Metrohm 1.873.0014 Manual Download Page 3

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Metrohm AG
CH-9101 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com

873 Biodiesel Rancimat

Manual

8.873.8003EN

03.2009 jb/ars

Summary of Contents for 1.873.0014

Page 1: ...873 Biodiesel Rancimat Manual 8 873 8003EN...

Page 2: ......

Page 3: ...Metrohm AG CH 9101 Herisau Switzerland Phone 41 71 353 85 85 Fax 41 71 353 89 01 info metrohm com www metrohm com 873 Biodiesel Rancimat Manual 8 873 8003EN 03 2009 jb ars...

Page 4: ...entation is protected by copyright All rights reserved Although all the information given in this documentation has been checked with great care errors cannot be entirely excluded Should you notice an...

Page 5: ...ernal air supply 10 3 2 2 Mounting accessories for the external air supply 13 3 2 3 Equipping the reaction and measuring vessels 13 3 2 4 Inserting vessels Establishing tubing connections 16 3 2 5 Mou...

Page 6: ...55 4 5 2 Parameter description 60 4 6 Determinations 75 4 6 1 Preparing the instrument and the accessories 76 4 6 2 Preparing the determination 77 4 6 3 Starting the determination 79 4 6 4 Cleaning th...

Page 7: ...lems 159 7 Technical specifications 165 7 1 General data 165 7 2 Temperature regulation and measurement 165 7 3 Conductivity measurement 166 7 4 Gas flow regulation 166 7 5 GLP test set 167 7 6 RS 232...

Page 8: ...re 2 Front 873 Biodiesel Rancimat 7 Figure 3 Rear 873 Biodiesel Rancimat 8 Figure 4 Mounting accessories for the air supply rear of the instrument 11 Figure 5 Equipping the reaction and measuring vess...

Page 9: ...so be determined In the case of con ductivity changes stages which do not have anything to do with the autoxidation the evaluation can be interrupted for definite time intervals The results determined...

Page 10: ...ylic acids as secondary oxidation products With the Rancimat method the sample is exposed to an air flow at a constant temperature between 50 220 C see Figure 1 page 3 Highly volatile secondary oxidat...

Page 11: ...into operation The documentation contains information and warnings which have to be followed by the user in order to ensure safe operation of the instrument 1 3 1 Symbols and conventions The followin...

Page 12: ...ge of instruments or instrument parts Note This symbol marks additional information and tips 1 4 Safety instructions 1 4 1 General notes on safety Warning This instrument may only be operated in accor...

Page 13: ...to the heating block can be dan gerous Check the glass vessels before each use 1 4 2 Electrical safety The electrical safety when working with the instrument is ensured as part of the international st...

Page 14: ...hemicals Warning All relevant safety measures are to be observed when working with flam mable solvents and chemicals Set up the instrument in a well ventilated location e g laboratory flue Keep all so...

Page 15: ...reached 4 Error display red Lights up or flashes when a fault has occurred in the instrument see Troubleshooting Chap ter 5 Instrument number display Indicates the number of the instrument Lights up i...

Page 16: ...ctrode connector For connecting the conductivity measuring cell integrated in the measuring vessel cover 2 7 3 Air supply connection For connecting the FEP tubing 250 mm 2 6 4 Mains switch For turning...

Page 17: ...ng 250 mm 6 1805 080 For supplying the air from the drying flask to the reaction vessel 2 11 15 From Flask connection 16 Air N2 in connection 17 FEP tubing 130 mm 6 1805 010 For connecting the Air out...

Page 18: ...sive environments Place the instrument in a location of the laboratory suitable for operation and free of vibrations if possible protected from corrosive atmospheres and contamination by chemicals The...

Page 19: ...250 mm 6 1805 080 For supplying the air from the drying flask to the reaction vessel 2 11 7 From Flask connection 8 Dust filter 6 2724 010 9 To Flask connection 10 Air out connection 11 FEP tubing 130...

Page 20: ...of the FEP tubing 250 mm 4 6 onto that open ing on the drying flask cover at the bottom of which the filter tube is located Screw the other end of the FEP tubing onto the From flask con nection 4 7 on...

Page 21: ...ection 4 12 on the rear of the Biodiesel Rancimat Screw the tubing adapter M6 olive 6 1808 020 onto the other end of the FEP tubing 2 Connect the gas supply Mount the gas supply from the bomb with syn...

Page 22: ...ead adapter M8 M6 6 1808 090 4 Tubing connector For connecting the Iso Versinic tubing 5 Air tube 6 2418 130 6 O ring 6 1454 040 7 Connection For connecting the thread adapter M8 M6 8 Reaction vessel...

Page 23: ...cover 5 16 on the measuring vessel 5 20 2 Mount the reaction vessel cover Insert the air tube 5 5 from below into the connection 5 7 of the reaction vessel cover Place the O ring 5 6 over the upper e...

Page 24: ...supply connections 3 3 of the Biodiesel Rancimat 3 Insert the reaction vessel Fill the reaction vessel 5 10 with the sample After reaching the required temperature insert the reaction vessel with the...

Page 25: ...e Iso Versinic tubing into the correspond ing opening on the collection tube Seal the unused openings on the collection tube with the enclosed plugs E 400 0010 3 Connect the exhaust collection tube Co...

Page 26: ...s connection socket 3 Replace fuses Carefully take the defective fuses out of the fuse holder and replace them with two new fuses suitable for the set mains voltage of the type TH slow acting with hig...

Page 27: ...with the RS 232 cable 6 2134 100 The PC program 873 Biodiesel Rancimat allows control of max 4 instru ments The following options are available for connecting the instruments to serial PC interfaces...

Page 28: ...og language Select the dialog language of the program Click on the OK button Click on the Next button 3 Accept the license agreement Read through the license agreement and accept it with Yes 4 Define...

Page 29: ...pdate 1 Exit 873 Biodiesel Rancimat if you have started the software after the installation Start the installation file by double clicking and follow the instruc tions of the installation program 3 4...

Page 30: ...s Leave the Old password field empty Enter a new password for the Administrator in the New pass word field Reenter the password in the Confirm new password field and confirm with OK The dialog window...

Page 31: ...3 Installation 873 Biodiesel Rancimat 23 Establishing the device communication 1 Follow the instructions in Section 4 2 1...

Page 32: ...program Proceed as follows to start and exit the program Note If you are starting the program for the first time you first have to set an Administrator password see Chapter 3 4 3 page 21 1 Start progr...

Page 33: ...sults window Reevaluation Reevaluation refers to the subsequent revision of a determination in particular the manual specifi cation of the induction time using tangents Recalculation The recalculation...

Page 34: ...user the instrument status Menus The Control window contains the following main menus File Create new methods open existing methods manage methods open Results window print new login close program Vi...

Page 35: ...atus overview for the instruments connected see Chapter 4 3 2 page 44 Instrument informa tion Instrument information see Chapter 4 3 1 page 42 GLP status Display GLP status see Chapter 4 8 3 page 140...

Page 36: ...ile Results or the symbol When opening the Results window the database Repos mrd is auto matically loaded in which all recorded determinations are saved by default 2 Close Results window In the dialog...

Page 37: ...indows Help Display program specific Online help Symbols The toolbar of the Results window contains the following symbols Print Print results curves and overview lists see Chapter 4 7 6 page 124 Copy...

Page 38: ...verview to Word see Chapter 4 7 6 page 124 Export to Excel Export Determination overview to Excel see Chapter 4 7 6 page 124 Export measured val ues Export measured values to a TXT file see Chapter 4...

Page 39: ...also be selected by click ing with the right mouse button on the required dialog window or element The menu options opened depend on the active dialog window or element selected 4 1 7 Mouse functions...

Page 40: ...hs appears Click on the menu item Zoom Off 4 1 8 Help You can call up help for the current topic anywhere with the symbol the menu item Help Help topics or the key F1 Green text can be clicked on This...

Page 41: ...munication between your PC and the 873 Biodiesel Rancimat as follows 1 Select number of instruments connected In the Control window click on the menu item Options Com munication The following dialog w...

Page 42: ...ll connected instruments 4 2 2 Managing access rights The 873 Biodiesel Rancimat program offers extensive password protec tion allowing each menu item to be provided with individual access rights The...

Page 43: ...sers and groups manager In the Control window click on the menu item Options User permissions 2 Create new group Right click on an existing group to select the menu item Add group Under Enter new grou...

Page 44: ...required options by clicking on the symbol Confirm the changes with OK Adding a new user Proceed as follows to add a new user 1 Open Users and groups manager In the Control window click on the menu it...

Page 45: ...to delete an existing group 1 Open Users and groups manager In the Control window click on the menu item Options User permissions 2 Delete group Right click on the group to be deleted in order to sel...

Page 46: ...e following dialog window appears 2 Set automatic start time Under Start heating select the option Once Under Start at enter the required time and date Confirm the entries with OK Starting heating blo...

Page 47: ...at enter the required time and confirm with OK 4 2 4 Gas flow control The gas flow produced by the internal pump through the reaction vessels to the measuring vessels can be switched on and off manua...

Page 48: ...emperature can be recorded at any time for each individual heating block The program writes the recorded measured values into a text file containing the following values t s Time in seconds Block C Te...

Page 49: ...installation this file is located at C Program Files Metrohm Biodiesel Ranci mat Template As soon as the file is greater than 10 MB you should optimize and compress the program so that this file no lo...

Page 50: ...ow and the program Biodiesel Rancimat see Chapter 4 1 1 page 24 2 Optimize database In the Windows Start menu click on the menu item Pro grams Metrohm Biodiesel Rancimat Opti mize Database 4 3 Program...

Page 51: ...d instrument Program number Number of the EEPROM program of the selected instrument Last maintenance Date of the last maintenance with signature of the service technician who has carried out the servi...

Page 52: ...dialog window In the Control window click on the menu item View Status overview The following dialog window appears 2 Adjust and save column width You can adjust the column width to the required size...

Page 53: ...on error between instrument and PC Stab time Stability time determined Induc time Induction time determined Set temp Setpoint temperature defined in the method Current temp Current block temperature 4...

Page 54: ...status of the log file 3 Save log file Click on the symbol or the menu item File Save as In the dialog window Save file as enter a file name and confirm with OK 4 Open saved log file Click on the sym...

Page 55: ...e certain entries from the event file 1 Open dialog window In the Control window click on the menu item Options Event log The following dialog window appears 2 Delete entries Enter the maximum age in...

Page 56: ...ts of the conductivity measuring cells used in the Biodiesel Rancimat which are normally in the range from 1 00 1 20 only have to be entered exactly if the absolute conductivity measured value is to b...

Page 57: ...h OK Determining cell constants automatically Proceed as follows if you wish to enter the cell constants automatically 1 Open dialog window Click on the menu item Tools Cell constants Automatic The fo...

Page 58: ...d can be used 3 Start determination and check the values Click on Start to start the determination of the cell constant After the determination is finished the dialog window Enter Check cell constants...

Page 59: ...05 080 For supplying air into the reaction vessel 2 Pt100 temperature sensor 3 Thread adapter M8 M6 6 1808 090 4 Opening for temperature sensor For inserting the temperature sensor 5 Air tube 6 O ring...

Page 60: ...the reaction vessel with 5 g silicone oil e g FLUKA 85409 Place the reaction vessel cover with the temperature sensor on the reaction vessel Push the temperature sensor fully downwards the sensor must...

Page 61: ...u item Tools Gas flow control Gas flow on Click on the button Heat to xx C Executing a Delta T determination After you have prepared everything for determining Delta T see Preparing Delta T determinat...

Page 62: ...ured temperature is now stable appears in the message box The following three values are displayed below the message box Block temperature Temperature which has been measured in the heating block with...

Page 63: ...e Please wait appears in the message box 3 Accept measured values Click on the Accept button in order to accept the determined temperature correction Delta T in the method This is followed by the mess...

Page 64: ...b Evaluation and also adjust the parameters Repeat for all remaining tabs Note You can find a detailed description of all tabs and their parameters at 4 5 2 Parameter description 3 Save method Click o...

Page 65: ...page 60 Confirm the changes with Save Opening an existing method and adjusting parameters Proceed as follows to open an existing method and adjust its parameters 1 Open existing method In the Control...

Page 66: ...he required method and then the button Rename The method name is highlighted in blue Enter the new method name and click with the mouse on the free white area below the method name in order to accept...

Page 67: ...n existing method Note A method which is still selected in one of the blocks A or B cannot be deleted Select another method first in order to delete the required method 1 Open Method manager In the Co...

Page 68: ...2 Print parameters Click on the Print button The dialog window Print Setup opens All the printers installed on your PC appear under Name Select the required printer and confirm with OK 4 5 2 Paramete...

Page 69: ...ature This value is determined through measurement of the deviation by the current temperature of the sample from the heating block temperature using a cali brated external temperature sensor see Chap...

Page 70: ...rnal pump on off Default value on Switch on off gas supply with internal pump If the internal pump is switched off an external gas supply must be connected to the Air N2 in connection see Chapter 3 2...

Page 71: ...ew of stop criteria Time Conductivity Endpoint s Analysis stops not automatically after the time entered independently of reach ing the induction stability time endpoint after reaching the conductivit...

Page 72: ...value off Automatic deactivation of the heating at the end of the determination Shut off gas flow on off Default value off Automatic deactivation of the gas flow at the end of the determination Cautio...

Page 73: ...Default value off Determination of the stability time see Stability time page 67 Note If you select this evaluation mode you always need to calibrate the con ductivity measuring cell beforehand Delta...

Page 74: ...cceptance of smaller maximums of the second derivative Higher values require a higher maximum Range 0 1 9999 Induction time The induction time is the time to the break point of the curve conduc tivity...

Page 75: ...ty time The stability time is the time which is necessary in order to attain a specified conductivity change Delta Kappa Stability time Time Delta Kappa Conductivity The entry of an evaluation delay o...

Page 76: ...e end value of the time axis End value End value of the time axis with manual scaling Range 0 5 100 h Conductivity axis y Selection Auto scaling Manual scaling Auto scaling Automatic definition of the...

Page 77: ...ny time in the determination overview see Chapter 4 7 5 page 117 Formula 1 for induction time on off Default value off If this option is switched on the automatically determined induction time will be...

Page 78: ...me for a temperature deviating from the measuring temperature the so called standard time The settings here do not have any effect on the measuring sequence or the evaluation After finishing the measu...

Page 79: ...ed at different temperatures Range 0 001 100 Target temperature Target temperature for the calculation of the standard time Range 20 300 C 4 5 2 6 Documentation tab This tab contains parameters for th...

Page 80: ...Stability time Standard time Formula 1 Formula 2 Formula 3 Automatic report output Send to printer immediately on off Default value on Automatic printout of the report defined under Include in report...

Page 81: ...109 h Induction time 3 23 Method name FAME Creator Administrator Creation date 08 02 2007 08 27 20 Temperature 120 Start delay 0 Stop time 0 00 Stop at conductivity 200 Stop at endpoint Evaluation del...

Page 82: ...4 5 Methods 74 873 Biodiesel Rancimat 4 5 2 7 Description tab You can enter a comment on the method in this tab...

Page 83: ...4 5 2 Start heating Enter sample identifiers Temperature reached no yes Insert and connect reaction vessels Start determination Section 4 6 2 Section 4 6 2 Section 4 6 2 Section 4 6 3 Stop crit reache...

Page 84: ...out of the openings with nitrogen If the instrument is not used always seal the openings with the sealing plugs 2 Fill the measuring vessels Note Only use measuring vessels and accessories which are...

Page 85: ...t film so that the vessel covers can be removed more easily after the determination Insert an air tube 5 5 in the connector 5 7 of the reaction vessel cover fix it with the O ring 5 6 and fasten it by...

Page 86: ...e color of the button frame changes to red and the temperature display 2 3 on the instrument flashes The current temperature is dis played directly next to the button Heating up duration for 120 C app...

Page 87: ...easuring vessel covers Screw the FEP tubings 250 mm 5 1 to the thread adapters 5 3 of the reaction vessel covers and the air supply connections 3 3 of the Biodiesel Rancimat 4 6 3 Starting the determi...

Page 88: ...with acetone or 2 propanol and rinse with distilled water Pre clean with washing up liquid in the case of severe contamination Remove the protective ring 5 19 to be able to clean the electrodes 2 Clea...

Page 89: ...parameters The following dialog window appears 2 Adjust the parameters Adjust all required parameters see Chapter 4 5 2 1 page 60 Confirm the changes with OK 4 6 6 Stopping the determination manually...

Page 90: ...Before a determination No active measurement The channel is ready for starting a determination No active measurement Communication error between instrument and PC During a determination Determination...

Page 91: ...he described methods via the context menu Further below in this section you will find a detailed description of all param eters of the dialog windows of the determination overview see Parameter descri...

Page 92: ...e right column under Display In the column Selection click on a field which is to be displayed in the determination overview Click on the button In the column Display click on a field which is not to...

Page 93: ...tween two col umns The cursor assumes the following form Drag the column width to the required size keeping the left mouse button pressed down 3 Adjust the cell format Click on the menu item Format Fi...

Page 94: ...the determination overview 1 Select a line Place the mouse button on the left edge of the line to be selected The cursor assumes the following form Click on the line 2 Select several lines Place the...

Page 95: ...ck on the button Find first in order to search through the determination overview Sorting determinations Proceed as follows to sort the columns of the determination overview 1 Sort column ascending Cl...

Page 96: ...ations Click on the symbol or the menu item Determination Fil ter Selection not in filter Filtering determinations with the Selection based filter Proceed as follows to filter the entries of the deter...

Page 97: ...on the symbol or the menu item Determination Fil ter Special filter sorting The following dialog window appears 2 Select the fields which are to be filtered In the dialog window Anzeige bersicht doub...

Page 98: ...ayed that was carried out on April 5 2000 at a temperature of over 110 C In addition the dialog window Determination data uses the word FILTER to indicate that the displayed data is filtered Click on...

Page 99: ...ile Directory in which the determination file TXT file has been saved Evaluation sensitivity Evaluation sensitivity used for the determation of the induction time User Name of the user who was logged...

Page 100: ...e automatic Automatically determined induction time Induction time manual Induction time manually determined with the reevaluation Channel Number of the channel used for the determination Method name...

Page 101: ...in Selection to Display Move selected field in Selection to Display The field is inserted at the end of the list Move selected field in Selection to Display The field is inserted above the field sele...

Page 102: ...Display horizontal grid lines Vertical on off Default value on Display vertical grid lines Cell Effect Selection Flat Raised Sunken Flat Flat view of the cells Raised Raised view of the cells Sunken...

Page 103: ...the fonts installed on the PC Selection Font type Effects Underline on off Default value off Choice of underlining for characters Color Color for the selected font type Selection Color Font style Cho...

Page 104: ...All Down Up All Search in the entire table Down Search downwards as far as the table end Up Search upwards as far as the table start Match Search area where the entered text is to be searched for Sel...

Page 105: ...for this option must be deactivated Search Only Current Field on off Default value off If this option is activated the search is restricted to the selected field The field name is displayed in the wi...

Page 106: ...d names Mathematical oper ators Comparison opera tors Between And Logical operators AND OR NOT Wildcards any character string single character sin gle numeral Current date Date Current time Now date a...

Page 107: ...n and method data Proceed as follows to display all determination and method data for a selec ted determination 1 Display determination overview See Displaying the determination overview page 83 2 Ope...

Page 108: ...onstant of the conductivity measuring cell used to record the deter mination GLP test GLP status at the time of recording the determination The following displays are possible GLP test switched off Th...

Page 109: ...ically or with the reevaluation manually determined stability time Delta Kappa Conductivity change for the determination of the stability time Formula 1 for induction time Result of the calculation wi...

Page 110: ...at Method name Name of the method Creation date Date when the method was last saved Creator Name of the logged in user who last saved the method Method description Description of the method Temperatur...

Page 111: ...individually per 2 channels 2 channels each have been started jointly per block the 4 channels of a block were started jointly Stop criteria Time Time until the automatic stop of the determination Con...

Page 112: ...ppa Conductivity change for the determination of the stability time Options for induction time Evaluation delay Waiting time until starting the curve evaluation Evaluation suppression Start Time from...

Page 113: ...rmula 2 for stability time The automatically determined stability time was calculated with these values and saved under the name shown in the field R2 Formula 3 for stability time The automatically de...

Page 114: ...axis x Autoscaling Automatic definition of the start and end value of the time axis Manual scaling Manual definition of the end value of the time axis End value End value of the time axis with manual...

Page 115: ...t of the results selected below Method parameters Output of the method parameters Results Output of the selected results Induction time Stability time Standard time Formula 1 3 Automatic report output...

Page 116: ...stopped manually with Stop Stop after communication error Automatic stop of the determination because of interrupted connection between the Biodiesel Rancimat and the PC Value Value for warning e g te...

Page 117: ...green A maximum of 16 single graph windows can be opened Note In contrast to the windows Multiple graph and Live graph the win dow with the single graph is not automatically updated upon selecting ano...

Page 118: ...n the dialog window of a multiple graph The context sensitive menu for graphs appears Click on the menu item Offset The offset for the displayed measurement curve is switched on or switched off In the...

Page 119: ...ly and manually set the induction time 1 Open dialog window Right click in the dialog window of a live graph and click on the entry Reevaluation in the context sensitive menu The dialog window Reevalu...

Page 120: ...ime is displayed both in the dialog window Live graph at the top right beside the gray line and also in the dialog window Reevaluation under Stability time 3 Save changes In the dialog window Live gra...

Page 121: ...d also in the dialog window Reevaluation under Manual 5 Save changes In the dialog window Live graph click on the button Save The new induction time is accepted in the determination overview Deleting...

Page 122: ...with the extrapolation values which the program has calculated from the selected results determinations appears 2 Select result and target temperature Click on the Settings button The following dialo...

Page 123: ...s are used Setting the correlation limit Note The correlation limit for the correlation coefficient r2 can only be set by an Administrator 1 Open dialog window In the Results window click on the menu...

Page 124: ...ated straight line T ln t B ln A B The measured values of the selected determination are shown in black the regression line in green and the time calculated for the target temperature in red Results F...

Page 125: ...a factor see Calculation of standard time page 105 Settings Open the dialog window Program settings The extrapolation parameters are to be entered in the tab Extrapolation see Extrapolation tab page 1...

Page 126: ...to the correct result for most appli cations Smaller values will cause the acceptance of smaller maxi mums of the second derivative Higher values require a higher maximum Confirm the entries with OK N...

Page 127: ...ecalculate formula 1 for induction time and Calculation active or Activate the options Recalculate formula 2 for stability time and Calculation active or Activate the options Recalculate formula 3 for...

Page 128: ...parameters can be found at Recalcu late standard time page 123 Parameter description Recalculate induction time on off Default value off Activate Deactivate recalculation of the induction time If the...

Page 129: ...ct result for most applications Smaller values will cause the acceptance of smaller maximums of the second derivative Higher values require a higher maximum The software suggests a value with which th...

Page 130: ...sult is deleted Recalculate formula 2 for stability time on off Default value off Activate Deactivate the recalculation of the result calculated with formula 2 If the recalculation is deactivated the...

Page 131: ...rd time from the induc tion time If the recalculation is deactivated the original result is kept Calculation active on off Default value off If this option is activated the parameters for the calculat...

Page 132: ...the column width see Formatting the determi nation overview page 83 Select the required determinations and click on Print The results are printed according to the settings which have been defined in t...

Page 133: ...a Proceed as follows to print the determination and method data of one or several determinations 1 Display determination overview See Displaying the determination overview page 83 2 Select determinati...

Page 134: ...s to print the report of one or several determinations which has been defined in the method see Chapter 4 5 2 6 page 71 1 Display determination overview See Displaying the determination overview page...

Page 135: ...mination according to settings 4 Carry out settings Click on the Settings button The dialog window Program settings appears Carry out the required settings see tab Report settings page 132 and confirm...

Page 136: ...is exported 2 Select export program Click on the symbol or the menu item Determina tion Export Export to MS Word The data is copied to a RTF file to be opened automatically by Microsoft Word or Click...

Page 137: ...created database Proceed as follows 1 Display determination overview See Displaying the determination overview page 83 2 Select determination Select the determination to be exported see Selecting dete...

Page 138: ...lick on the symbol or the menu item File Results The Results window appears 2 Read out database password In the Results window click on the menu item Options Administrator Database password The dialog...

Page 139: ...enter the file name and confirm with Save The measured values list will be exported 4 7 7 Program settings Carrying out settings for the representation and output of results You can carry out setting...

Page 140: ...ument infor mation determination date user cell constant and serial number Results on off Default value on Output of the results selected in the Results tab see page 134 Curve on off Default value on...

Page 141: ...e output of company logo and company text in the header Company logo Open the window Find company logo for selecting the graphics file with the company logo Only WMF or BMP files can be used After cli...

Page 142: ...Induction time on off Default value on Stability time on off Default value off Formula 1 for induction time on off Default value off Formula 2 for stability time on off Default value off Formula 3 fo...

Page 143: ...f the start and end values of the curve axes Manual scaling Manual definition of the start and end values of the curve axes X Start Start value of the time axis in hours X End End value of the time ax...

Page 144: ...calculated with formula 1 is used for extrapolation Formula 2 for stability time The result calculated with formula 2 is used for extrapolation Formula 3 for stability time The result calculated with...

Page 145: ...sults window you can arrange the opened dialog windows either above one another beside one another or overlapping Proceed as follows 1 Open windows Open all required dialog windows The following dialo...

Page 146: ...age 180 Further information on the subject of QA GLP and validation can also be found in the brochure Quality Management with Metrohm available from your Metrohm representative Electronic and mechanic...

Page 147: ...iption page 139 and confirm with OK 3 Switch off monitoring Open the dialog window GLP properties for unit with serial no x see step 1 In the required tab Temperature Conductivity Gas flow deactivate...

Page 148: ...s follows to display the status of the GLP monitoring 1 Open dialog window If several instruments are connected In the Control window use the menu item View Unit x to select the required instrument Cl...

Page 149: ...3 Biodiesel Rancimat 2 1 5 4 3 Figure 7 Accessories for GLP test Temperature 1 Pt100 temperature sensor 2 PTFE cylinder 3 Hexagon screw 4 Hexagon key 6 2621 120 5 Aluminum cylinder Preparing the GLP t...

Page 150: ...filled after the normal heating up time of the heating block and the GLP test set If the GLP test set on the other hand is used in an already heated heating block it is necessary to wait at least 30 m...

Page 151: ...a Sensor name for the temperature sensor Under Point 1 3 enter the Temperature and the Resistance of the calibration point Confirm the entry with Next The following dialog window appears 3 Enter test...

Page 152: ...he temperature sensor to the Pt100 connector on the rear of the 873 Biodiesel Rancimat In the dialog window GLP test for unit with serial no x click on Next The test measurement is started As soon as...

Page 153: ...t in the next selected channel rapidly carry out the change Carry out measurement for each of the selected channels After the last measurement is completed the dialog window with the test results appe...

Page 154: ...3 2 of the 873 Biodiesel Rancimat Carrying out the GLP test for the conductivity measurement Proceed as follows to carry out the GLP test Note Before carrying out the GLP test with standard solution f...

Page 155: ...Resistance enter the value of the test resistor in Ohms 10000 for 6 2109 030 and confirm with Next Connect the test resistor to the electrode connector 3 2 indicated in the dialog window and confirm w...

Page 156: ...l L can be used as a standard solution This is derived from the optionally available conductivity standard 6 2301 060 KCl 0 1 mol L through dilution with distilled water The conductivity of this dilut...

Page 157: ...Finish or Reject the results with Cancel 4 8 4 3 Gas flow For the GLP test for gas flow measurement you require a gas flow measuring device not available from Metrohm which can be used to measure the...

Page 158: ...window appears Enter the Gas flow and confirm with Next The following dialog window appears 2 Test all channels Measure the gas flow sequentially for all channels and enter the values in the correspo...

Page 159: ...firm the results with Finish or Reject the results with Cancel 4 8 5 GLP results Printing the GLP certificate Note To be able to print a test certificate you have to switch on the GLP mon itoring see...

Page 160: ...os mrd must be open If another database is open only those GLP tests are displayed which have also been exported into this database during export of the determinations Proceed as follows to display th...

Page 161: ...see Activating Deactivating GLP monitoring page 138 Proceed as follows to print the GLP results 1 Open dialog window with overview Open the Results window see Opening and closing the Results window p...

Page 162: ...icate of the selected overview window The printout contains the Serial number of the instrument the Date the Tester and the Test result Certificate of date Printout of the GLP certificate for the ente...

Page 163: ...ted the inside of the instrument so as to avoid serious damage to the instrument electronics In such cases the Metrohm Service must be informed 5 1 2 Maintenance by Metrohm Service Maintenance of the...

Page 164: ...hot molecular sieve directly into the drying flask after regeneration as otherwise the plastic filter on the filter tube will melt Wait until the molecular sieve has cooled down before filling 5 4 Se...

Page 165: ...brochure Quality Management with Metrohm available from your local Metrohm agent Validation Please contact your local Metrohm agent for support in validating instru ments and software Here you can al...

Page 166: ...on with Metrohm 158 873 Biodiesel Rancimat Note You can find information on the subjects of quality management valida tion and maintenance as well as an overview of the documents currently available a...

Page 167: ...ing flask cover 3 10 correctly on the drying flask and screw tight No air flow can be detected in the reaction vessel it does not bub ble although the pump is running The air supply is blocked Remove...

Page 168: ...t stop If the reaction vessel cover is loose on the reaction vessel despite correct assembly the cover has to be replaced The connection is wrongly con nected Ensure that the PTFE tube 5 17 is mounted...

Page 169: ...ough leaks when transferring from the reaction vessel to the measuring vessel The temperature in different channels of a heating block differs as there are burn marks at one or more places in the open...

Page 170: ...value of Delta Kappa defined in the method is correct see Chapter 4 5 2 2 page 64 See also The stability times are not reproducible for multiple determinations See also The induction time is longer s...

Page 171: ...nductivity e g 200 S cm see Chapter 4 5 2 1 page 60 The curves can then also be evaluated manually after finishing the determination The curve shows a step at the start of the meas urement which has n...

Page 172: ...running until the endpoint is automatically found A time or conductivity is defined as a stop criterion in the method which was reached before the endpoint Deactivate time or conductivity as a stop c...

Page 173: ...perature cor rection Delta T 0 9 9 C can be entered manually or determined automatically using the external temperature sensor Temperature measuring range 0 250 C Resolution 0 1 C Max deviation of the...

Page 174: ...3 Conductivity measurement Sensor Conductivity measuring cell integrated in the measuring vessel cover 6 0913 130 Structure Conductivity measuring cell with 2 steel electrodes Measuring princi ple AC...

Page 175: ...0 03 C Max deviation of the measured temperature from the true value 50 220 C 0 3 C Test resistor 10 k 7 6 RS 232 interface Plug Sub D plug 9 pin male Basic settings 9600 Baud 8 Bit 1 stop bit no pari...

Page 176: ...fol lowed by the user in order to ensure safe operation of the instrument 7 9 Electromagnetic compatibility EMC Emission Standards fulfilled EN IEC 61326 1 EN IEC 61000 6 3 EN 55011 CISPR 11 EN IEC 61...

Page 177: ...Cover material Polyurethane hard foam PUR with flame retardation for fire class UL94VO CFC free Base material Steel painted Width 405 mm Height 268 mm without accessories 353 mm with accessories Depth...

Page 178: ...61326 1 2006 EN IEC 61000 6 3 2004 EN 55011 CISPR 11 2007 EN IEC 61000 3 2 2006 EN IEC 61000 3 3 2005 Immunity EN IEC 61326 1 2006 EN IEC 61000 6 1 2007 EN IEC 61000 4 2 2001 EN IEC 61000 4 3 2006 EN...

Page 179: ...and instruments is also duly docu mented and the documents and source codes are archived Both remain the possession of Metrohm A non disclosure agreement may be asked to be provided by those requiring...

Page 180: ...ranty guarantee Metrohm guarantees that the deliveries and services it provides are free from material design or manufacturing errors The warranty period is 36 months from the day of delivery for day...

Page 181: ...Rancimat 8 6 0913 130 Measuring vessel cover for stability measur ing instruments With built in conductometric measuring cell Shaft material PP Measuring range 0 400 Measuring unit S cm 1 Cell constan...

Page 182: ...mat In combination with 6 2418 130 Set of 100 pieces Material Clear glass Outer diameter mm 24 Length mm 250 8 6 1451 010 Foam barrier Foam barrier in reaction vessels for stability measurements Mater...

Page 183: ...GL 45 Material Clear glass Height mm 100 Outer diameter mm 56 Volume mL 100 1 6 1805 010 FEP tubing M6 13 cm With light and kink protection Material FEP Inner diameter mm 2 Length mm 130 10 6 1805 08...

Page 184: ...ments Material PCTFE Length mm 30 16 6 1808 050 Tubing adapter olive M8 outer 1 M8 outer thread and 1 tubing olive E g for thermostat jacket of exchange units and stability measuring instruments Mater...

Page 185: ...050 drying bottle For Rancimats and Karl Fischer ovens Length mm 112 24 6 1839 000 Iso Versinic tubing 0 22 m Connection tubing for stability measuring instruments for determining the oxidation stabil...

Page 186: ...ssel cover for stability measuring instruments Labeling A1 A2 A3 A4 B1 B2 B3 B4 5 sets of 8 items Material PE Material 2 PP Width mm 25 Height mm 15 1 6 2418 130 Air tube long for biodiesel measuremen...

Page 187: ...EEE Height mm 14 7 Height description Without connections Outer diameter mm 28 6 1 6 2811 000 Molecular sieve Molecular sieve Bottle containing 250 g Pore size 0 3 nm Without moisture indicator For Ra...

Page 188: ...0 temperature sensor for 6 5616 010 GLP test set for stability measuring instruments Shaft material Stainless steel AISI 304 Measuring range 200 300 Measuring unit C Shaft diameter top mm 2 Shaft diam...

Page 189: ...nductivity standard 100 S cm 250 mL Conductivity standard for calibration of conductivity measuring cells with cell con stant 0 1 cm 6 2757 000 Air collection tube for stability instruments Including...

Page 190: ...adjustment and validation of temperature on 873 Bio diesel Rancimat Consists of 6 1111 020 Pt100 temperature sensor long 6 1253 000 Measuring insert for temperature sensor 6 2042 040 Clamp for tempera...

Page 191: ...lay 83 Export 128 Format 83 Print 124 Device information 42 Diagnosis 42 Drying flask Mount 12 Dust filter Mount 11 Replace 155 E Electrostatic charge 6 Evaluation 64 Event overview 45 Export Determin...

Page 192: ...rument information 43 Print method information 71 Results 25 Results window 27 Close 28 Menus 29 Open 28 Structure 28 Symbols 29 Rights Activate Deactivate 36 S Safety instructions 4 Sample identifica...

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Metrohm 1.873.0014, Manual

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