal household cleaning agents Treat the bottom and rear side dry In no case must liquid penetrate into the interior of the titra tion unit 7 2 3 Cleaning the glass parts of the dosing unit Please refer to the manual for the dosing unit for cleaning instructions After cleaning and complete...

Страница 126: ...s is only a guideline please verify and use your specific purity of the reference substance There fore check the respective Certificate of Analysis which is delivered from the manufacturer of the reference substance and create a modified reference substance according to it Parameters for checking the digestion distillation and titration with glycine Check Digestion distillation and titration Refer...

Страница 127: ...the surface getting scratched Exchange the mesh when it is deformed 7 3 Monthly maintenance 7 3 1 Calibrating the pump It is recommended to calibrate the pumps with the same volume as used for the methods To perform the calibration a graduated cylinder is needed Example H2O pump Path System Preparation Pump Calibration Select H2O for Pump Enter the quantity to be dosed e g 50 mL for the parameter ...

Страница 128: ...ume mL screen The value shown for Calibration volume is updated NOTE Repeat this procedure until the entered and the dosed volume correspond An acceptable difference at 50 mL is 5 mL H2O and NaOH can be dosed into the sample tube and then poured into a graduated cylinder for measurement The H3BO3 can be dosed directly into the receiving vessel and then poured into a graduated cylinder ...

Страница 129: ...H2O volume 0 mL NaOH volume 0 mL Reaction time 0 s Distillation mode Fixed time Distillation time 300 s Stirrer speed distillation 5 Steam output 100 Titration type None Aspiration sample tube Yes Aspiration receiving vessel No Run the method with an empty sample tube and empty receiving vessel Measure the distilled quantity in the receiving vessel using a graduated cylinder NOTE The distillate am...

Страница 130: ...vely the maintenance interval must be reduced accordingly 7 3 5 Inspecting the sample tubes Sample tubes are subject to wear and tear especially due to the impact of NaOH and also caused by cleaning in a dish washer To avoid leaks during distillations it is recommended to check each tube with the supplied test gauge and to sort out the ones not passing all criteria Follow the instructions given on...

Страница 131: ...n E 131 Check all glass parts for scratches 1 or chips 2 NOTE Sample tubes with scratches or chips can break during determinations Results Glass parts show no damage The glass parts are O K Glass parts have scratches 1 or chips 2 Replace faulty glass parts ...

Страница 132: ...ng The screw cap shall only be tightened hand tight Use the open end spanner 11058252 contained in the standard delivery of the device to loosen the screw cap holding the sealing Unscrew the screw cap by hand Carefully take the screw cap with the sealing away from the device and replace the sealing along with the inner fixation ring Reassemble in reversed order NOTE Depending on sample throughput ...

Страница 133: ...mend to replace it every half year together with the sealing cap CAUTION Risk of burns by hot surface Always let the device cool down after operation before touching the dip tube the sealing or the transfer and steam hoses Take the sample rack away from the tray Move the sampler arm to the service position System Preparation Sampler functions Move to service position The dip tube can be pulled out...

Страница 134: ...mpler functions Move to zero position Reinstall the sample rack NOTE Depending on sample througput and instrument care an exchange of the sealing cap should be consid ered after around 2000 distillations If steam leaks the sealing cap needs to be exchanged immediately 7 4 3 Replacing the splash protector Replace the glass splash protector after approximately 3000 distillations at the latest after ...

Страница 135: ...anual Version E 135 WARNING Death or serious injuries by contact with high voltage Make sure device is switched off and unplugged before replacing the pump Open the service door Disconnect the water connection 1 Disconnect the NaOH connection 2 ...

Страница 136: ... from the instrument and replace it with a new one Reassemble in reverse order 7 5 Yearly maintenance 7 5 1 Replacement of wear parts Replace the following components Seals including the sealing cap of the sampler and the splash protector seal NaOH pump and boric acid pump the other pumps as required Dip tube pH electrode if required depending on sample throughput and maintenance of the pH electro...

Страница 137: ... stops running Let the solution dissolve the lime for 0 5 1 hour Remove the solution of the steam generator see step 1 and 2 Perform a second decalcification see step 5 10 Connect the hose from the water tank with the pump for H2O Flush the steam generator 2 3 times with distilled water see step 6 8 and 10 Perform 2 3 times a CLEANING cleaning procedure of the instrument 7 5 3 Replacement of the s...

Страница 138: ...rs 1 Note for reassembly The upper one connects the green cable the lower one the brown cable Disconnect the tube on the front side 2 Unscrew the two screws 3 from the front panel and take the front panel away The pump becomes loose now and can be replaced Reassemble in reversed order 7 5 3 Replacement of the wave spring Remove the rack and move the sampler arm to the service position Remove the d...

Страница 139: ...s chemical burns by corrosives Risk of burns by hot steam Never operate the K 375 together with a sampler while the sample transfer and or steam hose is getting porous or cracked WARNING Serious chemical burns by corrosives Always wear protective goggles Always wear protective gloves Always wear protective clothes The transfer connection consisting of the transfer hose the steam hose and the black...

Страница 140: ... room temperature Loosen the connections of the transfer hose and the steam hose on the rear side of the K 375 see chapter 5 3 2 for details Loosen the protective sleeve and the connections for the steam hose and the transfer hose on the sampler arm of the KjelSampler see chapter 5 3 1 for details Take the transfer connection away from the devices and replace it with a new one ...

Страница 141: ...the shaft 4 to the hose 1 Slip the distance holder 3 onto the shaft Push the slip on tip 5 onto the end of the shaft 7 7 2 Cleaning the pH electrode If the glass membrane or diaphragm are dirty clean them to maintain the measuring function Depending on the degree of contamination submerge only the glass membrane or the glass membrane with the diaphragm into the cleaning solution Depending on the d...

Страница 142: ...ination was not removed during the daily maintenance work proceed as follows Dismount the splash protector and remove the rubber seal Rinse the splash protector with water to remove sample residues We recommend to replace the glass splash protector after approximately 3000 5000 determi nations depending on the kind of application and frequency of maintenance The plastic splash protector can last m...

Страница 143: ...distributor disc remedying the adherence of both is explained in chapter 4 1 3 Discs adhere to one another 7 7 7 Adjusting the sample tube holder In case the K 375 does not detect the sample tube displaying ther error message 10102 No sample tube present or if leaks are observed the sample tube holder needs to be adjusted To adjust the sample tube holder the adjustment gauge 11059802 is needed Fig...

Страница 144: ...ustment of the sample tube holder does not remedy the problem it may be necessary to exchange the sample tube holder and or the splash protector seal 7 8 Customer service Only authorised service personnel are allowed to perform repair work on the instrument These persons have a comprehensive technical training and knowledge of possible dangers which might arise from the instrument Addresses of off...

Страница 145: ...team generator by pushing the Ready button No sample transfer from K 376 K 377 to K 375 Check the system for leakages K 376 K 377 K 375 and transfer tubes connections Check the position of the dip tube on the K 376 K 377 distance between sample tube bottom and dip tube must be about 2 mm If necessary adjust the dip tube accordingly Check the system by means of a Priming If this does not help check...

Страница 146: ...used for dilution Other problems that may occur Problem Cause Corrective measure Nitrogen content too high Air in titration system buret tubes Carry over during distillation Wrong titrant Error in calculation Defective pH electrode Defective colorimetric sensor Dirty glassware Air bubbles disturb the colori metric titration Refill buret Use less volume or increase water volume for dilution Use rig...

Страница 147: ...pH electrode Defective colorimetric sensor Dirty glassware Air bubbles disturb the colori metric titration Increase digestion time Increase volume Correct ratio Not more than 200 mg Nitrogen per sample tube Correct volume until color change is visible Check and tighten check connection between condenser and splash protector replace seal if required Check sealing and scrubber suction capacity Check...

Страница 148: ...ri metric titration Incorrect positioning of the titration dosing tip Indicator aging Incorrect ratio of indicator to boric acid or incompatible indicator used Loose contact of the sensor cables Fix tubing and refill buret Check for leaks and fix Calibrate electrode with fresh buffer Perform Setpoint determina tion Homogenize sample Use weighing boats to improve procedure Check color of samples du...

Страница 149: ...perating mode 10 011 Real time clock battery is low Date and time have been reset Please set correct date and time in settings Change of battery is recommended Exchange the battery 10 101 Door is open Close the door 10 102 No sample tube present Attach sample tube or adjust sample tube holder 10 103 Tube shield open Close tube shield 10 104 Preheating recommended Perform preheating 10 105 Cleaning...

Страница 150: ...t of order Faulty valve or wire harness Call service 12 002 Valve cooling water in Y5 out of order Faulty valve or wire harness Call service 12 003 Valve sampler steam Y6 out of order Faulty valve or wire harness Call service 12 004 Valve sampler transfer Y7 out of order Faulty valve or wire harness Call service 12 005 Valve 5 not used out of order Faulty valve or wire harness Call service 12 006 ...

Страница 151: ...eed 14 010 Titrator module could not create service 11 Distillation unit needs to be switched off and on 14 011 Titrator module could not create service 21 Distillation unit needs to be switched off and on 14 012 Titrator module could not create service 41 Distillation unit needs to be switched off and on 14 013 Titrator module could not create service 3 Distillation unit needs to be switched off ...

Страница 152: ...ervice 15 103 Sampler Tube not found Put sample tube in place or call service 15 104 Sampler Tube not released Remove sample tube or call service 15 105 Sampler Error 5 reserve does not exist Call service 15 106 Sampler Error 6 reserve does not exist Call service 15 107 Sampler Shield not locked Call service 15 108 Sampler Error reference position Call service 15 109 Sampler zeroadjustment not pos...

Страница 153: ...exact posi tion proceed as follows Close the protective shield Press the toggle switch at the back and hold it until the sampler arm is in the upper end position NOTICE Risk of device damage There is no mechanical end stop for the sampler arm movement Only keep on pressing the toggle switch until the sampler arm is slightly above the rack to be able to move the sampler arm If an error on the K 376...

Страница 154: ...e hose is not immersed deep enough into the reagent bottle Immerse the hose deeper into the bottle or fill up reagents The buret is not properly locked Lock the buret Air bubbles in the titration system Possible reasons Action remedy The hose connections are not tight Check whether the hose has been pulled out of the threaded connection and screw it on manually Replace the hoses including the thre...

Страница 155: ...ide dosage must be rinsed thoroughly with distilled water 9 1 Emptying the steam generator To empty the steam generator proceed as follows Turn off the instrument Let the steam generator cool down for 30 minutes CAUTION Risk of burns by hot surface The steam generator heats up during operation Always let the device cool down after operation before opening the service door Open the service door Att...

Страница 156: ...ce and clean it thoroughly Store and transport the device in its original packaging NOTE Move the K 376 sampler arm to the washing position for transport 9 4 Disposal To dispose of the device in an environmentally friendly manner a list of materials is given in chapter 3 This helps to ensure that the components are separated and recycled correctly Make especially sure to dispose of the gas springs...

Страница 157: ...bes set of 20 300 mL 11059690 1 Sample tubes set of 4 graduated 300 mL 43049 2 Sample tubes set of 4 100 mL 11057442 3 Sample tubes set of 4 500 mL 43982 4 Receiving vessel 340 mL 43333 5 Receiving vessel 420 mL 43390 6 Receiving vessel optical sensor 11068263 O ring 190 1 x 3 53 EPDM 75 049767 7 O ring 247 2 x 3 53 EPDM 11058241 Buffer solution pH 4 250 mL 11064974 8 Buffer solution pH 7 250 mL 1...

Страница 158: ...rotor blade colorimetric titration 11068266 Stirrer complete 11056590 23 Dosing unit 20 mL 11056836 24 Driving motor for dosing unit 11056835 25 Colorimetric sensor with cable 11066601 26 Drip tray 11057428 27 Seals for cooling water hose set 040043 Hoses for receiver FEP set 043191 Titrator dosing tip 11058745 Accessory kit for colorimetric sensor 11068260 Receiving vessel optical sensor 11068263...

Страница 159: ...9 Shutdown storage transport and disposal K 375 K 376 K 377 Operation Manual Version E 159 14 18 22 26 23 27 24 25 19 20 21 15 16 17 28 ...

Страница 160: ...mplete for K 376 for K 377 11059035 11059036 1 2 Dip tube 11056031 Dip tube with cross slot 00047845 Drip tray K 376 K 377 00043827 Sealing cap 11057284 3 10 3 Hosing connection scheme Kjeldahl Sampler System K 375 K 376 DVWH 1D2 2 2 DVWH 97 97 2 CAPTION Fig 10 1 Hosing connection scheme Kjeldahl Sampler System K 375 K 376 Standard 1 2 3 ...

Страница 161: ...e harmful interference in which case the user will be required to correct the interference at his own expense Français Cet appareil a été testé et s est avéré conforme aux limites prévues pour les appareils numériques de classe A et à la partie 15 des réglementations FCC ainsi qu à la réglementation des interférences radio du Canadian Department of Communications Ces limites sont destinées à fourn...

Страница 162: ...ia BUCHI India Private Ltd IN Mumbai 400 055 T 91 22 667 75400 F 91 22 667 18986 india buchi com www buchi com in en Indonesia PT BUCHI Indonesia ID Tangerang 15321 T 62 21 537 62 16 F 62 21 537 62 17 indonesia buchi com www buchi com id in Japan Nihon BUCHI K K JP Tokyo 110 0008 T 81 3 3821 4777 F 81 3 3821 4555 nihon buchi com www buchi com jp ja Korea BUCHI Korea Inc KR Seoul 153 782 T 82 2 671...

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