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9 | Carrying out a determination

Büchi Labortechnik AG

78/106

Operation Manual K-365 Dist Line

9

Carrying out a determination

9.1

Preparing the instrument

Navigation path

 

Precondition:

R

All commissioning operations have been completed. See Chapter 5 "Installation",
page 29

u

Set the On/Off master switch to On.

ð

The instrument is starting up.

u

Make sure that no defective sealings or glass parts are used.

u

Navigate to the 

Home

 menu according the navigation path.

u

Tap the 

[READY]

 button on the function bar.

ð

The instrument is heating up.

u

Install a receiving vessel (EasyDist and BasicDist only). See Chapter 8.9 "Installing
a receiving vessel", page 73

u

Install the sample tube. See Chapter 8.8 "Installing the sample tube", page 72

u

Close the protection shield.

u

Flush the tubing. See Chapter 8.13 "Dosing manually", page 74

u

Aspirate the receiving and the sample vessels. See Chapter 8.14 "Aspirating
manually", page 75

9.2

Starting a determination

Navigation path

 

Precondition:

R

The instrument is prepared. See Chapter 9.1 "Preparing the instrument",
page 78

R

The sample is prepared.

R

The connected instruments are prepared (MultiDist T only). See related
documentation.

u

Navigate to the 

Home

 menu according the navigation path.

u

Press the 

[PREP]

 button on the function bar.

ð

Wait until the status bar shows the status READY.

u

Select the operation mode. See Chapter 8.12 "Selecting the operation mode",
page 74

u

Tap the 

[START]

 button on the function bar.

Содержание K-365 Dist Line

Страница 1: ...K 365 Dist Line Operation Manual 11594193 B en...

Страница 2: ...the right to make changes to the manual as deemed necessary in the light of experience especially with respect to structure illustrations and technical details This manual is copyrighted Information f...

Страница 3: ...isks 12 2 8 1 Hot surfaces 13 2 8 2 Faults during operation 13 2 8 3 Glass breakage 13 2 8 4 Not suitable titrators 13 2 8 5 Dosing pump defect 13 2 9 Modifications 13 3 Product description 14 3 1 Des...

Страница 4: ...the level sensor on the canister option 35 5 13 Installing a titrator with LAN MultiDist T with Eco Titrator only 35 5 14 Installing a titrator with RS232 MultiDist T only 36 5 15 Installing a dispen...

Страница 5: ...ging the reaction detection for a method option for MultiDist only 61 8 6 5 Changing the H O volume for a method MultiDist only 62 8 6 6 Changing the H SO volume for a method MultiDist only 62 8 6 7 C...

Страница 6: ...mple tube manually 75 8 14 2 Aspirating the receiving vessel manually 76 8 15 Changing the stirring speed manually 76 8 16 Switching valve adjustment MultiDist only 76 9 Carrying out a determination 7...

Страница 7: ...er 84 10 13 Cleaning and servicing the steam generator 85 10 14 Calibrating the pumps 85 10 14 1 Calibrating the H O pump 85 10 14 2 Calibrating the acid pump 86 10 14 3 Calibrating the NaOH pump 86 1...

Страница 8: ...1 Accessories 99 13 1 2 Splash protector spare parts 100 13 1 3 Tank spare parts 101 13 1 4 Condenser spare parts 101 13 1 5 Titration spare parts 102 13 1 6 Sample tubes 103 13 1 7 Cable and tubing 1...

Страница 9: ...character draws attention to a requirement that must be met before the instructions below are carried out u This character indicates an instruction that must be carried out by the user This character...

Страница 10: ...nd are therefore exposed to greater dangers The device may only be operated by suitably qualified laboratory staff These operating instructions are aimed at the following target groups Users Users are...

Страница 11: ...s in this document Warning notices warn you of dangers that can occur when handling the device There are four danger levels each identifiable by the signal word used Signal word Meaning DANGER Indicat...

Страница 12: ...tion devices 3 1 2 Fig 2 Protection devices 1 Protection shield 2 Protection shield 3 Stop button 2 8 Residual risks The device has been developed and manufactured using the latest technological advan...

Страница 13: ...are not in use Always visually inspect glass components for damage every time they are to be used Do not continue to use glass components that are damaged Always wear protective gloves when disposing...

Страница 14: ...l and Devarda methods MultiDist Steam is introduced into the sample solution to drive out volatile components After condensation in condenser the condensate is collected in a receiver solution 3 2 Con...

Страница 15: ...ne 15 106 4 3 5 9 8 7 1 2 6 Fig 3 Front view 1 Splash protector 2 Condenser 3 Ventilation slots 4 On Off master switch 5 Ventilation slots 6 Receiving area See Chapter 3 2 3 Receiving area page 16 7 S...

Страница 16: ...ation slots 4 Dosing pumps window 5 Connections on the rear side See Chapter 3 2 5 Connections on the rear side page 20 6 Steam valve 7 Cooling water out 8 Drain connection according to the instrument...

Страница 17: ...Receiving vessel area Receiving area MultiDist T only 4 6 5 7 11 10 9 1 2 3 8 Fig 6 Receiving area 1 Cable duct reaction detection sensor 2 Condenser outlet tubing 3 Rear cable duct 4 Tubing for bori...

Страница 18: ...3 4 7 1 5 6 Fig 7 Communication connections 1 BUCHI standard communication port COM marked COM 2 BUCHI standard communication port COM marked COM 3 Level detection sensor port marked Level Detection...

Страница 19: ...communication port COM marked COM 3 BUCHI standard communication port COM marked COM 4 Level detection sensor port marked Level Detection 5 H O tank level sensor port marked H O 6 Waste tank level se...

Страница 20: ...tirrer port marked Stirrer 6 Level detection sensor port marked Level Detection 7 H O tank level sensor port marked H O 8 H BO tank level sensor port marked H BO 9 Waste tank level sensor port marked...

Страница 21: ...H O supply for steam generation Connections on the rear side BasicDist option The connections are located at the rear side of the instrument See Chapter 3 2 2 Rear view page 16 1 2 3 4 5 Fig 11 Connec...

Страница 22: ...Reserve 5 Reserve 6 Acid supply for sample tube Connections on the rear side MultiDist The connections are located at the rear side of the instrument See Chapter 3 2 2 Rear view page 16 2 3 4 5 6 1 F...

Страница 23: ...eceiving vessel 2 Waste pump for sample tube 3 H O supply for sample tube 4 H O supply for steam generation 5 Boric acid supply 6 NaOH supply for sample tube 7 Acid supply for sample tube 3 3 Scope of...

Страница 24: ...ata 3 5 1 K 365 Dist Line EasyDist BasicDist MultiDist Dimensions W x D x H 320 x 400 x 730 mm 320 x 400 x 730 mm 320 x 400 x 730 mm Weight 23 kg 23 kg 23 kg Connection voltage 220 240 10 VAC 220 240...

Страница 25: ...c distillation analyte specific analyte specific N 0 8 Instrument specifications EasyDist BasicDist MultiDist Distillation capacity 100 40 mL min 40 mL min 40 mL min Distillation capacity 10 12 5 mL m...

Страница 26: ...uage en de fr it es pt ja zh ru pl ko id en de fr it es pt ja zh ru pl ko id 3 5 2 Ambient conditions For indoor use only Max altitude above sea level 2000 m Ambient and storage temperature 5 40 C Max...

Страница 27: ...fely The installation site has an own mains outlet socket for the instrument The installation site allows that the power supply can be disconnected at any time in an emergency The installation site is...

Страница 28: ...ll glass components for damage u Damage that has occurred in transit should be reported to the carrier u Keep packaging for future transportation 4 2 Storage u Make sure that the ambient conditions ar...

Страница 29: ...I power supply cables Precondition R The electrical installation is as specified on the type plate R The electrical installation is equipped with a proper grounding system R The electrical installatio...

Страница 30: ...the connection marked Cooling Water Chiller IN u Install the drain hose to the connection marked OUT Cooling Water Chiller u Put the other end of the hose in a sink 5 4 2 Installing the recirculating...

Страница 31: ...he drain tubing option u Install the drain hose to the connection marked Drain u Place the other end of the hose in an aqueous waste container located lower than the instrument 5 6 Installing the wast...

Страница 32: ...device 5 8 Installing the H O supply for steam generation NOTE MultiDist only The water supply comes from one canister Precondition R The water complies with the specified parameters See Chapter 3 5 T...

Страница 33: ...MultiDist T only u Install the inlet hose onto the connection marked NaOH Sample Tube IN u Attach the inlet hose in place with a hose clip u Moist the aspiration hose u Push the hoses together 20 mm...

Страница 34: ...the inlet hose into the H BO 5 11 Installing the H O supply for the sample tube MultiDist MultiDist T only NOTE MultiDist only The water supply comes from one canister u Install the inlet hose to the...

Страница 35: ...gnetic field in the frequency range of 2 to 10 MHz u Attach the hook and loop fastener sticker to the sensor u Attach the strap to the canister u Fix the sensor on the canister u Connect the sensor ca...

Страница 36: ...Select the titrator model you wish to use u Tap the specified function on the function bar The titrator model is saved SAVE 5 14 Installing a titrator with RS232 MultiDist T only Precondition R The do...

Страница 37: ...connection marked Dosing Unit u Secure the plug in place 5 16 Installing the reaction detection sensor MultiDist T only u Attach the reaction detection sensor to the instrument u Connect the sensor ca...

Страница 38: ...e rear cable duct u Connect the sensor cable to the related connection on the instrument See Chapter 3 2 Configuration page 14 5 19 Installing the stirrer MultiDist only u Attach the stirrer to the re...

Страница 39: ...ls representing the menus See Chapter 6 3 Menu bar interface page 40 3 Content area Shows current settings submenus or actions de pending on the current operation 4 Function bar Shows functions that c...

Страница 40: ...IT Edit Allows the selected item to be edited READY Ready Steam generator is ready to distill PREP Preparation Carries out the method selected in the Priming submenu See Chap ter 8 2 Editing the primi...

Страница 41: ...pter 10 3 Cleaning the glass components page 83 Stirring See Chapter 8 15 Changing the stirring speed manually page 76 Pump Calibration See Chapter 10 14 Calibrating the pumps page 85 6 3 3 Method men...

Страница 42: ...pensation of the steam power caused by voltage fluctuations AutoDist Mode On Off Conditioning and distillation are per formed automatically Level Detect Max Time Enter value The time after which the d...

Страница 43: ...evice name MAC address DHCP System IP address Subnet mask Gateway DNS server BUCHI Cloud Server IP address Service submenu NOTE Only super user can carry out changes in the Service submenu System Info...

Страница 44: ...k level sensor is connected to the instru ment Dosing unit attached Titration unit attached SD White A SD card is in the instrument Red The SD card in the instrument is in read only mode A USB input d...

Страница 45: ...pro 1 3 6 5 4 2 Fig 17 Interface pro No Description Function 1 Status bar Shows the determination name and status of the instrument See Chapter 7 4 Status bar interface pro page 50 2 Menu bar Shows sy...

Страница 46: ...he display reverts to the previous view OK Confirm Confirms an entry START Start Starts an extraction process COPY Copy Copies the selected method EDIT Edit Allows the selected item to be edited READY...

Страница 47: ...System information Determination data menu View processed determinations 7 3 1 Home menu 1 2 3 5 4 Fig 18 Home menu during a determination 1 Select and shows operation mode 2 Preview of next determin...

Страница 48: ...60 7 3 4 Configuration menu Settings submenu Action Option Explanation Language Choice of display lan guage on the interface The following languages are avail able English German French Italian Spani...

Страница 49: ...Keypress Enter value Dosage volume which is applied by pressing the related button Acid Dosage per Keypress Enter value Dosage volume which is applied by pressing the related button H BO Dosage per K...

Страница 50: ...termination data menu Shows the history of the determination data 7 4 Status bar interface pro The status bar shows actual information about the instrument View Status The instrument is in standby mod...

Страница 51: ...B chi Labortechnik AG Description of the interface pro 7 Operation Manual K 365 Dist Line 51 106 View Status A recirculating chiller is connected...

Страница 52: ...ion on the function bar EDIT u Enter the preheating time in seconds u Tap the specified function on the function bar The time is saved SAVE 8 2 Editing the priming function NOTE The method selected in...

Страница 53: ...thout sample Reference Substance For determinations with a defined reference sub stance Sample For determinations with unknown sample Specifications on the display u Navigate to the specified submenu...

Страница 54: ...er a value for the sample weight u Tap the specified function on the function bar The sample weight is saved SAVE 8 3 5 Changing the unit for a single determination The following units are available U...

Страница 55: ...new series is created NEW Creating a new series from a template Specifications on the display u Navigate to the specified submenu Templates u Select the template from which you want to create a serie...

Страница 56: ...ns on the display u Navigate to the specified submenu Series u Select the series you wish to edit u Select the determination you wish to copy u Tap the specified function on the function bar The deter...

Страница 57: ...n type within a series The following determination types are selectable Determination type Explanation Blank For determinations without sample Reference Substance For determinations with a defined ref...

Страница 58: ...ination within a series Specifications on the display Precondition R The determination type is set to Sample or Reference Substance See Chapter 8 4 6 Selecting the determination type within a series p...

Страница 59: ...determination you wish to edit u Select the specified action Unit u Tap the specified function on the function bar EDIT u Select the determination type you wish to use The determination type is select...

Страница 60: ...lect the name of the template that you wish to edit u Select the specified action Template Name u Tap the specified function on the function bar EDIT u Enter a name for the template u Tap the specifie...

Страница 61: ...u wish to edit u Select the specified action Method Name u Tap the specified function on the function bar EDIT u Enter a name for the method u Tap the specified function on the function bar The name i...

Страница 62: ...in the corresponding Application note Specifications on the display u Navigate to the specified submenu Methods u Select the method that you wish to edit u Select the specified action H O Volume u Tap...

Страница 63: ...r MultiDist only page 61 Enter manually the quantity of NaOH for alkalizing the sample For the correct quantity check related Application note or use the KjelOptimizer App Specifications on the displa...

Страница 64: ...ifications on the display u Navigate to the specified submenu Methods u Select the method that you wish to edit u Select the specified action Reaction Time u Tap the specified function on the function...

Страница 65: ...cified function on the function bar SAVE 8 6 11 Changing the time a steam step is carried out for a method NOTE Calculating the starting time for a steam step R Make sure that the distillation time is...

Страница 66: ...u wish to edit u Select the specified action Steam Power u Tap the specified function on the function bar EDIT u Enter the level for the steam power u Tap the specified function on the function bar Th...

Страница 67: ...u Navigate to the specified submenu Methods u Select the method that you wish to edit u Select the specified action Distillation Time u Tap the specified function on the function bar EDIT u Enter a va...

Страница 68: ...n Titration Type u Tap the specified function on the function bar EDIT u Select the titration type you wish to use u Tap the specified function on the function bar SAVE 8 6 17 Changing the H BO volume...

Страница 69: ...function on the function bar The volume is saved SAVE 8 6 19 Changing the titration stirring speed for a method MultiDist T only NOTE The availability depends on the selected titration type Specificat...

Страница 70: ...e for the sample tube for a method BasicDist MultiDist MultiDist T only Specifications on the display u Navigate to the specified submenu Methods u Select the method that you wish to edit u Select the...

Страница 71: ...ice User is a default user and password protected 8 7 1 Creating a new user Specifications on the display u Navigate to the specified submenu User Administration u Tap the specified function on the fu...

Страница 72: ...on the function bar The new name is saved SAVE 8 7 4 Selecting a user Specifications on the display u Navigate to the specified submenu User Administration u Select the user you wish to use u Tap the...

Страница 73: ...ample tube against the end stop and the sample tube sealing u Secure the sample tube in place with the handle 8 9 Installing a receiving vessel u Insert the sample receiving vessel to the instrument u...

Страница 74: ...ation mode Explanation Single Determination For carrying out one determination Editing settings see Chapter 8 3 Editing the single determination page 52 Series For planning and carrying out a series o...

Страница 75: ...hapter 8 8 Installing the sample tube page 72 u Navigate to the specified menu u Tap the specified button The pump applies a defined quantity of NaOH NaOH 8 13 3 Dosing H BO manually NOTE The quantity...

Страница 76: ...iquid from the receiving vessel Receiver Aspiration 8 15 Changing the stirring speed manually Specifications on the display u Navigate to the specified submenu Stirring u Select the specified action S...

Страница 77: ...8 Operation Manual K 365 Dist Line 77 106 Precondition R The On Off master switch is set to on u Rinse the pump you want to use See Chapter 10 20 Rinsing a pump page 90 u Turn the valve in the correc...

Страница 78: ...g a receiving vessel page 73 u Install the sample tube See Chapter 8 8 Installing the sample tube page 72 u Close the protection shield u Flush the tubing See Chapter 8 13 Dosing manually page 74 u As...

Страница 79: ...ter 8 8 Installing the sample tube page 72 u Install an empty receiving vessel EasyDist and BasicDist only See Chapter 8 9 Installing a receiving vessel page 73 u Set the On Off master switch to off 9...

Страница 80: ...L u Confirm the secure question All determination data are deleted 9 8 Exporting determination data Interface pro only 9 8 1 Exporting one determination Interface pro only Specifications on the displa...

Страница 81: ...only carry out the servicing and cleaning operations described in this section Any servicing and repair work which involves opening up the casing may only be carried out by BUCHI service technicians u...

Страница 82: ...2 years 10 7 Cleaning and servicing the steam inlet and condenser outlet tube 2 Replace the tube once per year 10 8 Cleaning the housing 2 10 9 Cleaning and servicing the warning and directive sym bo...

Страница 83: ...ample tube is installed See Chapter 8 8 Installing the sample tube page 72 R A sample receiving vessel is installed See Chapter 8 9 Installing a receiving vessel page 73 u Navigate to the specified su...

Страница 84: ...epending on the use 10 8 Cleaning the housing u Wipe down the housing with a damp cloth u If heavily soiled use ethanol or a mild detergent u Wipe down the display with a damp cloth 10 9 Cleaning and...

Страница 85: ...t is less than 160 mL water per 5 minutes distillation after preheating decalcify the instrument See Chapter 10 15 Decalcifying the instrument page 87 10 14 Calibrating the pumps 10 14 1 Calibrating t...

Страница 86: ...the value in the numeric dialog u Tap the specified function on the function bar SAVE 10 14 3 Calibrating the NaOH pump Specifications on the display Precondition R A sample tube is installed See Chap...

Страница 87: ...olume in the sample receiving vessel u Enter the measured volume u Tap the specified function on the function bar SAVE 10 15 Decalcifying the instrument Time required approximately 2 5 hours Decalcifi...

Страница 88: ...ps stop working u Set the On Off master switch to Off u Remove the water from the instrument See Chapter 12 4 Removing water from the steam generator page 98 u Do steps 11 thru 16 five times 10 16 Rep...

Страница 89: ...rse sequence u Remove the protection shield See Chapter 10 18 Attaching and removing the protection shield page 89 u Loosen the cap nut at the condenser u Remove the cooling water hoses u Remove the r...

Страница 90: ...a pump Precondition R A sample tube is installed See Chapter 8 8 Installing the sample tube page 72 u Put the side of the hose in distilled water u Apply 100 mL with the manual functions See Chapter 8...

Страница 91: ...B chi Labortechnik AG Cleaning and servicing 10 Operation Manual K 365 Dist Line 91 106 u Open the splash protector nut u Remove the splash protector u Remove the seal...

Страница 92: ...e to optimize the digestion download available on BUCHI website Digestion temperature is too low u Decrease digestion time u Compare to conditions to similar applications Temperature is too high u Dec...

Страница 93: ...volume Amount of water used for dilu tion is too low u Increase dilution volume Measured nitrogen content is too high Air in titration system burette or tubes u Tighten the connections u Flush the tub...

Страница 94: ...200 mg Nitrogen per sample tube u Use KjelOptimizer software to optimize the digestion download available on BUCHI website Not enough NaOH or incorrect concentration of NaOH used required is 32 u Corr...

Страница 95: ...n diges tion time too short u Choose digestion time accordingly u Check color of samples during digestion Solution should be transparent by the end of the digestion Stirrer is defective u Clean the st...

Страница 96: ...le from the instrument to the display u Contact BUCHI Customer Service No cooling water flow The cooling water supply is blocked u Make sure that the hoses are not bend u Check for leaks between instr...

Страница 97: ...B chi Labortechnik AG Help with faults 11 Operation Manual K 365 Dist Line 97 106 11 4 Turning the splash protector nut u Turn the splash protector nut...

Страница 98: ...instrument 12 2 Disposal The operator is responsible for proper disposal of the instrument u When disposing of equipment observe the local regulations and statutory requirements regarding waste dispo...

Страница 99: ...cable Indicates the status of the instrument instrument is ready to use has an error or is in operation 11068959 BUCHI Bluetooth Dongle connects instrument to smartphone via Bluetooth 11067770 Adapter...

Страница 100: ...044989 Dispenser unit Titronic 300 11062956 13 1 2 Splash protector spare parts Order no Image Glass splash protector EasyDist 11071015 Plastic splash protector EasyDist 11072055 Glass splash protecto...

Страница 101: ...t GL14 033577 Hose barbs set 4 pcs straight GL14 FPM seal Content Hose barbs cap nuts seals 040296 Seals set 10 pcs for hose barbs GL14 FPM green 040040 13 1 3 Tank spare parts Order no Image Cap Set...

Страница 102: ...70669 Check valve 11071740 Dist Outlet PTFE L 300 11071940 13 1 5 Titration spare parts Order no Image Receiving vessel 043390 Stirrer cpl 11070246 pH electrode refillable electrolyte 11065834 pH Elec...

Страница 103: ...1057442 Sample tubes 300 mL 20 pcs 11059690 Sample tubes 300 mL For sample volumes up to 200 mL or 5 g in weight 4 pcs 037377 Sample tubes graduated 300 mL 4 pcs 043049 Sample tube 500 mL 026128 Sampl...

Страница 104: ...3618 Cable to Metrohm 7 series Mettler T series titrator 043617 Silicone hose D6 9 L 3 m 048355 13 1 8 Other spare parts Order no Image Cap RJ 45 cap 11055949 USB cover 11069375 Level sensor capacitiv...

Страница 105: ...Upgrade Basic base unit with aspiration pump and I 300 Pro 11072754 Upgrade Multi base unit with titration vessel 11072755 13 1 1 2 Documentation Order no Kjeldahl Knowledge Base EN Comprehensive guid...

Страница 106: ...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 J...

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