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Perkin-Elmer TITAN MPS, User Manual

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Perkin-Elmer TITAN MPS User Manual Download Page 69

59

Performing a Digestion

Performing a Digestion

ATTENTION: 

Prior to the very first digestion, a pressure calibration must be 

performed. Please see Pressure Calibration on page 69. 

General

After turning the unit on and logging in, you will see the 

Home

 screen of the Titan 

MPS controller.

Figure 5-2.

The Titan MPS Home Screen

Performing a sample digestion consists of a few basic steps.

1. Select the digestion method.

2. Weigh samples into the vessels and add reagents.

3. Enter the digestion and sample data.

4. Review the method and place the samples in the oven.

5. Begin the digestion.

6. Review the results.

Summary of Contents for TITAN MPS

Page 1: ...TITAN MPS Customer Users Guide ATOMIC SPECTROSCOPY ...

Page 2: ......

Page 3: ...Titan MPS Users Guide ...

Page 4: ...l consequential damages in connection with fur nishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or translated into any language without the prior written permission of PerkinElmer Inc Copyright 2013 PerkinElmer I...

Page 5: ...ranty Limitation of Warranty 22 Preparing Your Laboratory Introduction 23 Environmental Requirements 23 Exhaust Line Venting Requirements 24 Lab Space Requirements 24 Microwave Radiation 2 6 System Description Titan Microwave Prep System 27 Pressure Vessels and Turntables 34 Specifications 37 Installation Unpacking 39 Power Cord Options 41 Installation 46 Operation Method Preparation 53 System Log...

Page 6: ...ethod 97 Edit Method 98 Data Management 99 File Management Data Export 100 Maintenance Cleaning 101 Turntable System 106 Fuse Replacement 107 Repairs Customer Service 107 Maintenance Tips 108 Output Power Measurement 108 Troubleshooting Overview 113 Microwave Oven 114 Control Unit 116 Pressure Digestion Vessel 117 Appendix References 119 Conversion Table 121 Index of Controller Screens 121 ...

Page 7: ... this manual For your own safety and to avoid property damage you must strictly heed these warnings The safety signals are printed in boldface or are otherwise marked throughout this Safety Information in the Manual Safety information is contained in Chapter 1 of this manual Before setting up and operating this instrument carefully read the safety precautions described in this chapter and observe ...

Page 8: ...alerts you to the risk of hot surfaces that could cause personal injury to yourself or other persons Details about these circumstances are in a box like this one This symbol alerts you to the risk of strong magnetic fields that could cause injury to persons wearing a heart pacemaker or having metallic implants Details about these circumstances are in a box like this one Caution A caution indicates...

Page 9: ... in this chapter 2 Preparing Your Laboratory The preparation of your laboratory needed for the Titan MPS 3 System Description This chapter contains information on the components of the instrument how it works and instrument specifications 4 Installation Information on moving and reinstalling your instrument is provided 5 Operation Information on hardware and software operation 6 Maintenance Mainte...

Page 10: ... manual before you call a PerkinElmer service engineer The Troubleshooting chapter contains suggestions to help you determine what the problem may be offer a solution and prevent extended downtime or the need for a service call Conventions Used in this Manual Normal text is used to provide information and instructions Bold text refers to text that is displayed on the screen UPPERCASE text for exam...

Page 11: ...ratory environment is the responsibility of the analyst and the analyst s organization Please consult all documentation supplied before you start working with the instrument Carefully read the safety information in this chapter and in the other manuals supplied When setting up the instrument or performing analyses or maintenance procedures strictly follow the instructions provided Note This instru...

Page 12: ...ls Proper Use The instrument emits microwave radiation Never operate the microwave oven if the drop lid or the related lock mechanism have been damaged Contact Perkin Elmer Inc to obtain the required service Refer to the Repairs Customer Service on page 107 for contacts Note PerkinElmer products should only be used in a laboratory setting Explosion hazard The instrument is not designed for extract...

Page 13: ...t designed to prevent the spontaneous combustion of any solvent vapors that may escape into the oven chamber Heating in the pressure vessel can frequently result in digestion temperatures in excess of 200 C 392 F The Titan MPS has been specially developed for sample preparation for AAS and ICP spectroscopy procedures Temperature spikes 280 C 536 F can occasionally occur during the course of exothe...

Page 14: ...ions or modifications By qualified and trained users General Safety Information Performing microwave digestion procedures involves taking into account various safety precautions which go beyond those for general laboratory practices The following general safety information should therefore be read carefully prior to using the system and should be observed at all times The following information mus...

Page 15: ...bstances include explosives TNT etc perchlorates ether pyrophoric substances etc Pressure vessels Use only digestion vessels and spare parts authorized by Perkin Elmer for use with the Titan MPS Refer to the Repairs Customer Service on page 107 section for contact addresses Always wear safety glasses goggles and protective gloves when working with the pressure vessels Note any changes in the appea...

Page 16: ...es away from both yourself and other individuals Only open the digestion vessel under a fume hood or other exhaust system Particular care is required when working with hydrofluoric acid HF Due to the extreme damage it inflicts Observe all relevant data sheets and safety instructions Note Replace the vessels after around 5000 digestions to maintain reliable operating conditions and to prevent negat...

Page 17: ...the wall outlet used is equipped with a ground connection the supplied power cord will ensure proper connection If it is necessary to use an extension cord to connect the system to the power supply only a three wire cord with a ground connection may be employed The instrument should not be set up near any devices which are sensitive to electromagnetic radiation Should there be any suspicion or ind...

Page 18: ...ay occur after the vessel has been removed from the microwave oven Gas Exhaust High Voltage The housing cover may only be removed by authorized trained personnel The instrument must be disconnected from the power outlet before being serviced Rupture discs as overpressure protection Use only original Perkin Elmer rupture discs and pressure seals These can be obtained from Perkin Elmer Inc Refer to ...

Page 19: ...ng on page 33 An emergency shut off occurs in case of a rupture disc break Pressure Control The system is also equipped with a pressure monitoring system for a reference vessel located at position one as described in the Repairs Customer Service on page 107 Over Temperature Protection For safety reasons the microwave automatically switches itself off in case the magnetron the microwave oven or the...

Page 20: ...n up spilled chemicals immediately and dispose of them properly Do not allow smoking in the work area Smoking is a source of significant contamination and also a potential route for ingesting harmful chemicals The laboratory manager is responsible for warning users of this instrument concerning biohazardous materials that are processed in this instrument and about waste that results from the opera...

Page 21: ...ature range 5 C to 40 C 41 F to 104 F Ambient relative humidity 20 to 80 without condensation Altitude in the range 400 m to 2000 m 1300 to 6500 feet The location must be free of dust smoke and corrosive fumes Mains fluctuations not exceeding 10 of the nominal voltage You can store the instrument safely under the following conditions Ambient temperature 20 C to 60 C 4 F to 140 F Ambient relative h...

Page 22: ...ake adjustments replacements repairs or modifications to this instrument except as described in the documentation supplied with the instrument Lethal voltages are present at certain areas within the instrument Installation and internal maintenance of the instrument should only be performed by a PerkinElmer service engineer or similarly authorized and trained person When the instrument is connected...

Page 23: ...d Do not attempt to make internal adjustments or replacements except as directed in the manuals Disconnect the instrument from all voltage sources before opening it for any adjustment replacement maintenance or repair If afterwards the opened instrument must be operated for further adjustment maintenance or repair this must only be done by a PerkinElmer Service engineer or a similarly trained and ...

Page 24: ...e FCC Rules These limits are designed to provide reasonable protection against harmful interference when the instrument is operated in a commercial environment This instrument generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this instrument in a residenti...

Page 25: ...U S Federal Communications Commission emission regulations and because of this violation could void the user s authority to operate this instrument This symbol indicates the risk of electric shock Before opening disconnect mains High voltage Use only cable with plug and protective earth Explosive Vessel under pressure open carefully after cooling This symbol indicates the risk of hot surfaces Proh...

Page 26: ...cates the on position of the main power switch or circuit breaker With the switch in this position the instrument is connected to the line power supply but is not necessarily switched on and operational This symbol indicates the operational on off switch This symbol indicates alternating current When this label is attached to an instrument it means refer to the manual ...

Page 27: ...Warning Labels on the Instrument Warning Label On The Inside Lid of the Instrument Figure 1 1 Warning label on the Inside of the lid Item Description 1 Vessel under pressure open carefully after cooling 1 ...

Page 28: ...plug is not to be removed during or after installation 2 Danger For protection against fire hazard replace only the same type and rating of fuse 3 High Voltage To avoid electrical shock disconnect power supply before changing the fuse Disconnect supply whenever cover is removed 4 Caution This device is to be serviced only by properly qualified service personnel Consult the service manual for prope...

Page 29: ...gure 1 3 Warning labels on the right side of the instrument Item Description 1 Prohibited for persons with heart pacemakers 2 Danger Before opening disconnect mains Use only cable with protective earth 3 High Voltage Before opening disconnect mains Use only cable with protective earth 1 3 2 ...

Page 30: ...linfo dts_instrumentdeconprocedure pdf Certificate form http www perkinelmer com Content technicalinfo dts_perkinelmercertificationofdecontaminationform pdf If you do not have access to the internet and are located in the U S call toll free at 1 800 762 4000 or 1 203 925 4602 8 30 a m 7 p m EST and speak to Customer Support In Canada call toll free 800 561 4646 and speak to Customer Support If you...

Page 31: ...r s environment Requirements for waste collection reuse recycling and recovery programs vary by regulatory authority at your location Contact your local responsible body e g your laboratory manager or authorized representative for information regarding applicable disposal regulations Contact PerkinElmer at the web site listed below for information specific to PerkinElmer products Web address http ...

Page 32: ...ed as are claims for replacement of parts meant to be expended during the operation of the equipment Perkin Elmer Inc also includes its digestion vessels under this warranty However high temperatures 280 C 536 F such as may briefly occur when exothermic reactions take place can result in irreversible damage to the TFM vessels Since such scorching can only be avoided by proper sample and reagent se...

Page 33: ...ocation where the Titan MPS is to be installed must fulfill the criteria listed below Indoors Free from vibrations Free from dust smoke and corrosive fumes Out of direct sunlight Away from radiators and heaters Have a suitable fume ventilation system Do not use above 2000 m in elevation Ambient room temperature between 15 C to 35 C 59 95 F In addition the temperature should lie between 40 C 40 F a...

Page 34: ...ould be vented to the outdoors or be connected to an exhaust system The oven must not be set up in wet conditions it is not resistant to water sprays and not under the extraction hood exhaust increased risk of corrosion We recommend setting the unit up next to the extraction hood exhaust in order to lead the vent hoses to this extraction hood exhaust Note You are responsible for assuring that appr...

Page 35: ...ons Specifications For information on the instrument s power supply see Specifications section in Chapter 3 System Descriptions Power Cord Options For information on the power cord options see Power Cord options in Chapter 4 Installation Corrosion of the unit due to placement in a chemical hood or other corrosive environment is not covered under warranty Warning ...

Page 36: ...y be employed The unit should not be set up near any devices which are sensitive to electromagnetic radiation If necessary a warning sign or label indicating Caution Microwave Emissions should be applied or attached to the unit Should there be any suspicion or indication of increased levels of microwave radiation please immediately inform PerkinElmer your PerkinElmer Representative and stop using ...

Page 37: ...ng mechanism and a circular sample chamber for uniform microwave distribution The oven has a chemically resistant PFA coating protecting it from corrosion Three over temperature switches and four micro switches guarantee the necessary operating safety The microwave unit is equipped with a ventilation system the area of the oven ventilation is completely separated from the electronic and magnetron ...

Page 38: ...ference vessel This records the internal vessel pressure If the vessel is approaching the maximum oven program pressure the system automatically switches to a pressure controlled mode for the microwave output Two software controlled unpulsed 2 45 GHz magnetrons provide up to 1 500 W output power The microwave is controlled by a built in control unit with color touchscreen After entering the desire...

Page 39: ...llowing figures illustrate the various connections on the Titan MPS Figure 3 2 Instrument Connections Item Description Item Description 1 Drop lid with vent connection 4 Ethernet 2 Built in control unit 5 Mains power 3 USB connection 6 Power switch fuse 2 3 4 5 6 1 ...

Page 40: ...he mains power switch is located on the right hand side of the unit The switch functions also as a thermal fuse not self resetting Figure 3 3 Electrical Connections Item Description 1 Ethernet 2 Mains power connection 3 Main power switch fuse 1 2 3 ...

Page 41: ...rated from the electronic and magnetron ventilation For laboratories that cannot meet the nominal exhaust requirements of the Titan MPS an optional external exhaust fan is available to ventilate the oven cavity and the Gas Containment Manifold Figure 3 4 Ventilation Connections Item Description 1 Exhaust hoses 2 Magnetron cooling 3 Electronic cooling 3 2 1 ...

Page 42: ...grated control unit with 5 7 inch color touch screen and graphics display is used to control the microwave oven The English German French Italian and Spanish language software is pre installed at the factory Figure 3 5 Controller Main Window ...

Page 43: ...temperature monitoring information is passed on to the power control module which uses the highest measured temperature to regulate the oven power Continuous adjustment of the magnetron s output allows the digestion temperature of every sample to be tightly controlled Only temperatures above 50 C 122 F are displayed Temperatures below 50 C 122 F are indicated on the display as low Key Function Met...

Page 44: ... and Turntables All Perkin Elmer pressure vessels are manually operated A rupture disc placed on the vessel seal limits the interior pressure of each vessel type to a maximum permissible value appropriate for the vessel For all vessels acid vapors that escape when a rupture disc activates are guided to the Gas Containment Manifold at the top center of the turntable The gasses are then vented throu...

Page 45: ...ntables Figure 3 6 Complete 16 position standard pressure assembly with DPC cap 15 standard pressure vessels made of TFM 1 standard pressure vessel with DPC pressure cap 16 position Turntable 16 position Gas Containment Manifold ...

Page 46: ...p In addition this vessel consists of a ceramic pressure jacket and a TFM insert 7 high pressure vessels made of TFM with ceramic insert and TFM liner 1 high pressure vessel with DPC pressure cap with ceramic insert and TFM liner 8 position turntable 8 position Gas Containment Manifold Figure 3 7 Complete 8 position high pressure assembly with DPC cap ...

Page 47: ...in breaker Magnetron frequency 2450 MHz Magnetron power continuous 1200 W Magnetron power peak 1500 W Exterior dimensions W x D x H 530 x 630 x 420 mm 20 9 x 24 8 x 16 5 inches Interior dimensions ID 360 mm 14 2 inches Weight approx 53 kg 117 lb without vessels Noise level 70 dB A DTC temperature range 50 C 260 C 122 500 F DPC pressure range Standard 75mL vessel 0 40 bar 580 psi High pressure 100m...

Page 48: ... memory 100 programs 25 preprogrammed Data file memory approximately 1000 data files Display 320 x 240 pixel Interface Ethernet USB Pressure Vessels PKI 75 PKI 100 Volume 75 ml 100 ml Operating Pressure 40 bar 580psi 100 bar 1450psi Maximum Temperature 230 C 446 F 250 C 482 F Minimum Fill Volume Acid 7ml 7ml Vessels Per Rotor 16 8 Material of Construction TFM TFM Ceramic ...

Page 49: ...diately A representative of the shipping carrier must be present for insurance purposes Unpacking the Titan MPS The Titan MPS is shipped in one carton Tools You Will Need Snips for banding and tie wraps Remove the Top of the Box Use snipers to remove the banding which is around the box 1 Check the shockwatch and the two tip and tell indicators Record the status of the indicators on the waybill if ...

Page 50: ... The bench should be nearby Recycling the Instrument Box If you plan on moving your Titan MPS you may want to keep the cardboard box that the Titan MPS was shipped in If you need to dispose of the cardboard box please do so in accordance with local environmental regulations SUPPLIES ACCESSORIES AND REPLACEMENT PARTS can be ordered directly from PerkinElmer For further information visit our website...

Page 51: ...Power Cord Options The Titan MPS offers a number of power cord options The cord is 2 5 meters long and black Plug Type C 19 Connection on Titan MPS Part Number Country Plug N3135000 Europe N3135001 Switzerland N3135002 Italy ...

Page 52: ...42 Installation N3135003 India South Africa N3135004 United Kingdom requires receptacle 09290305 not included N3135005 Australia N3135006 Israel Part Number Country Plug ...

Page 53: ...43 Power Cord Options N3135007 China N3135008 Brazil N3135009 Denmark requires receptacle 09290305 not included N3135010 North America included Part Number Country Plug ...

Page 54: ...uck and Boost Transformer in Japan N3135012 In Line Connector For use with the Buck and Boost Transformer in Japan N3135013 Buck and Boost Transformer 0 5 KVA Japan and U S Canada 100 VAC 50 60 Hz Japan 208 VAC 60 Hz US Canada 09290305 Receptacle Surface Mount Receptacle for Denmark and United Kingdom ...

Page 55: ...45 Power Cord Options Buck and Boost Transformer 0 5 KVA Japan and U S Canada Connections ...

Page 56: ...y a three wire cord with a ground connection may be employed The unit should not be set up near any devices which are sensitive to electromagnetic radiation If necessary a warning sign or label indicating Caution Microwave Emissions should be applied or attached to the unit Should there be any suspicion or indication of increased levels of microwave radiation please immediately inform PerkinElmer ...

Page 57: ...laboratory is responsible for ensuring that the exhaust system can appropriately vent the released gases Make sure that all ventilation procedures conform to applicable laws Note Important Note for North American Users Voltage of mains supply has to be in the range of 230V 15V AC Even with a maximum load of approximately 2700 W the supply voltage should not drop below 215 V AC Low voltage can resu...

Page 58: ...ing on the device please log in as User or Administrator First Time Setup Power the system on and wait for it to initialize When presented with the login screen select Admin and enter the factory default code of 0000 and press OK This will then take you to the home screen of the Titan MPS controller Item Description 1 Power switch and fuse 2 Power plug 3 Ethernet interface 1 2 3 ...

Page 59: ...will allow the release of the top lid of the Titan MPS Figure 4 4 The Titan MPS home screen With the top of the Titan MPS now open remove and packing material from within the oven cavity and any that remains around the body of the Titan MPS The turntable and vessels can now be unpacked from their box Remove the vessels ...

Page 60: ...and gently place it within the oven cavity The base of the turntable is keyed to match the semi circular drive at the base of the oven cavity Align the turntable with the support ring and carefully rotate the turntable until the key lines up with the semi circular drive and the turntable drops into place Ensure that the turntable is centered in the oven cavity and that it rests firmly on the suppo...

Page 61: ...des and the language of the interface can be set The global maximum operating parameters for digestion programs can be set here as well but it is recommended to leave these at the factory settings unless directed otherwise by a service technician Figure 4 6 The Setup screen with the Set Time button at the bottom ...

Page 62: ...cal date and time and the press save to store the information Press back to return to the home screen The Titan MPS is now ready to use Figure 4 7 The Date and Time setup screen For a complete list and explanation of the instrument Setup menu please refer to the Appendix on page 119 ...

Page 63: ... increase in vapor pressure In addition to vapor pressure reaction gasses primarily carbon dioxide generated by the decomposition of carbon containing samples also generate pressure The total pressure within the vessel is therefore dependent on the sample temperature the amount and carbon content of the sample and volume of the vessel remaining after reagent addition All Titan MPS digestion vessel...

Page 64: ... target temperature to complete the digestion Caution Reaching peak digestion pressure Peak digestion pressure typically occurs several minutes after the target temperature has been reached A rupture disc release may occur even after the sample temperature has reached a constant level Caution Rupture disc and seal replacement Depending on the digestion parameters the metal rupture discs and pressu...

Page 65: ...ee the following figure Figure 5 1 The Keyboard and Numeric Keypad Always wear eye protection and appropriate PPE Always wear safety glasses goggles a lab coat and protective gloves when working with acids pressure vessels and during cleaning Caution Use only digestion vessels and spare parts authorized by Perkin Elmer for use with the Titan MPS These can be obtained from Perkin Elmer Refer to the...

Page 66: ...e pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the gas containment manifold when vessels experience excessive pressure In rare cases pressure release may occur after the vessel has been removed from the microwave oven Always make sure the vent opening on pressure vessel faces away from both yourself and other individuals Hot gases ...

Page 67: ...ete datafiles and perform method development A list of the access restrictions for each login is listed below Note All digestion vessels are subject to a long term aging process which is dependent on the type and frequency of digestions It is recommended to replace the digestion vessels after approximately 10 000 digestion cycles to maintain reliable operating performance Caution The minimum liqui...

Page 68: ...list X X Edit method on Favorites list X Create a method X Data Section Select a Datafile X X Review previous digestions X X Export Delete Datafiles X Digestion Start Edit Digestion Comment X X Edit Sample Details X X Review digestion parameters X X Select the number of vessels X X Select Rename a Datafile X X Edit the method in realtime X ...

Page 69: ...ng the unit on and logging in you will see the Home screen of the Titan MPS controller Figure 5 2 The Titan MPS Home Screen Performing a sample digestion consists of a few basic steps 1 Select the digestion method 2 Weigh samples into the vessels and add reagents 3 Enter the digestion and sample data 4 Review the method and place the samples in the oven 5 Begin the digestion 6 Review the results ...

Page 70: ...me screen and select the chosen method which will highlight the method and then press the Select button 3 For replacing or editing methods on the favorites list please refer to Method Creation and Editing Favorites on page 73 Weigh Samples Into the Digestion Vessels Using a weigh boat or similar accurately weigh the sample and quantitatively transfer the sample to a digestion vessel When adding th...

Page 71: ...ool and then place the seal with the rupture disc onto the vessel body At this point the cap can be placed on the vessel and the vessel with sample is now ready to be placed in the Titan MPS Figure 5 4 Expanding the lip on the TFM seal Caution Vessel minimum fill amount In each pressure vessel no less than 5ml of liquid should be employed so that the temperature sensor can determine the sample tem...

Page 72: ...t manifold Each vessel must be securely connected to the gas containment manifold by gently tightening the thumbscrew on the gas containment manifold over the threads on the vessel cap Figure 5 5 Do not cross thread the Gas Containment Manifold connectors Note The caps of the vessels do not need force to be tightened Lightly tightening by hand is all that is required for reliable performance Note ...

Page 73: ...e Digestion and Sample Information Once the method favorite has been selected the Home screen will be displayed and the Method button will show the name of the currently selected method 1 Press the Start button to display the digestion comment screen and to begin the process of digestion Caution The supplied vent tubes and hoses must always be properly connected and attached to an adequate exhaust...

Page 74: ...een select the text field and enter information or comments about the digestion 3 Pressing the Sample Details button will open the Sample Details screen This will allow data entry for each individual sample Digestion Comments and Sample Details are optional The Next button moves forward in the digestion process ...

Page 75: ...le 4 For 16 vessel configurations press Next when on the Sample Details 1 8 screen to enter details for sample 9 16 5 When all the sample details have been entered and Next selected the Digestion Comments screen will appear 6 On the Digestion Comments screen pressing Next will move to the Digestion Review screen ...

Page 76: ...gh Pressure 8 vessel configuration press the gray vessels button and enter the number of sample prepared An information screen will popup showing where the samples should be placed in the turntable for the best results These sample locations can also be used as a reference for Sample Details data entry Note If logged in as an Administrator the Digestion Review screen allows editing of the method p...

Page 77: ...n This is necessary when the laboratory has more than one DPC cap from multiple sets of vessels or as a backup Select the appropriate cap and press Start to begin the digestion Begin the Digestion 1 Once the digestion method has been reviewed press Start to begin the digestion The Titan MPS will execute the temperature program of the method while monitoring and controlling the sample digestion usi...

Page 78: ...ast ten minutes After this cool down time all vessels can be removed and can be placed under a vent hood or other exhaust system for further cooling The vessels should be opened in the hood only after an adequate cooling period This cool down time can vary depending on the total heating time and the final target digestion temperature The sample temperatures must be well below the boiling point of ...

Page 79: ...ing the Review Digestion button see Data Review File Management and Export on page 84 You can press Finish to return to the Home screen Pressure Calibration Creating a Pressure Calibration for a DPC Cap From the Home screen press the Method button This will open the Select Method screen On the Select Method screen are the 10 favorites to choose from and at the bottom select the Pressure Adjust but...

Page 80: ...n brings up a second button where the vessel type must be highlighted by pressing on the appropriate vessel type Press the green Select button to use the highlighted method and vessel and return to the Home screen Note Each vessel type has its own calibration parameters Be sure to correctly select the vessel type before continuing ...

Page 81: ...art button enter a digestion comment if desired on the Digestion Comment screen and press the Next button When this is done the Pressure Adjust Select Cap screen appears There are ten locations to select from to save a cap calibration If the laboratory is using more than one DPC cap multiple sets of vessels or as a backup this allows separate calibrations to be stored The Delete button allows a ca...

Page 82: ...bring up a second Pressure Adjust screen with additional instructions Follow the instructions for filling and placing the vessels and press Start The pressure calibration method will commence with data being displayed in real time At the finish of the calibration cycle the Pressure Adjust Deploy screen appears On the screen the calibration is accepted by pressing the Deploy button and then pressin...

Page 83: ...list provide an easy way to select the most common methods used during the workday The list comes pre populated when the Titan MPS is delivered To change the methods on the favorites list the you should first highlight the method you would like to replace by pressing on the appropriate button When the method is highlighted press the Replace button This will bring up the Replace Favorite screen ...

Page 84: ... list replaces and overwrites the method on the Favorites list and in the system memory 1 To edit a method highlight the method on the Favorites list to edit and then press the Edit button This will bring up the Edit Method screen Caution Methods that are overwritten are permanently changed When making large changes to a method it is advisable to first place a blank user method onto the Favorites ...

Page 85: ...d screen is the method name To change the method name press the current method name to bring up the keyboard 3 Using the keyboard use a combination of letters and numbers to create a unique method name It is advisable that the method name be descriptive enough to allow for easy recognition in the future In the center of the screen is the temperature program table a description of which follows in ...

Page 86: ...orking pressure of the vessel This allows a margin of pressure overhead should the digestion evolve more gas than expected Ramp The time in minutes the system should take to reach the target temperature for the program step Very aggressive short ramp times can cause exothermic reactions to proceed very rapidly and cause a rupture disc release and will limit the ability of the Titan MPS to moderate...

Page 87: ...hod Method creation is nearly identical to editing a method In this case a blank user method is placed onto the Favorites list and is then edited to create the desired method 1 To find a blank user method and place it onto the Favorites list highlight a method on the Favorites list and then presses Replace 2 When the Replace Favorite screen appears scroll down and highlight and select the first me...

Page 88: ...lank user method onto the Favorites list and then edit the user method This preserves the original list of methods in the system memory Note The digestion ends when no more time remains To ensure vessel cool down is performed at the end if the digestion as a final step the max pressure parameter should match the previous step the ramp and power should be set to zero and a time of ten minutes enter...

Page 89: ... pressing on the name of the datafile and then pressing elect This will then return the display t to the Home screen and the active datafile will be displayed at the bottom of the data button 3 This datafile will remain active and any digestion data will be saved to this file until it is changed Figure 5 20 The Select Review Datafile screen The second place where a datafile can be selected is on t...

Page 90: ...he gray datafile button opens the Datafile Select Rename screen 2 On the Datafile Select Rename screen select a different datafile by pressing the name of the datafile to highlight it and then pressing Select 3 This will select the highlighted Datafile and return to the Digestion Review screen ...

Page 91: ...cessed via the Digestion Review screen 1 On the Datafile Select Rename screen highlight the datafile that is to be renamed 2 The current name of the datafile will be displayed next to the Rename field To change the name press the current name of the Datafile and enter the new name on the keyboard that appears 3 When the name has been changed press the Save button to make this change permanent ...

Page 92: ...ower in response to this Figure 5 23 The realtime digestion information display During digestion the top of the Realtime Display screen shows a graph of the target temperature of the method program and the hottest measured sample temperature per turntable revolution Until the sample temperature rises above 50 C the display will only report the temperature as low The graph immediately below this di...

Page 93: ...iption Set Two columns C and bar pressure These are the current temperature set point and the maximum pressure for the selected vessel During the temperature ramp portion of the digestion the temperature setpoint will change to reflect the rising target temperature until the final digestion temperature has been reached Vessel shown as 0 in fig Two columns C and bar pressure These are the current m...

Page 94: ...created that cannot be modified and is used by the Titan MPS to display the digestion results and a text file which is a duplicate of the data and is available for export to a PC via USB stick or Ethernet connection The binary file ensures that the original data is always present and unmodified to ensure auditability and traceability Note Data is exported as a text file using semi colon separated ...

Page 95: ...he Digestion Finished screen On this screen is a button labeled Review Digestion This allows the for review the data for the just completed digestion Figure 5 24 The Digestion Finished screen When the Review Digestion button is pressed the Data Review screen appears which is similar to the Reatime Display in both appearance and function ...

Page 96: ...n is a time display and two buttons which can be used to advance or retreat the time A vertical line appears on the temperature and pressure graphs to indicate where in the digestion this point in time lies This point in time is used for the display of the individual sample numeric data located in the lower right of the screen This allows the review of the numeric data for the entire digestion Pre...

Page 97: ...od summary screen is the location where the data is stored and any digestion comment entered 1 Select the Next button to advance through the Sample Details screens 2 When data review is complete you can either select Finish on the Digestion Finished screen or Exit on the last Sample Details screen ...

Page 98: ...88 Operation Figure 5 27 Sample Details review 1 8 Figure 5 28 Sample Details review 9 16 ...

Page 99: ...ata button opens the Select Review Datafile screen Figure 5 29 The Select Review Datafile screen The File Manager button is in the upper right 2 Pressing the File Manager button allows access to the data export and file management capabilities on the Titan MPS Note You must be logged in as an Administrator to access the File Manager section of the Titan MPS controller ...

Page 100: ...agement screen Accessible only by Administrator log in Pressing the Export Data button will take the administrator to the Export Data screen See the following screen Figure 5 31 The Export Data screen Accessible only by Administrator login ...

Page 101: ...an be used as quick references on the operation of the Titan MPS interface Note To prevent problems or errors it is best to use a USB stick that has no other files on it The Erase USB button can also be used to clear the USB stick To export digestion data insert a USB stick and wait for the status to show ready Press the Copy all to USB button and wait for the system to complete the file copy Pres...

Page 102: ...92 Operation Select Method Choose Favorites Selecting a method from the Favorites List for digestion or making alterations to the Favorites List ...

Page 103: ...t Digestion Start Digestion Once a method has been chosen the steps needed to enter information complete a digestion and review the results Begin by accurately weighing samples into vessels and adding reagents ...

Page 104: ...94 Operation Sample Details Entering individual sample information ...

Page 105: ...95 Digestion Results Digestion Results Reviewing the data from completed digestions ...

Page 106: ...96 Operation Change Rename Datafile Locating and or renaming the datafile used to save digestion data ...

Page 107: ...97 Create Method Create Method The process of generating a new method Once saved the method is permanently changed ...

Page 108: ...98 Operation Edit Method The process of editing a current method Once saved the method is permanently changed ...

Page 109: ...99 Data Management Data Management Options available via the Data button on the Home screen ...

Page 110: ...100 Operation File Management Data Export Exporting or deleting the data files of previous digestions This action is irreversible and all files will be permanently deleted ...

Page 111: ...ny changes in the appearance of the pressure vessel which could indicate possible material fatigue e g deformation of the vessel difficulty screwing on lids etc even when the vessel is cold and not under pressure All such vessels should be immediately returned to PerkinElmer Inc for inspection Always wear eye protection Always wear safety glasses goggles and protective gloves during work which may...

Page 112: ... tube using the screw fittings ensuring a tight seal Vessels Since the vessels exhibit practically no memory effects it is generally sufficient to thoroughly rinse out the vessels with distilled water after each digestion procedure that results in complete sample digestion If discoloration is noted or if carry over is suspected the vessels are cleaned by a digestion using clean acid with no sample...

Page 113: ...m a Blank Digestion To carry out a blind digestion it is advisable to create a new program with only a three to five minute heating up time and 10 15 minute holding time for the final temperature The final temperature depends on the final temperature of the subsequent digestion and on potential gas development If no gas development is anticipated when carrying out the blank test the final temperat...

Page 114: ...e Figure 6 1 Exploded Diagram for Cap Item Description Item Description 1 Polarization foil 6 Glass ring 2 Glass prism 7 Cap insert 3 Thumbscrew 8 O ring 4 Connecting fitting 9 Assembling tool 5 Cap 9 8 7 6 4 3 5 2 1 ...

Page 115: ...nt Manifold tube by unscrewing it and removing it from the cap Be very careful not to damage the threads used to connect to the Manifold With the tube removed the cap disassembly tool with the long narrow post can be used to push out the inner piston and glass ring Insert the narrow post on the disassembly tool through the hole where the prism was located Place the bottom of the cap on a tabletop ...

Page 116: ...ve had a chance to dissipate before opening the lid 2 Carefully remove all vessels from the oven and open them in a hood as normal Be aware that if the remaining vessels have the same sample type and reagents as the vessel that vented they will also be under high pressure 3 Remove the gas Containment Manifold and then lift out the turntable 4 Rinse all components clean and allow them to dry 5 Rein...

Page 117: ...age parts are protected by a single fuse in each inverter These fuses can only be replaced by qualified service personnel Repairs Customer Service The unit employs high voltage and generates microwave radiation Any repair and service work may only be performed by properly trained and qualified personnel Always unplug the unit from the power supply before beginning any repair or maintenance work Th...

Page 118: ...nd will not affect its Function until it exceeds 2mm in height For a bulge taller than 2mm we recommend replacing the rupture disc and seal It is common for the TFM seal to last almost twice as long as the metal rupture disc Output Power Measurement The output power of the Magnetron has been thoroughly tested and certified by PerkinElmer before it is delivered However all magnetrons are subject to...

Page 119: ... 42 seconds and then the rise in temperature measured The output power can be calculated from this To perform the power test start the power test program from the operator library and follow the instructions in the program Start the power test program from the user library and follow the instructions in the program ...

Page 120: ...110 Maintenance ...

Page 121: ...111 Output Power Measurement The output power should be at least 1300 watts If values of less than 1300 watts are determined the contact PerkinElmer Service Repairs Customer Service on page 107 ...

Page 122: ...112 Maintenance ...

Page 123: ...describes the error messages for the system and their meaning Where possible corrective actions are suggested Servicing of the instrument by someone other than a PerkinElmer trained and authorized person will render the warranty null and void ...

Page 124: ...eck of the oven is clear Adjust the PFA tube to allow the lid to fully close Lid will not close Turntable not correctly engaged in drive axis Position turntable correctly Microwave does not start Defective door switches Unauthorized tampering with door switches Contact your PerkinElmer Service Representative Oven chamber gets very hot especially the turntable Acid volume too low Increase quantity ...

Page 125: ...switch of the supply line triggers often Magnetron defective Short circuit in the device Contact your PerkinElmer Service Representative Lack of sample pressure or samples not reaching temper ature Vessel seals not sealing effec tively Use the seal lip forming tool each time to ensure a cor rectly formed seal Replace old or damaged seals Problem Possible Cause s Corrective Action ...

Page 126: ... piston o rings Temperature begins with val ues 80 C during digestion start Defect on the temperature sensor Highly exothermic reaction Contact your PerkinElmer Service Representative After adding acids wait for the reaction to taper off before closing the caps Signals at unoccupied posi tions Wrong number of vessels configured Check and set number of ves sels prior to start Program stops during t...

Page 127: ...eplace the seal Expand the lip of the TFM seal using the TFM seal tools If the TFM seal is damaged replace the seal see Chapter 6 Maintenance Replacing TFM Seals and Metal Rupture Discs Corroded rupture disks Corroded rupture disks Turntable function faulty Sample quantity too big Spontaneous reaction DTC Temperature measure ment inaccurate Replace burst disks more fre quently Check turntable func...

Page 128: ... If you are located outside of the U S call your local PerkinElmer sales or service office Please provide your unit s serial number with all repair questions or repair orders The serial number is located on the nameplate ...

Page 129: ... use is normal and will not affect its function for a bulge larger than 2mm it is recommend to replace the rupture disc TFM Seal Inspection and Replacement A bulge in the center of the TFM seal after use is normal and will not affect its function for a bulge larger than 2mm it is recommend to replace the seal ...

Page 130: ...irectly into the weighing cups made from TFM These are placed in the digestion vessel with the sample and remain there during digestion Since the TFM cups exhibit practically no memory effects the cleaning process is the same as in the case of the digestion vessels Volume 2 0 ml 2 5 ml External Diameter 15 ml 20 ml ...

Page 131: ...h 2 540 cm Volume 1 ml 0 06102 inch 2 642 10 4 gallon 1 inch3 16 387 ml 43 29 10 4 gallon 1 gallon 3785 ml 231 inch3 Pressure 1 bar 4 504 psi 0 1 Mpa 1 psi 0 06895 bar 0 0068948 Mpa 1 Mpa 10 bar 145 04 psi Weight 1 kg 2 2046 lb 1 lb 0 4536 kg Login page 122 Home page 124 Method page 125 Data page 128 Start page 131 Setup page 143 ...

Page 132: ...122 Appendix Login Login 1 Select the login access desired ...

Page 133: ...123 Index of Controller Screens Login Passcode 1 Enter the login passcode ...

Page 134: ...tes screen Data Takes the user to the Select Review Datafile screen Start Takes the user to the Digestion Comment screen Setup Access the Admin setup menu Service For authorized PerkinElmer Service Engineers only Login Return to the login screen OPEN open the Titan MPS lid ...

Page 135: ...e highlighted method favorite and returns to the Home screen Replace Opens the methods library Selecting a library method replaces the favorite method Edit Edit the highlighted favorite Admin only Pressure Adjust Selects the DPC pressure calibration process Caution Saving any edits permanently replaces the edited method ...

Page 136: ...e Favorite Method Library 1 Highlight a method by pressing on it Select Replace the favorite with the highlighted method and return to the Favorites screen Cancel Discard any selections and return to the Favorites screen ...

Page 137: ... Select any field for entry by pressing on it Save Save changes to the current method and return to the Favorites screen Cancel Discard any changes and return to the Favorites screen Caution Saving any edits permanently replaces the edited method ...

Page 138: ...lect Selects the highlighted datafile and returns to the Home screen View Digestion Reviews the digestion data from the highlighted datafile and file index Back Discard selections and return to the Home screen File Index Increment or de increment the file index of the digestions within the datafile File Manager Access the file export and deletion screen Admin only ...

Page 139: ...ile by pressing on it View Digestion Reviews the digestion data from the highlighted datafile Back Discard selections and return to the Select Review Datafile screen Delete All Deletes all datafiles confirmation required Export Data Accesses the USB data export screen ...

Page 140: ...130 Appendix Export Data USB Erase USB Erases the connected USB stick Copy all to USB Copies datafiles to the USB stick Back Returns to the File management screen ...

Page 141: ...eens Start Digestion Comment 1 Press the comment field to enter information Sample Details Go to the Sample Details screen to enter sample specific information Next Go to the Digestion Review screen Back Return to the Home screen ...

Page 142: ...2 Appendix Sample Details 1 8 1 Highlight a field to enter information for that sample Next Go to the next Sample Details page if using 16 vessel configuration Back Return to the Digestion Comment screen ...

Page 143: ...133 Index of Controller Screens Sample Details 9 16 1 Highlight a field to enter information for that sample Done Return to the Digestion Comment screen Back Return to the Sample Details 1 8 screen ...

Page 144: ...t The method is not permanently changed but the datafile will record the altered method for future review Vessels Select this button to enter the number of samples vessels to be digested Store to Datafile Takes the user to the Datafile Select Rename screen Pressure Turn on off the pressure regulation of the method program Back Returns to the Digestion Comment screen Start Begin the digestion ...

Page 145: ...y Reset Reset the digestion index of the all datafiles and overwrite previous data Admin only Rename Press in this field to rename the currently highlighted datafile Save Save the name of the highlighted datafile if not saved the file name reverts when the user leaves this screen Cancel Discard any changes except a saved name change and return to the Digestion Review screen Select Select the curre...

Page 146: ...he currently stored pressure calibrations Select the appropriate calibration cap to continue the digestion Back Use this button to return to the Review Digestion screen Start This button will start the digestion if a pressure calibration is selected ...

Page 147: ... a graph of the pressure in the reference vessel The bottom chart displays a bar chart of each individual vessels current temperature Each vessel bar can be pressed which will then change the display to show the data for that vessel only Select another vessel or return to the default display by pressing on max next to the vessel numbers Stop Use this button to halt a digestion ...

Page 148: ...138 Appendix Digestion Complete 1 Press the Digestion Comment field to edit the current comment Review Digestion Review the current digestion data Finish Return to the Home screen ...

Page 149: ...139 Index of Controller Screens Digestion Graph Back Returns to the Digestion Complete screen Next Go to the Review Method screen ...

Page 150: ...140 Appendix Review Method Back Return to the Digestion Graph screen Next Go to the Review Sample Details 1 8 screen ...

Page 151: ...141 Index of Controller Screens Review Sample Details 1 8 Back Return to the Review Method screen Next Go to the Review Sample Details 9 16 screen ...

Page 152: ...142 Appendix Review Sample Details 9 16 Back Return to the Review Sample Details 1 8 screen Exit Return to the Home screen ...

Page 153: ...143 Index of Controller Screens Setup Setup 1 10 1 Select the operating language by pressing the appropriate button Set time set the system time Back return to the Home screen Next Go to Setup 11 20 ...

Page 154: ...in set bar Global pressure min Power max set Global max microwave power Power min set Global min microwave power Standard favorite Favorite selected by default on bootup User management 1 on 0 off no passcode required Set by button Pressure measuring Global pressure control 1 on 0 off Set by button Max digestion time Global max digestion time ...

Page 155: ...n Admin login code Set the passcode for admin login default 0 User login code Set the passcode for user login default 0 File overflow warning Number of total digestions stored before the system gives a capacity warning Time count up down 1 0 Set time during a digestion to display counting up 1 or counting down 0 ...

Page 156: ...146 Appendix ...

Page 157: ...Datafile Rename 135 Datafile Select 135 Datafiles renaming 81 selecting 79 Decontamination 20 Digestion 53 131 complete 138 graph 139 information 63 method 60 starting 67 vessels 60 Digestion Comment 131 Digestion Complete 138 Digestion Edit 134 Digestion Procedure 59 Digestion Review 134 Digestions reviewing 85 Dimensions 25 Display maintenance 102 DPC Cap maintenance 103 Drop Lid 8 E Edit Method...

Page 158: ...in Passcode 123 Login Screen 122 M Main Window system description 32 Method creating 77 editing 74 Method Library 126 Method Preparation 53 Method Screen 125 Microwave Device Troubleshooting 114 Microwave Oven 114 specifications 37 Microwave Radiation 26 O Output Power Measurement 108 Oven Chamber maintenance 102 Over Temperature Protection safety practices 9 P Partial Digestion maintenance 103 PF...

Page 159: ...3 Setup 11 20 145 Setup Screen 143 Specifications 37 control unit 38 microwave oven 37 pressure vessels 38 Standard 75mL Vessels 34 Start Screen 131 T Temperature Control safety practices 9 Temperature Monitoring system description 33 TFM Seal inspection 119 replacement 119 Tubes 102 Turntable Configurations 106 Turntable System maintenance 106 Turntables system description 34 U Unpacking 39 V Ven...

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Page 161: ...PerkinElmer Inc 710 Bridgeport Avenue Shelton CT 06484 4794 U S A Internet http www perkinelmer com email info perkinelmer com PerkinElmer is a registered trademark of PerkinElmer Inc ...

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