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21

Perform a Digestion

 

CAUTION

 

If resistance is felt when trying to insert probe, ensure that the thermowell is not broken inside the Teflon 
cover. The sharp edges of any break can restrict the movement of the probe.  
 
The "MTS-300 High Temp" (P/N 281461) Fiber Optic probe is required for applications running 250 ºC or 
greater in temperature.

2. 

Load the remaining vessel assemblies into the turntable one by one, ensuring that the notch in the bottom 
rear of the frame engages the locking ring on the turntable. See “Vessel Distribution” section of this manual 
for optimal vessel distribution. 

3. 

Ensure that the notch in the bottom of the frame engages the locking ring on the turntable. 

Содержание EasyPrep

Страница 1: ...EasyPrep Series High Performance Vessels Manual ...

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Страница 3: ...ditioning 13 Non Nitric Acid Liner and Cover Conditioning 14 Perform a Digestion Vessel Assembly 15 Turntable Setup 20 Load and Perform a Method 24 Vessel Removal 25 Vessel Cleaning Liner 27 Liner Bake out Procedure 27 Covers 28 Sleeves 28 Turntable Frame Load Disc Screw 28 Vessel Distribution Even Vessel Distribution 29 Methods One Touch Method Creation 30 Classic Method Creation 30 Fiber Optic T...

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Страница 5: ...bservation or action as described below NOTE A NOTE is intended to provide emphasis of procedures that may be misinterpreted or overlooked or to otherwise clarify confusing situations CAUTION A CAUTION is intended to provide essential information and to emphasize procedures which if not strictly followed may result in improper instrument operation WARNING A WARNING is intended to emphasize dangero...

Страница 6: ... is intended for use by both novice and experienced users for the operation and maintenance of the vessel Additional information including but not limited to training notes and videos application notes software updates and parts can be viewed on CEM s website at https cem com CEM recommends updating the MARS 6 and MARS 6 iWave system to software version 1 49 or greater Contact CEM Corporation for ...

Страница 7: ...C 310 ºC 310 ºC Nitric Acid 230 ºC 230 ºC 230 ºC Hydrochloric Acid 230 ºC 230 ºC 230 ºC Hydrofluoric Acid 210 ºC 210 ºC 210 ºC Sulfuric Acid 300 ºC 300 ºC 300 ºC Phosphoric Acid 300 ºC 300 ºC 300 ºC Aqua Regia 230 ºC 230 ºC 230 ºC Water 200 ºC 200 ºC 200 ºC Maximum Sample Weight Food Plant and Animal Tissue 1 0 g 1 0 g 1 0 g Oil and Plastic 0 25 g 0 25 g 0 25 g Pharmaceutical 1 0 g 1 0 g 1 0 g Ino...

Страница 8: ... the cavity Microwave Safeguards Always use the TempGuard feature in the method for software versions 1 48 TempGuard is preset and non adjustable in version 1 49 or greater Set the TempGuard limit at 30 C control temperature if control temperature is 230 C Set the TempGuard limit at 20 C control temperature if control temperature is 230 C Limit TempGuard to 250 C for digestion of organics with HNO...

Страница 9: ... may become nitrated and potentially explosive Absence of a particular chemical compound from this list does not imply microwave acid decomposition of such a sample is safe under all conditions Explosives TNT Nitrocellulose etc Propellants Hydrazine Ammonium Perchlorate etc Pyrophoric chemicals Hypergolic mixtures Nitric Acid and Phenol Nitric Acid and Triethylamine Nitric Acid and Acetone etc Ani...

Страница 10: ...ons using primarily HNO3 HF H2 SO4 and H3 PO4 The Titanium metal ring is recommended for non HF applications where HCl and aqua regia are heavily used WARNING Only use consumables accessories vessels and vessel components purchased directly from CEM or through its authorized dealer network The use of consumables accessories vessels and vessel components other than original CEM parts will put opera...

Страница 11: ...r Vessel Liner Standard Cover Premium Cover P N 432175 P N 131125 P N 131126 Contains acid and sample 110 mL Liner 5 30 mL working volume Seals liner to contain acid and sample Seals liner to contain acid and sample Recommended for use with HCl Frame Screw EasyPrep iWave Turntable P N 144996 P N 404305 Uniformly provides pressure seal among vessels when torqued Holds assembled vessels inside MARS ...

Страница 12: ...sc Temperature Control Load Disc Vessel Liner P N 131130 P N 131165 P N 432175 Evenly distributes load from cover Fiber Optic Temperature Control Evenly distributes load from cover Contains acid and sample 110 mL Liner 5 30 mL working volume Standard Cover Premium Standard Cover Control Cover T only P N 131125 P N 131126 P N 131195 Seals liner to contain acid and sample Seals liner to contain acid...

Страница 13: ...ntain acid and sample Recommended for use with HCl Frame Screw Control Frame Screw Pressure Nut P N 144996 P N 144995 P N 431311 Uniformly provides pressure seal among vessels when torqued Fiber Optic Temperature Control Uniformly provides pressure seal among vessels when torqued Seals Pressure connector when ESP 1500 not in use Sapphire Thermowell Thermowell Nut EasyPrep and EasyPrep Plus Turntab...

Страница 14: ...ntrol Supports sleeve load disc vessel liner cover and screw Sleeve Load Disc Temperature Control Load Disc P N 431740 P N 131130 P N 131165 Supports vessel liner Evenly distributes load from cover Fiber Optic Temperature Control Vessel Evenly distributes load from cover Vessel Liner Standard Cover Premium Standard Cover P N 432175 P N 131125 P N 131126 Contains acid and sample 110 mL Liner 6 30 m...

Страница 15: ...commended for use with HCl Premium Control Cover T P Frame Screw Control Frame Screw P N 131206 P N 144996 P N 144995 Fiber Optic Temperature and pressure control Seals liner to contain acid and sample Recommended for use with HCl Uniformly provides pressure seal among vessels when torqued Fiber Optic Temperature Control Uniformly provides pressure seal among vessels when torqued Pressure Nut Easy...

Страница 16: ...l Vessel Loosening Wrench Torque Stand P N 514140 P N 430660 P N 144925 Provides appropriate vessel seal 84 inches per pound 7 ft lbs Removes frame screw Holds Vessels in place while torquing Vessel Liner Holder P N 166222 Holds up to a set of 16 vessel liners ...

Страница 17: ... appropriate sample into each liner Never add sample or liquid to liner with sleeve in place The liner containing the highest amount of weighed sample will be the control vessel 3 Add 10 mL of HNO3 to each liner Use the acid to rinse the inside of the liner to ensure that the sample is in the base of the liner 4 Wait 15 minutes to allow pre digestion 5 Assemble and torque each vessel See Vessel As...

Страница 18: ...oad for water is 50 mL so more than one vessel is required 4 Wait 15 minutes to allow pre digestion 5 Assemble and torque each vessel See Vessel Assembly for detailed instructions 6 Select and load the Easy Prep Clean method from the One Touch directory 7 Place vessels on turntable and insert the turntable into the cavity See Turntable Setup and Vessel Distribu tion for detailed instructions 8 Clo...

Страница 19: ... liner holder 4 Add sample to the liner s WARNING Proper precautions must be taken to avoid contact with acids or acid vapors Protective gear should be worn as outlined in the user s safety program for hazardous materials and the acid manufacturer s safety data sheet Refer to these guidelines for proper handling and disposal of the acids 4 1 Inspect liners for abnormalities 4 2 Weigh and transfer ...

Страница 20: ...asy Prep Plus Control Cover 6 1 Insert the open end of the thermowell into the control cover until it stops CAUTION Do not force thermowell into control cover as it is fragile and may break 6 2 Slide the nut onto the thermowell and tighten the nut until finger tight 7 Place the cover on the liner If a control vessel is required use the liner containing the highest amount of weighed sample as the c...

Страница 21: ...rmity of the liner and sleeves 9 Place the load disc on the cover with the tab on the disc facing downward so that it fits into the center notch of the cover The fiber optic temperature control cover requires the load disc with a hole in the center 10 Position the sleeve into the correct frame ...

Страница 22: ...ire the shorter frame If the cover has pressure control select the Easy Prep Plus control frame and position the pressure connector so it passes through the frame and aligns toward the outside of the frame 11 Verify vertical placement by ensuring the sleeve is aligned on the disc at the bottom of the frame 12 Tighten the screw onto the top of the load disc until it is finger tight ...

Страница 23: ...nnector is not touching the frame before or after torquing 14 3 Use the provided torque wrench and tighten the screw until a single click is heard or felt The EasyPrep vessel series requires a torque setting of 84 in lbs 7 ft lbs WARNING Vessel torquing is critical to optimize controlled venting of the system and for the integrity of the vessel Over or under torquing may lead to sealing issues If ...

Страница 24: ...1500 pressure option is not available tighten the nut until finger tight 1 2 If the control vessel has fiber optic temperature control insert the fiber optic probe into the control vessel The fiber optic probe should slide easily into the thermowell through the frame screw and load disc until the probe reaches the bottom of the thermowell Do not force the fiber optic probe If probe cannot be easil...

Страница 25: ...P N 281461 Fiber Optic probe is required for applications running 250 ºC or greater in temperature 2 Load the remaining vessel assemblies into the turntable one by one ensuring that the notch in the bottom rear of the frame engages the locking ring on the turntable See Vessel Distribution section of this manual for optimal vessel distribution 3 Ensure that the notch in the bottom of the frame enga...

Страница 26: ... mat positioning ensuring that the mat is not covering the temperature sensors 5 Load the turntable into the instrument by aligning the Control Vessel or position 1 with the front of the instru ment Ensure turntable is seated down on drive lug ...

Страница 27: ...right side of the instru ment cavity facing instrument by rotating the pressure sensor and gently pushing it into the connec tor port until it slips locks into the correct position 6 3 Secure the pressure line into the ceiling clip 7 If applicable connect the fiber optic probe to the port in the top center of the MARS 6 cavity by pushing in the plug until it snaps into place 8 With the door open u...

Страница 28: ... to the Home page 3 Select load the method from the directory One Touch or Classic See Methods section or contact CEM Cor poration if assistance is needed creating a new method 4 Close the instrument door 5 Select Start to run the method The instrument will begin the method according to the selected parameters initializing ramping holding cooling etc 5 1 Verify that vessel count type and position ...

Страница 29: ...able keeping the vent holes pointed away from the user at all times and place into a fume hood 5 If applicable remove the fiber optic probe from the control vessel 6 Remove the vessel assemblies from the turntable one by one keeping the vent hole pointed away from the user 7 With the vent hole pointed away from the user use the vessel loosening wrench to slowly and carefully loosen the vessel scre...

Страница 30: ...13 Transfer the sample from liner and proceed with work up CAUTION Never pour sample or liquid from liner with sleeve in place 14 Inspect vessel components and replace worn or damged parts 15 Clean vessels as outlined in Vessel Cleaning section ...

Страница 31: ...ed for sample digestion HNO3 HCl H2 SO4 H3 PO4 or HF 4 2 Prepare vessel and turntable as outlined in manual 4 3 Select and run the Easy Prep Clean method in the One Touch directory 4 4 Wait for vessels to cool for a minimum of 15 minutes before opening microwave door 4 5 Discard acid and rinse the liners and covers with deionized water Liner Bake out Procedure As needed The bake out procedure can ...

Страница 32: ...covers with deionized water and allow to dry completely before use Shake covers to remove liquid that might be trapped between the cover and ring Sleeves 1 If water or acid gets on a sleeve wipe it off with a damp paper towel and allow to dry Never soak sleeves CAUTION Never soak sleeves in water or detergent Remove composite sleeves before adding acid to vessel liners or before pouring digested s...

Страница 33: ...el distribution is required for optimal performance Proper spacing will eliminate hot spots issues regarding turntable balance and provide optimal temperature sensing 2 vessels 3 vessels 4 vessels 5 vessels 6 vessels 7 vessels 8 vessels 9 vessels 11 vessels 12 vessels 10 vessels ...

Страница 34: ... Contact CEM before selecting any other sample types 6 Select Hold Time and enter in the appropriate hold time 7 For software versions 1 49 or greater proceed with step 8 For software versions 1 48 or lower enable Temp Guard as outlined below Always use TempGuard Set the TempGuard limit at 30 C control temperature if control temperature is 230 C Set the TempGuard limit at 20 C control temperature ...

Страница 35: ...GF value as outlined below 1 Connect the fiber optic probe to the port in the top center of the MARS 6 cavity by pushing in the plug until it snaps into place 2 Select the System Settings icon in the bottom right corner of the screen 3 Select Settings 4 Select Sensors 5 Select the current GF Number 6 Using the Keyboard enter the GF Number on the Fiber Optic Probe installed in the instrument The GF...

Страница 36: ...ture If the fiber optic probe is new or the temperature is not reading correctly enter the GF number See the Fiber Optic section of the manual for details If appears as the temperature then the MARS 6 does not recognize the Fiber Optic Probe The probe is either not installed or is not working properly See the Fiber Optic section of the manual for details 5 The probe can also be inserted into a bea...

Страница 37: ...evice Daily If installed remove the ESP 1500 cable connection from the connector port and thoroughly clean the connector with a paper towel or soft cloth Thoroughly wipe and clean both the inside and outside surfaces of the connector If necessary dampen the towel with isopropyl alcohol to assist in cleaning Weekly Inspect Vessel Components See Vessel Inspection section of this manual for acceptabl...

Страница 38: ...Sample Preparation Safeguards for specific details when running acid blanks Liner not getting as hot due to leaking Inspect vessel components and replace worn or damged parts Max Power Monitor message appears during run Vessels leaking Vessels possibly not assembled properly or not torqued using torque tool Turntable not aligned Perform turntable calibration as outlined in the MARS Manual Corrosio...

Страница 39: ... liner and sleeve Alligator skin on outside of liner Result of high heat pressure May be ok to run but will need to be grouped with like vessels Liner and or Sleeve distorted flared or frayed Discard See Vessel assembly for preventative measures Sleeve has turned white no longer golden brown and or stained on ends Replace sleeve To prevent sleeve damage avoid high temperatures for long periods of ...

Страница 40: ...itting Technology LET that accurately measures the temperature of the actual sample not the outer surface of the vessel One Touch Methods created by CEM Applications Specialists Determines all of the parameters adjusts power output and performs the digestion for all major sample types MAXPower Aborts the run if full programmed power is applied continuously over a specified period of time ReactiGua...

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