OPERATOR`S MANUAL - Agilent Technologies
Contents
1. Document 6 27121 v1 05 9 PL BV 400 RT Viscometer Operator s Manual Chapter 3 The Graphical User Interface 3 2 Summary View The summary view displays all the components of your PL GPC 50 Plus instrument as a Tree providing you with status for each of the modules and a quick way of access to the various components parameters and options available within the PL Instrument Control software For the PL BV 400 RT Viscometer the status information within the Summary View reports the differential and inlet pressure outputs DP and IP amp PL GPC Instrument Instrument Settings Samples Automation Tools Help O F Detectors gt viscometer DP Output Pa 1 00 IP Output kPa 36 90 Clicking on the component names displayed in red in the Summary View of the screen changes the control display shown in the Component View A green LED next to the viscometer component indicates the detector is being controlled and running whereas a red LED would indicate the detector is either not running or not controlled For further information on the Summary View please see the on line help within the PL Instrument Control software Document 6 27121 v1 05 10 PL BV 400 RT Viscometer Operator s Manual Chapter 3 The Graphical User Interface 3 3 Component View The component view displays the component view of the selected component providing you access to parameters and or direct commands for that specific component In gen2. OPERATOR S MANUAL FOR PL BV 400 RT VISCOMETER NOTICE This document contains references to Varian Please note that Varian Inc is now part of Agilent Technologies For more information go to www agilent com chem Document 6 27121 Revision 1 05 ob June 2010 if Agilent Technologies Varian Inc offices Varian Inc has offices in most countries The major offices for chromatography products are listed below Varian Inc Manufacturing site Essex Road Church Stretton Shropshire SY6 6AX UK International telephone 44 1694 723581 International fax 44 1694 722171 Varian Inc Scientific Instruments 2700 Mitchell Dr Walnut Creek CA 94598 Telephone 1 800 926 3000 International telephone 1 925 939 2400 International fax 1 925 945 2360 Varian B V Postbus 8005 4330 EA Middelburg The Netherlands International telephone 31 118 67 1000 International fax 31 118 62 3193 Varian Australia Pty Ltd 679 Springvale Rd Mulgrave Victoria 3170 Australia International telephone 61 3 9560 7133 International fax 61 3 9560 7950 Varian Industria e Comercio Ltda Avenida Dr Cardoso de Mello 1644 Sao Paulo 04548 005 Brazil International telephone 55 11 3238 0400 International fax 55 11 3238 0410 www varianinc com Varian Inc is the owner of copyright on this document and any associated software Under law the written permission of Varian Inc must be obtained before eith
3. 1 1 Introduction The PL BV 400 RT viscometer is based on the proven four capillary design and is intended for online measurement of viscosity when integrated into the PL GPC 50 Plus instrument The combination of refractive index RI and viscosity detection provides accurate molecular weight determination for all polymer types based on the universal principle as well as valuable branching information not otherwise accessible from a concentration detector alone Due to the four capillary technology the differential pressure DP signal is very stable to flow rate fluctuations A continuous monitor of the pressure through the bridge network also provides a consistent reference of the system flow the inlet pressure IP The instrument can be used in both a batch mode which yields an average intrinsic viscosity and in true gel permeation chromatography GPC mode which yields a slice by slice intrinsic viscosity distribution From the intrinsic viscosity and known retention volumes or known Mark Houwink Sakurada coefficients the molecular weight as well as distribution of a polymer may be determined The PL BV 400 RT Viscometer consists of three components 1 Precision engineered 4 capillary bridge 2 High sensitivity pressure transducers 3 State of the art low noise electronics The viscometer is located in the detector compartment section of the PL GPC 50 Plus with the inlet and outlet of the detector accessed within the column oven co
4. Control software and ensure the initialization is completed successfully Otherwise turn the PL GPC 50 Plus off and then on again ensure the control software has been closed before turning the instrument off If unsuccessful and no obvious cause for the error then contact Varian or your local agent Document 6 27121 v1 05 14 PL BV 400 RT Viscometer Operator s Manual Chapter 4 Troubleshooting 4 2 General Troubleshooting Guide DP IP Baseline Drift Allow sufficient time for system to equilibrate Ensure the instrument is located in a thermally stable environment Degas solvent Purge DP IP transducers Ensure laboratory temperature not changing dramatically DP IP Baseline Noise Purge DP IP transducers thoroughly to remove any air bubbles Purge pump head to remove any air bubbles Degas solvent Low Sensitivity Purge DP IP transducers Check flow split Long Retention Times Check pump flow rate Check for leak on system Document 6 27121 v1 05 PL BV 400 RT Viscometer Operator s Manual 15 Appendix 1 Cleaning amp Decontamination Procedures Appendix 1 Cleaning amp Decontamination Procedures CLEANING AND DECONTAMINATION PROCEDURES ARE ONLY TO BE CARRIED OUT BY TRAINED SERVICE PERSONNEL WARNING Cleaning The exterior of the instrument should be cleaned by wiping down with a soft cloth moistened with dilute detergent solution followed by wiping down with a cloth moistened with
5. The ATTENTION sign denotes relevant information Read this information first before proceeding it will be helpful or necessary to complete the task NOTE The NOTE sign denotes additional information It provides the user with advice and suggestions to facilitate the operation of the instrument NOTE General Precautions Safety Practices The following general safety precautions must be observed during all phases of operation service and repair of this detector Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the detector Varian assumes no liability for the customer s failure to comply with these requirements Perform periodic leak checks on liquid supply lines and connections Do not allow flammable and or toxic solvents to accumulate Follow recommended procedures and protocols for evacuation and disposal of flammable and or toxic solvents Never dispose of such products through municipal waste systems WARNING Cleaning The individual or group responsible for the use and maintenance of this equipment must carry out appropriate decontamination if hazardous material is spilt on or inside the instrument Before using any cleaning or decontamination method except those recommended by Varian users should check with Varian that the proposed method would not damage the equipment See Appendix for detailed
6. deionised water Do not attempt to clean any of the connectors on the rear panel water may gain ingress and accessible pins may become bent Ensure that no moisture enters the instrument Allow instrument to dry off completely before reinstalling into the PL GPC 50 Plus and reconnecting power Decontamination The operator should wear appropriate personal protective equipment for this operation gloves safety glasses lab coat and respirator if level of hazard has been risk assessed to be sufficiently high Disconnect the instrument completely and remove it to a fume cupboard if necessary Open the cover of the instrument to see if any solvent has contaminated the interior Excess quantities of liquid spilt on or inside the instrument should be mopped up using absorbent cloths followed by repeated wiping down with soft cloths moistened with Acetone or deionized water as appropriate to the spilt solvent until the last traces of the hazardous liquid have been removed Identify and if possible correct the source of the leak Inspect cabling parts and surfaces to determine whether any damage has occurred If in doubt contact your local Varian Service Dept for assistance Allow the interior and exterior of the instrument to dry out completely before replacing the cover and reinstalling the PL BV 400 RT into the PL GPC 50 Plus Dispose of contaminated waste appropriately Document 6 27121 v1 05 16 PL BV 400 RT Viscometer Operator
7. 0 RT Viscometer The differential pressure transducer monitors the pressure drop across the bridge AP and the inlet pressure transducer measures the pressure drop through the bridge P When the sample is introduced across capillary 4 C4 of the bridge an imbalance is caused due to the holdup columns This change in pressure AP is proportional to the specific viscosity 7755 according to the following equation 4AP Vl ee ae P P 2AP Where AP is the differential pressure across the bridge and P is the pressure of the flow through the capillarv bridge The instrument makes a true differential measurement directly making it very sensitive to dilute solution viscositv measurements The intrinsic viscosity 7 is ideally obtained by measuring the specific viscosity values at several finite concentrations and extrapolate to zero concentration 71 lim 7 c Document 6 27121 v1 05 7 PL BV 400 RT Viscometer Operator s Manual Chapter 2 Overview of Viscometry Theory However the concentrations used in GPC are low enough for the equation to be valid over a typical chromatogram and thus an extrapolation to the true intrinsic viscosity is not required since the concentration is close enough to the limiting concentration All of the data acquisition and data processing are accomplished using Cirrus Multi software which enables calculation of molecular weight and intrinsic viscosity distributions using algorithms for
8. USTOMARY OR OTHERWISE WHICH BUT FOR SUCH EXCLUSION WOULD OR MIGHT SUBSIST IN FAVOUR OF THE BUYER EXCEPT THAT SUCH EXCLUSION WILL NOT APPLY TO ANY IMPLIED CONDITION THAT THE SELLER HAS OR WILL HAVE THE RIGHT TO SELL THE GOODS WHEN THE PROPERTY IS TO PASS OR WHEN THE BUYER DEALS AS A CONSUMER AS DEFINED IN SECTION 12 OF THE UNFAIR CONTRACT TERMS ACT 1977 ANY IMPLIED TERM RELATING TO THE CONFORMITY OF THE GOODS WITH THEIR DESCRIPTION OR SAMPLE OR AS TO THEIR QUALITY OR FITNESS FOR A PARTICULAR PURPOSE IN NO CIRCUMSTANCES WILL THE SELLER OR ITS EMPLOYEES AGENTS OR SUB CONTRACTORS BE LIABLE FOR ANY LOSS OR DAMAGE OF ANY KIND WHATSOEVER WHETHER CONSEQUENTIAL OR OTHERWISE CAUSED DIRECTLY OR INDIRECTLY BY ANY NEGLIGENCE OR OTHER TORTIOUS ACT OR BREACH OF STATUTORY DUTY ON THE PART OF THE SELLER OR ON THE PART OF ANY OF ITS EMPLOYEES AGENTS OR SUB CONTRACTORS IN CONNECTION WITH OR ARISING OUT OF THE MANUFACTURE OR SUPPLY OF THE GOODS OR IN CONNECTION WITH ANY STATEMENT GIVEN OR MADE OR ADVICE NOT GIVEN OR MADE BY OR ON BEHALF OF THE SELLER Any statement made about the Seller s goods by the Seller or its servants or agents whether orally or in writing is intended for guidance only and the Buyer should not place any reliance thereon without specific enquiry and without ensuring that any matter of concern to him is specifically mentioned in the contract The Buyer is solely responsible for the suitability of the site for the installation of the goods for obtai
9. Universal Calibration Branching information can also be obtained from Cirrus Multi Document 6 27121 v1 05 8 PL BV 400 RT Viscometer Operator s Manual Chapter 3 The Graphical User Interface 3 The Graphical User Interface A Windows based Graphical User Interface GUI providing total instrument control is used to operate the PL BV 400 RT Viscometer as well as the other components of the PL GPC 50 Plus and the PL AS RT amp MT autosamplers This intuitive interface provides simplistic control as well as a comprehensive monitoring system The instrument status can be rapidly assessed for each of the instruments modules For further information on the PL Instrument Control software please see the on line help within the NOTE program To start the control software select the PL Instrument Control item in the PL Instrument Control program group of the Programs option in the Start menu 3 1 Overview if PL GPC Instrumen t Instrument Settings Samples Automation Tools Help 8 Sample Handling l kit si O asomo Current Vial Position Temperature C 4 03 00 00 hh mm ss ofa Injection Valve Current Position Inject 2 Pump Flow Rate ml min 1 00 1 00 Pressure MPa 5 00 e Oven Temperature C TO 40 00 BW n Output mW Component View Summary View The Control screen is effectively divided into two main Views these are 1 The Summary View 2 The Component View
10. detector bottom connection for the PL RI detector and top connection for the Knauer RI detector obtain a 50 50 flow split between the RI and viscometer See below for flow split ratio NOTE calculations The length of tube to the RI inlet will vary so as to 3 Connect the two supplied 10 cm 0 040 in ID PTFE tubes from the outlets of the viscometer and RI to the other Valco T piece 4 Connect the PTFE tube labelled with the blue band the waste tube to the same Valco T piece Viscometer RI Viscometer RI Figure 1 3 3 1 Schematics of the Inlet and Outlet Connections for the PL BV 400 RT Viscometer and the PL RI Detector in Parallel Flow Split Ratio Calculations The flow split ratio is the ratio between the recorded inlet pressures IP from the viscometer with and without the RI detector connected in the system IPri Visc Flow Split Ratio 100 P visc Only Therefore if the flow split ratio were 60 then 60 of the flow would be going through the viscometer i e if running the system at 1 0 mL min then the flow through the viscometer would be 0 6 mL min To record the IP for the viscometer only disconnect the stainless steel tube connecting the RI inlet to the Valco T piece and connect a column end plug to the T piece Autozero the IP output at zero flow and then set the same flow rate as used Document 6 27121 v1 05 3 PL BV 400 RT Viscometer Operator s Manual Chapter 1 General Information when b
11. elp Window will be a short description about the action or parameter the Factory Default Value and the Minimum and Maximum Values for the purge time Action List This is a drop down list of the actions that are available for the viscometer To run an action select the required one from the Action List and press the Submit Action button m Action Button s The actions available for the viscometer are displayed as Action Buttons as well as being found in the Action List To run an action press the required Action button Press the Stop button D to stop all the procedures currently running on the viscometer For further information on the viscometer component view please see the on line help within the PL Instrument Control software For information on the Toolbar menus please see the on line help within the PL Instrument Control software Document 6 27121 v1 05 12 PL BV 400 RT Viscometer Operator s Manual Chapter 4 Troubleshooting 4 Troubleshooting 4 1 Errors Any error s that occur with communications or operations running component actions updating parameters etc with the viscometer the Diagnostic Output Window will automatically open with the error s displayed in the Component Error Status Tab of the Diagnostic Output Window as shown below Each error is uniquely identified with a number that can be referenced back to the control code g PL GPC Instrument Diagnostic Window Display Help A Se
12. en polymer and solvent system at a specified temperature n can be related to molecular weight M through the Mark Houwink Sakurada equation n KM Where K and a are coefficients specific to the polymer solvent system and temperature These can be determined by calibrating with polymer standards of known molecular weights A plot of Log n versus Log M a Mark Houwink Sakurada plot will be a straight line as long as the Universal Calibration is obeyed roa 4 K Log Log M Document 6 27121 v1 05 5 PL BV 400 RT Viscometer Operator s Manual Chapter 2 Overview of Viscometry Theory Values of a reflect the size of the molecule in solution and for a random coil polymer range between 0 5 for a polymer dissolved in a theta solvent to about 0 8 in a very good solvent 2 2 Universal Calibration Benoit 1967 showed that polymers of different structure fall on the same calibration curve if the intrinsic viscosity is included as a calibration parameter A calibration plot of the product of intrinsic viscosity and molecular weight 7 M versus elution volume is a Universal Calibration as shown below in Figure 2 2 1 This allows the system to be calibrated with polymer standards of one type and then analyze polymers of another type and still obtain accurate molecular weight distributions s PS o PS Comb 108 PS Star A Hetero Graft Copol x Poly methy methacrylate log n M 5 e Poly vinyl chloride V G
13. er the documentation or the software is copied reproduced translated or converted to electronic or other machine readable form in whole or in part First published June 2010 in Church Stretton UK Comments about this manual should be directed to the MarCom Manager Europe at the factory address above or by e mail to eumktg varianinc com 2010 Varian Inc Varian and the Varian Logo are trademarks or registered trademarks of Varian Inc in the U S and other countries All product and company names herein may be the trademarks of their respective owners All rights reserved CE DECLARATION OF CONFORMITY We Varian Inc Essex Road Church Stretton Shropshire SY6 6AX UK declare that the product PL BV 400 RT Viscometer Part PL0810 3060 conforms with the requirements of EC Directives 89 392 91 368 amp 89 336 by complying with the following Harmonised European Standards Safety EN61010 1 EMC EN55022 Conducted emissions Class B Radiated emissions Class B EN50082 ESD C Radiated immunity A Fast Transient Burst B Surge immunity B Conducted immunity A S Dm Dr S O Donohue Head of Instrumentation Church Stretton 8 June 2010 Document 6 27121 v1 05 PL BV 400 RT VISCOMETER WARRANTY Extract from General Conditions of Sale Subject as hereinafter stated if any goods supplied are proved to the reasonable satisfaction of the Seller to be defective in material or workmansh
14. eral each component view contains a number of common items and options The actual items available in a view are dependent on the component selected The component view for the PL BV 400 RT Viscometer is shown below gt VISCOMETER Ready Status Bar On line Help Button kd Parameter Set Value This action autozeros the DP detector Purge Time secs ame Parameter Grid el l tika DP Autozero i 2 E Action List DF Autozero DF Purge E EA IP Autozero IP Purge Action Button s Status Bar This displays information about the viscometer component and it s current status On line Help Button This is a direct link to the on line help for the viscometer component view Parameter Grid This displays the current set purge time for both the DP and IP purges To set and update the purge time enter the required value in the Set Value rm column and press the Update button Uedate_ To undo the new set value prior to pressing the Update button press the Undo button Ej To reset the purge time back to the default value press the Factory Reset button 9 ES Document 6 27121 v1 05 11 PL BV 400 RT Viscometer Operator s Manual Chapter 3 The Graphical User Interface Help Output Window This displays a simple summary help for the purge time parameter and viscometer actions To view this information select the parameter or action The information displayed in the H
15. ip within a period of 12 months from the date of despatch and the Buyer notifies such defect to the Seller in writing within fourteen days of it becoming apparent the Seller shall repair or replace at its option the goods or any part thereof free of charge and any repaired or replacement goods will be guaranteed on these terms for the unexpired portion of the 12 month period PROVIDED THAT the Seller shall be under no liability in respect of any defect that has arisen because of fair wear and tear or where the goods have not been used maintained stored or protected in the proper manner or the goods have been altered in any way whatsoever or have been subject to unauthorised repair or the goods have been improperly installed or connected unless the Seller carried out such installation and connection or in the case of Instrument Consumables including wetted parts lamps etc they prove defective as aforesaid more than 30 days after delivery notwithstanding the foregoing provisions of this condition or the Buyer is in breach of any other contract made with the Seller such as the Company s General Conditions of Sale SAVE AS PROVIDED ABOVE THE SELLER WILL BE UNDER NO LIABILITY UNDER THE CONTRACT FOR ANY PERSONAL INJURY DEATH LOSS OR DAMAGE OF ANY KIND WHATSOEVER WHETHER CONSEQUENTIAL OR OTHERWISE INCLUDING BUT NOT LIMITED TO LOSS OF PROFITS AND THE SELLER HEREBY EXCLUDES ALL CONDITIONS WARRANTIES AND STIPULATIONS EXPRESS OR IMPLIED STATUTORY C
16. mpartment The differential pressure DP and inlet pressure IP signals are obtained from the rear panel of the PL GPC 50 Plus analog output channels 3 DP and 4 IP 1 2 Specifications PL BV 400 RT Linearity 0 5 FS Viscometer Shear rate typical 3000 s Sensitivity Nsp 1x10 Pa s Baseline noise for DP output lt 0 25mV Baseline drift for DP output lt 5mV Capillary dimensions 0 01 in ID x 24 in L Recorder output differential 1mV Pa pressure Recorder output inlet pressure 10mV Pa Cell volume 120 uL Document 6 27121 v1 05 1 PL BV 400 RT Viscometer Operator s Manual Chapter 1 General Information 1 3 Installation Procedures 1 3 1 Configuring the PL BV 400 RT Viscometer The PL BV 400 RT Viscometer needs to be added to the instrument configuration in order to control it from the PL Instrument Control software To add the viscometer to the configuration open the PL Instrument Configuration Editor program and select Add Component from either the Configure menu or toolbar icon From the Add Component dialog select the PL BV 400 RT component Once the viscometer component has been added assign the correct Com port For further information on configuring the system then please see the on line help within the PL Configuration Editor program and the PL GPC 50 Plus Operator s Manual 1 3 2 Connecting the Detector Outputs to the PL DataStream Using the Detector output cables su
17. ning all and any necessary consents and approvals under planning and building regulations and by laws and for the preparation of the site the constitution of foundations and the provision of services so that the site is suitable to receive the goods Unless expressly provided therein the contract does not include the installation erection or commissioning of any goods or equipment or the supervision thereof Where installation is included in the contract it is the responsibility of the Buyer to advise the Seller of prevailing site conditions and in particular but without prejudice to the foregoing physical characteristics availability of services normal labour working hours and any local or national labour arrangement or practices which might affect the work and any other relevant factors Any additional costs caused by any interruption or delay not attributable to the Seller or to its employees or because the Seller cannot gain access to the site shall be charged to the Buyer together with an appropriate allowance for profit The Buyer shall also be responsible for providing a safe and healthy working environment for the Seller s employees and the Seller s subcontractors and their employees and shall bear or reimburse the Seller against any loss damage or compensation due to any person in relation to any death or personal injury or destruction or damage to property except to the extent that the same is due to the negligence of the Seller and the Buye
18. ot connected Ensure the correct Com port has been assigned within the PL Instrument Configuration Editor program Ensure the PL GPC 50 Plus is powered on and the USB cable is connected No response received from the device Incorrect Com port assigned to the component or communications lost with the component e g power failure Ensure the correct Com port has been assigned within the PL Instrument Configuration Editor program Ensure the PL GPC 50 Plus and or component is powered on If assigned Com port is correct and the system is powered on then contact Varian or your local agent Unrecognized response from the device Turn the PL GPC 50 Plus off and then on again ensure the control software has been closed before turning the instrument off If this error persists then contact Varian or your local agent The device rejected the last command Incorrect component assigned to the Com port Ensure the correct component has been assigned to the correct Com port within the PL Instrument Configuration Editor program Autozero operation could not completely cancel the transducer offset The Viscometer failed to autozero the DP signal correctly Purge the DP Transducer and ensure it is flushed with solvent If this error persists then contact Varian or your local agent The device returned an error The component failed to complete an action Reinitialize the component from the PL Instrument
19. oth detectors are connected Purge both the IP and DP transducers and allow the system to stabilize Once the system has stabilized record the IP value Document 6 27121 v1 05 4 PL BV 400 RT Viscometer Operator s Manual Chapter 2 Overview of Viscometry Theory 2 Overview of Viscometry Theory 2 1 Theory of Online Viscosity Measurements When a polymer dissolves in a liquid the interaction of the two components stimulates an increase in polymer dimensions over that of the unsolvated state Due to the vast difference in size between solvent and solute the frictional properties of the solvent in the mixture are drastically altered and an increase in viscosity occurs which should reflect the size and shape of the dissolved solute even in dilute solutions gt The dissolved polymer coil disturbs the linear flow of solvent gt resulting in a resistance to flow which is observed as an increase eee gt in viscosity This was first recognized in 1930 by Staudinger who found an empirical relation between relative magnitude of increase in viscosity and the molar mass of the polymer The Intrinsic viscosity n is a measure of the viscosity of a polymer solution as the concentration tends to zero i e at very low concentrations It is this parameter therefore that is a characteristic of isolated polymer chains in solution and can be considered to be proportional to the density of the polymer coil For a giv
20. p Sales amp Service Service Tel 44 1694 723581 Fax 44 1694 722171 Service Tel 44 1694 724333 Fax 44 1694 723994 In the Benelux countries Varian B V Technical Assistance amp Service Tel 31 118 671500 Fax 31 118 671502 Document 6 27121 v1 05 Tel toll free 800 767 3963 Tel 413 253 9554 Fax 413 253 2476 In Germany Varian Deutschland GmbH Technical Assistance amp Service Tel 49 6151 7030 Fax 49 6151 703237 iii Tel 61 3 9566 1134 Fax 61 3 9566 1471 In France Varian SA Technical Assistance amp Service Tel 33 1 6986 3838 Fax 33 1 6928 2308 SAFETY The following general safety precautions must be observed during all phases of operation service and repair of this detector Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the detector Varian assumes no liability for the customer s failure to comply with these requirements Signs and Pictograms Used in this Manual WARNING ATTENTION NOTE Document 6 27121 v1 05 WARNING THE WARNING SIGN DENOTES A HAZARD IT CALLS ATTENTION TO A PROCEDURE OR PRACTICE WHICH IF NOT CORRECTLY CARRIED OUT OR ADHERED TO COULD RESULT IN SEVERE PERSONAL INJURY OR DAMAGE OR DESTRUCTION OF THE INSTRUMENT PLEASE DO NOT PROCEED BEYOND A WARNING SIGN UNTIL THE INDICATED CONDITIONS ARE FULLY UNDERSTOOD AND MET ATTENTION
21. pplied attach the BNC connector ends of the cables to the Ports labelled Analogue Output 3 and 4 on the rear of the PL GPC 50 Plus and the other ends to the Detector Input Channels e g Channel 2 and 3 on the front of the PL DataStream The differential pressure DP and the inlet pressure IP outputs from the PL BV 400 RT viscometer are connected internally to analogue outputs 3 and 4 respectively e __ ANALOGUE OUTPUT OUTPUT CI gt a CO PL DataStream The PL BV 400 RT Viscometer also has a Specific Viscosity output which is obtained from analogue NOTE output 8 N THE SPECIFIC VISCOSITY OUTPUT CANNOT BE USED WITH CIRRUS MULTI WARNING Document 6 27121 v1 05 2 PL BV 400 RT Viscometer Operator s Manual Chapter 1 General Information 1 3 3 Connecting the PL BV 400 RT Viscometer Inlet Outlet The PL BV 400 RT Viscometer is connected in parallel to the RI detector The plumbing connections are all situated within the column oven compartment The PL BV 400 RT Viscometer and RI detector should be connected as follows 1 Connect the supplied 30 cm 0 010 in ID stainless steel tube from the outlet of the column to one of the supplied Valco T pieces 2 From the same Valco T piece connect the supplied 10 cm 0 010 in ID stainless steel tube to the inlet of the viscometer bottom connection of the viscometer and connect the approximately 40 cm 0 010 in ID stainless steel tube to the inlet of the RI
22. r shall except as aforesaid keep the Seller fully indemnified in respect thereof Document 6 27121 v1 05 ii HEALTH AND SAFETY PL BV 400 RT Viscometer This detector should be used only in accordance with the instructions stated within this manual If the detector is used in a manner not specified by the manufacturer the protection provided may be impaired Users should observe the following general safety precautions Ensure that the instructions within this manual are understood and carried out in the operation of the detector All persons utilizing the detector should have adequate training in its proper set up operation and particularly its safety features Access covers should not be removed by anyone other than properly trained personnel No attempt should be made to service the detector without authorization from Varian s service department and contravention of this may result in personal hazard or damage to the detector and will invalidate the manufacturer s warranty We stress the importance of standard laboratory safe practice e g COSHH regulations for dealing with electronic laboratory equipment solvents etc in preventing accidents fires or potentially hazardous conditions If in any doubt about the use of the detector contact your local Varian office or local distributor In the UK and Europe United States Australia Varian Inc Varian Inc Varian Australia Pty Ltd Technical Assistance Technical Assistance am
23. raft Copol PS PMMA Poly phenyl siloxane 10 o Polybutadiene 18 20 22 24 26 28 30 Elution Volume 5ml counts THF Solvent Figure 2 2 1 A Universal Calibration Plot Therefore for an unknown polymer sample the Universal Calibration is used to convert the intrinsic viscosity determined for each slice across the distribution from the viscometer to molecular weight 2 3 Polymer Branching The determination of the degree of long chain branching has long occupied polymer chemists In polymer solutions the branching factor g is the starting point for many branching calculations Document 6 27121 v1 05 6 PL BV 400 RT Viscometer Operator s Manual Chapter 2 Overview of Viscometry Theory Ye MID g A 7 Where 7p is the intrinsic viscosity of the branched polymer and 7 is the intrinsic viscosity of the linear polymer of the same molecular weight s is the structural model parameter which is user defined 2 4 Four Capillary Viscometry Theory The PL BV 400 RT Viscometer employs the fluid flow equivalent of the analogous Wheatstone bridge electrical circuit Solvent travels down a bridge of four capillaries of equal resistance arranged as shown in Figure 2 4 1 IP IP Inlet pressure DP Differential pressure Specific viscosity 4DP IP 2DP From columns IV Specific viscosity Concentration In the limit as conc tends to zero Figure 2 4 1 Plumbing Diagram of PL BV 40
24. recommended procedures Document 6 27121 v1 05 CONTENTS 1 GENERAL INFORMATION 1 1 INTRODUGTION i a eras ea cs Pe aa aa a Tet 1 2 SPECIFICATIONS ccccecccecceeccecceceneececeeeececcuceaueceecaeececcueeaeeceeceteaeeeaees 1 3 INSTALLATION PROCEDUREG escceccecceeececcececeececeeeececcuseceeceeeaeeneeeuss 1 3 1 Configuring the PL BV 400 RT Viscometer 1 3 2 Connecting the Detector Outputs to the PL DataStream 1 3 3 Connecting the PL BV 400 RT Viscometer Inlet Outlet 2 OVERVIEW OF VISCOMETRY THEORY 2 1 THEORY OF ONLINE VISCOSITY MEASUREMENTS sse eeeennnzznnnnzzznnnzznzi 2 2 UNIVERSAL CALIBRATION 0 cccccccessececcccssececccceseeeececeseesecteaseeeeeseees 2 3 POLYMER BRANCHING cc c0eeecececceeseeceeceeseceeceeesceeeeceeneceeeseeseeseeseens 2 4 FOUR CAPILLARY VISCOMETRY THEORY 2 ccccccssseceecceeseeeeceeeseeseeseees 3 THE GRAPHICAL USER INTERFACE 3 1 OVERVIEW nuanean nanna e en 3 2 SUMMARY AV IEW a vex cance qa a a ana ta an uanil ecaceodtaciameabacttnrabeciamcneack 3 3 COMPONENT VIEW is ins ch aitnjt daisies Marka tika a u oa ibe a Ne baa Reha ti 4 TROUBLESHOOTING 4 1 ERROR Soen a kai aa disa bi ii bb i ei iii ik 4 1 1 PL BV 400 RT Viscometer Errors 4 2 GENERAL TROUBLESHOOTING GUIDE L nn nn mnn nn nn nn enza APPENDIX 1 CLEANING amp DECONTAMINATION PROCEDURES APPENDIX 2 PARTS LIST Document 6 27121 v1 05 Vi Chapter 1 General Information 1 General Information
25. s Manual Appendix 2 Parts List Appendix 2 Parts List PLO810 3071 PL BV 400 Bridge Assembly for BV 400HT PL GPC 120 220 PLO810 3087 PL BV 400 Bridge Assembly for BV 400RT PL GPC 50 PLO810 3072 PL BV 400 Transducer Assembiv PL GPC 220 PLO810 3073 PL BV 400 Transducer Assembly PL GPC 120 PLO810 3074 PL BV 400 Electronics Control Module PLO810 3076 PL BV 400 Delay Columns x2 PLO810 3077 PL BV 400 Pulse Dampener PLO810 3078 PL BV 400 IP Transducer PLO810 3079 PL BV 400 DP Transducer PLO810 3080 PL BV 400 IP Purge Valve PLO810 3081 PL BV 400 DP Purge Valve PLO810 3082 PL BV 400 Transducer to Bulk Head Cable PLO810 3083 PL BV 400 Control Cable PLO810 3084 PL BV 400 Displav PCB PLO810 3085 PL BV 400 Main PCB PLO810 3086 PL BV 400 PSU Document 6 27121 v1 05 PL BV 400 RT Viscometer Operator s Manual
26. tup Email l Date Time Procedure ID Select 28 06 2006 13 25 33 VISCOMETER Get IP Output Could not initialise specified comms port Figure 4 1 1 Diagnostic Output Window Note The information displayed in last two Tabs is primarily for service diagnostics and the Window does not need to be open for normal operation of the instrument If an error is displayed it needs to be cleared in order for the diagnostic window to be closed allowing access back to the PL Instrument Control software To clear an error press the Select button to highlight the row and press the Clear button Multiple errors can be selected at a time Once all errors have been cleared the diagnostic window can be closed Clearing an error will stop all procedures that are running and attempting to communicate with the viscometer To re establish communications with the viscometer either select the Reconnect option from the nstrument menu or return to the component view and resend the parameter or repeat the required action The errors that can be displayed from the software for the viscometer are listed on the following pages Document 6 27121 v1 05 13 PL BV 400 RT Viscometer Operator s Manual Chapter 4 Troubleshooting 4 1 1 PL BV 400 RT Viscometer Errors Error Cause s Action Could not initialize specified comms port Incorrect Com port assigned to the component the PL GPC 50 Plus is not powered on or the USB cable is n
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