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Dionex ASE 150, Operator'S Manual

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ASE 150 Operator’s Manual

22

Doc. 065207-02 9/08

OPP (Organophosphorous Pesticides) Method Parameters

Solvent

MeCl

2

/Acetone (1:1, v/v)

Temperature

100 

°

C 

Static Time

5 min

Rinse Volume

60% 

Purge Time

100 sec

Static Cycle

1

Cell Type

Stainless steel

PCB (Polychlorinated Biphenyls) Method Parameters

Solvent

Hexane

Temperature

100 

°

C 

Static Time

5 min

Rinse Volume

60% 

Purge Time

100 sec

Static Cycle

1

Cell Type

Stainless steel

PDF (Dioxins and Furans) Method Parameters

Solvent

Toluene

Temperature

200 

°

C 

Static Time

5 min

Rinse Volume

60% 

Purge Time

100 sec

Static Cycle

1

Cell Type

Stainless steel

Summary of Contents for ASE 150

Page 1: ...ASE 150 Accelerated Solvent Extractor Operator s Manual Document No 065207 Revision 02 September 2008...

Page 2: ...IED REPRESENTATIONS REGARDING THE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT...

Page 3: ...and Regulatory Information 5 1 4 Safety Labels 5 2 Description 2 1 Operating Features 7 2 1 1 Control Panel 9 2 1 2 Sample Cells and Rinse Cells 11 2 1 3 Collection Vessels 13 2 1 4 Solvent Reservoir...

Page 4: ...Installing the Waste Bottle 41 3 2 Running 42 3 2 1 Selecting the Method 42 3 2 2 Selecting the Cell Size 42 3 2 3 Verifying the Cell Type 43 3 2 4 Starting the Run and Checking the Oven Status 43 3 2...

Page 5: ...4 Stopped System 67 5 Service 5 1 Replacing Tubing and Fittings 69 5 2 Replacing the Cell End Cap Seal 69 5 3 Replacing the Cell End Cap O Ring 72 5 4 Removing the Right Side Panel 73 5 5 Replacing P...

Page 6: ...eting the Procedure 83 5 7 Replacing the Pressure Relief Valve 84 5 8 Rebuilding the Static Valve 86 5 8 1 Removing the Static Valve from the System 88 5 8 2 Disassembling the Static Valve Body 90 5 8...

Page 7: ...n Hose 110 B 2 3 Checking the Oven Voltage Switches 110 B 2 4 Connecting the Power Cord 111 B 2 5 Checking Pressure Readings 112 B 2 6 Connecting the Solvent Reservoir 113 B 2 7 Installing the Waste B...

Page 8: ...3 C 2 4 Hydrocarbon Sensor Screen 134 C 2 5 Extraction Counters Screen 135 C 2 6 Moduleware Screen 136 D Reordering Information 137 E Theory of ASE 141 E 1 Introduction 141 E 2 Operation 143 E 3 Metho...

Page 9: ...and small amounts of mineral acids The ASE 150 accelerates the traditional extraction process by using solvent at elevated temperatures and pressures Pressure is maintained in the sample cell to main...

Page 10: ...ake you to other locations within the file These links include Table of contents entries Index entries Cross references underlined in blue to sections figures tables etc If you are not familiar with h...

Page 11: ...the ASE 150 Appendix E Theory of ASE Describes the theory behind performing extractions with ASE Indicates an imminently hazardous situation which if not avoided will result in death or serious injur...

Page 12: ...ituation de danger potentiel qui si elle n est pas vit e pourrait entra ner des blessures mineures mod r es galement utilis pour signaler une situation ou une pratique qui pourrait gravement endommage...

Page 13: ...ding appropriate usage contact Dionex before proceeding In the U S call 1 800 346 6390 and select the Technical Support option Outside the U S call the nearest Dionex office 1 4 Safety Labels The cTUV...

Page 14: ...50 Operator s Manual 6 Doc 065207 02 9 08 Power supply is on Power supply is off Hot surface Indicates a potential hazard Refer to the operator s manual for an explanation of the hazard and how to pro...

Page 15: ...n operating features of the ASE 150 Accelerated Solvent Extractor Figure 2 1 ASE 150 Operating Features 1 Solvent Reservoir Control Panel 2 Door OPEN Lever 4 5 6 3 1 2 Oven Sample Cell Waste Bottle Co...

Page 16: ...n Control Panel The ASE 150 control panel includes a display screen and a membrane keypad which are used to control ASE 150 operation Waste Bottle The waste bottle is a 250 mL collection bottle that i...

Page 17: ...doors must be closed for safe operation 2 1 1 Control Panel Use the control panel screen and buttons to control ASE 150 operation The screen displays status and operating information You can edit any...

Page 18: ...and displays the ABORT screen Pressing the button lights the LED The LED turns off when you select an option on the ABORT screen See Section 3 4 for details Exits the screen currently displayed and re...

Page 19: ...other high temperature applications Moves the cursor in the direction of the arrow to the next selectable line on the display if any When the cursor is in an editable field pressing an arrow button di...

Page 20: ...cell in a different size than the size originally ordered order the cells from Dionex You will also need to order the Startup Kit appropriate for the new cell size For cell and Startup Kit part numbe...

Page 21: ...mL clear graduated bottle Class B 068249 1 Before each run carefully inspect all collection vessels for chips scratches or cracks If a collection vessel shows any sign of damage do not use it Use eac...

Page 22: ...150 Ship Kit P N 066399 provides vent tubing P N 053514 that you can connect to the vent outlet on the rear panel see Figure 2 3 and then route to a vent hood NOTE Check the waste bottle daily and em...

Page 23: ...s see Section B 2 3 The model data label lists fuse and power information as well as the ASE 150 serial number You will be asked to provide the serial number when ordering replacement parts for the sy...

Page 24: ...teps are required before the ASE 150 can perform an extraction Refer to Chapter 3 for detailed instructions for each step Fill the solvent reservoir Prepare the sample and load it into the sample cell...

Page 25: ...erature in the cell is heated to the set point specified in the method 3 Static extraction the cell remains filled with the solvent at the temperature set point Figure 2 4 Extraction Process Schematic...

Page 26: ...splays the following status states in the order given Oven Wait Oven Ready Load Preheat optional Fill Heat Static Rinse Purge Relief Unload and Idle METHOD the name or number of the current method VOL...

Page 27: ...RGE TIME the amount of time the cell is purged with nitrogen STATIC CYCLE the number of times the static extraction and rinse cycles are performed CELL TYPE the type of cell to use stainless steel or...

Page 28: ...tions for each preprogrammed method You cannot edit or delete a preprogrammed method Preprogrammed Method Method Name Semivolatiles BNA Total Fat crude FAT Chlorinated Herbicides HRB Organochlorine Pe...

Page 29: ...ess steel HRB Chlorinated Herbicides Method Parameters Solvent MeCl2 Acetone 1 1 with 1 H3PO4 Temperature 100 C Static Time 5 min Rinse Volume 60 Purge Time 100 sec Static Cycle 1 Cell Type Stainless...

Page 30: ...100 sec Static Cycle 1 Cell Type Stainless steel PCB Polychlorinated Biphenyls Method Parameters Solvent Hexane Temperature 100 C Static Time 5 min Rinse Volume 60 Purge Time 100 sec Static Cycle 1 Ce...

Page 31: ...Alcohol Temperature 140 C Static Time 3 min Rinse Volume 100 Purge Time 60 sec Static Cycle 3 Cell Type Stainless steel TPH Total Petroleum Hydrocarbons Method Parameters Solvent MeCl2 Acetone 1 1 v v...

Page 32: ...ASE 150 Operator s Manual 24 Doc 065207 02 9 08...

Page 33: ...leau ci dessous liste quelques solvants qui ne doivent pas tre utilis s avec l ASE 150 Contactez Dionex si vous avez un doute concernant l usage d un solvant absent de la liste Solvants ne pas utilise...

Page 34: ...ath are more resistant to acids and bases at elevated temperatures than other metallic materials follow these guidelines to prevent degradation and ensure optimum performance a As a general rule stron...

Page 35: ...extraction f Table 3 1 lists the allowable concentrations for several acids and bases If a sample needs to be treated with acids stronger than the concentrations here pretreat the sample with the con...

Page 36: ...ric acid 5 Yes Yes Yes If acids bases salts or buffers are used as extraction solvents rinse the system with 100 polar organic solvent for example acetone or methanol or distilled water before turning...

Page 37: ...screw the solvent line fitting into the solvent connector on the ASE 150 and then push the gas line fitting into the gas connector Use only Dionex solvent reservoirs These are glass bottles with a pl...

Page 38: ...line to the solvent connector first and then the gas line to the gas connector If you need to disconnect the lines reverse the order It is not necessary to disconnect the solvent and gas lines before...

Page 39: ...sulfate is readily available it should not be used in ASE 150 cells The use of sodium sulfate with very wet samples 30 moisture will result in clogging of system components such as the solvent line or...

Page 40: ...o not use a stainless steel cell Use this ratio of acid to ASE Prep CR whenever using strong acids for pretreatment of samples If you have any questions about compatibility of an acid or base please c...

Page 41: ...ent samples usually do not need to be ground but it may be necessary to remove stones or sticks from the samples prior to extraction Polymer samples must be in a ground state for an efficient extracti...

Page 42: ...ltration or may interfere with the analytical technique Cell filters are available in two sizes Use 27 mm filters for 1 mL 5 mL 10 mL or 22 mL cells Use 30 mm filters for 34 mL 66 mL or 100 mL cells E...

Page 43: ...d bottom designate the end of the cell with the groove around the body and the Dionex logo and serial number as the cell top see Figure 3 4 Figure 3 4 Sample Cell Top Larger Cells 2 Follow the steps i...

Page 44: ...The photos in Figure 3 5 show a zirconium cell Figure 3 5 Installing a 30 mm Cell Filter in a 34 66 or 100 mL Cell Insert a 30 mm filter into the cell at a slight angle Position the filter insertion t...

Page 45: ...top of the sample cell To accommodate different sample cell sizes three funnels with different inner diameters are available see Figure 3 6 2 Optional To reduce the amount of solvent used during the r...

Page 46: ...it If a white Teflon O ring is discolored replace it see the following instructions Figure 3 8 Installing a Cell End Cap O Ring To replace a cell end cap O ring 1 Locate the small flathead screwdriver...

Page 47: ...he acceptable locations for this information Figure 3 9 Acceptable Locations for Collection Vessel Labels Before each run carefully inspect all collection vessels for chips scratches or cracks If a co...

Page 48: ...3 Toggle the needle switch to the DOWN position and close the door Untersuchen Sie vor jedem Lauf alle Sammelgef e auf Abplatzungen Kratzer oder Risse Wenn ein Sammelgef eine Besch digung aufweist sol...

Page 49: ...nd position it below the built in bottle cap 3 While being careful not to bend the tubing that extends from the bottle cap insert the bottle into the bottle cap 4 Tilt the cap and bottle toward you an...

Page 50: ...efer to Section 2 5 5 When the method required for the run is displayed press ENTER 3 2 2 Selecting the Cell Size The ASE 150 determines various internal operating parameters for example the rinse vol...

Page 51: ...Run and Checking the Oven Status 1 On the MENU screen move the cursor to STATUS and press ENTER The STATUS screen see Section C 1 2 appears 2 Press START and then observe the STATUS field If the STAT...

Page 52: ...ell door 2 While holding the cell at a slight angle position the bottom end cap under the bottom latch of the cell holder 3 Raise the cell so that the bottom end cap lifts the bottom latch 4 Straighte...

Page 53: ...3 3 for post run procedures 6 Put on the thermal gloves P N 060372 provided in the ASE 150 Ship Kit P N 066399 7 Remove the cell from the cell holder and place it on the cell rack P N 059927 to cool...

Page 54: ...The composition of the extracts generated by the ASE 150 is very close to that generated by Soxhlet and other standard solid liquid extraction techniques when using the same solvent Use the same anal...

Page 55: ...in diagnostics and sensors that continuously monitor the system Under certain conditions for example if the collection vessel becomes too full or if the hydrocarbon vapor level exceeds the upper limi...

Page 56: ...1 Rinse cells are similar to sample cells but they are blue in color Check that the rinse cell size is matched to the sample cell size 2 Install the rinse cell in the cell holder Rinse cells are inst...

Page 57: ...itable for a particular extraction edit one of the custom methods provided with the ASE 150 Before beginning review the method development guidelines in Section 3 7 and the range of values allowed for...

Page 58: ...a 34 mL cell 160 to 200 seconds for a 66 mL cell 250 to 290 seconds for a 100 mL cell 20 to 900 sec default 100 STATIC CYCLE Number of times the static heating and rinsing steps are performed When mo...

Page 59: ...o edit the method a Press an arrow button to move the cursor to the first parameter that you want to change for example TEMPERATURE b Press ENTER The cursor moves to the editing field NOTE If you deci...

Page 60: ...see Section 3 6 4 Run the new method three times with the same cell and sample into three separate collection vessels and analyze the extracts 5 If target analytes are present in extract 2 or 3 make...

Page 61: ...o balance the number of static cycles and the rinse volume to prevent the collection bottle from being overfilled 6 If analytes still appear in the extract from the second extract make the adjustments...

Page 62: ...e it from the holder dispose of the liquid and reinstall the tray 3 8 2 Periodic Maintenance NOTE The EXTRACTION COUNTERS screen indicates the number of extractions the ASE 150 has performed see Secti...

Page 63: ...nance is performed The solvent lines must be replaced by a qualified Dionex representative 3 9 Shutting Down Overnight or Longer Shutdowns If acids bases salts or buffers are used as extraction solven...

Page 64: ...ASE 150 Operator s Manual 56 Doc 065207 02 9 08...

Page 65: ...ne of these problems occurs an error message is displayed on the screen The message remains until you press any button to clear it or until another error message appears Each error message is identifi...

Page 66: ...temperature low Cause The heater cable connection to the power supply is loose or a heater component malfunctioned Action Contact Dionex for assistance Error 004 Oven temperature high Cause The heater...

Page 67: ...collection vessel Action If solvent leaks into the collection vessel during the static cycle the static valve seals are worn Rebuild the static valve see Section 5 8 Action If the error message reapp...

Page 68: ...ings and solvent line fittings Use a 1 4 inch open end wrench P N 049452 to tighten any leaking fittings Do not overtighten If tightening does not stop a leak the tubing and fitting assembly must be r...

Page 69: ...tion Remove the right side panel of the ASE 150 see Section 5 4 Inspect the following fittings for leaks see Figure 4 1 pump fittings pump check valves pressure transducer fittings pressure relief val...

Page 70: ...s between 100 and 120 Vac or 220 for voltages between 220 and 240 Vac For details see Section B 2 3 Cause The heater cable connection to the power supply is loose or a heater component malfunctioned A...

Page 71: ...check valves pressure transducer fittings pressure relief valve fittings static valve fittings and solvent line fittings Use a 1 4 inch open end wrench P N 049452 to tighten any leaking fittings Do no...

Page 72: ...rear panel Action Set both oven voltage switches to match the voltage from the power source at the installation site either 110 for voltages between 100 and 120 Vac or 220 for voltages between 220 and...

Page 73: ...heck valves pressure Error 023 Top plate heater malfunction Cause Incorrect settings of the oven voltage switches on the ASE 150 rear panel Action Set both oven voltage switches to match the voltage f...

Page 74: ...op a leak the tubing and fitting assembly must be replaced Contact Dionex for assistance If the pump head is leaking replace the pump seals see Section 5 6 Figure 4 1 ASE 150 Plumbing Diagram Pressure...

Page 75: ...3 Gas Leaks Gas leaks are usually audible In addition excessive gas consumption often indicates a gas leak If you suspect a leak check the following locations gas supply rear panel solvent reservoir...

Page 76: ...ASE 150 Operator s Manual 68 Doc 065207 02 9 08...

Page 77: ...tighten If tightening a fitting does not stop a leak the tubing and fitting assembly must be replaced Contact Dionex for assistance 5 2 Replacing the Cell End Cap Seal A worn PEEK seal is deeply groov...

Page 78: ...nless steel and zirconium caps is identical The photos show a stainless steel cap Figure 5 1 Removing the Snap Ring 3 Remove the cap insert see Figure 5 2 Remove the PEEK seal from the groove in the b...

Page 79: ...d cap 7 With the cap assembly upright on the workbench install the snap ring a Insert the snap ring tool into the holes on the ring b Squeeze the tool handles to bring the ends of the ring together c...

Page 80: ...it flat on the workbench 3 Place a new O ring Teflon P N 049457 pkg of 50 Viton P N 056325 pkg of 50 over the opening in the end of the cell end cap Press the O ring into place using the O ring insert...

Page 81: ...e the vessel from the holder and set it aside 3 Turn off the gas supply Disconnect the gas source at the ASE 150 rear panel and let the system vent 4 Turn off the ASE 150 main power switch 5 Unscrew t...

Page 82: ...ht side panel from the system and set it aside Reinstalling the Right Side Panel 1 Hold the panel against the right side of the system Engage the small tabs on the top and bottom of the panel with the...

Page 83: ...in the lower right corner see Figure 5 7 2 Disconnect the red tubing and the transparent blue tubing from the two black elbow press fittings on top of the pump To disconnect a press fitting use your f...

Page 84: ...lve cartridge from the housing see Figure 5 8 2 Turn the pump over so that the outlet check valve is facing down 3 Use a 1 2 inch open end wrench to loosen the outlet check valve housing Remove the ho...

Page 85: ...pump head 2 Install the outlet check valve assembly on the top of the pump head 3 Tighten the check valves fingertight and then use a wrench to tighten an additional one quarter to one third turn 5 5...

Page 86: ...the right press fitting 3 Reconnect the solvent lines to the inlet and outlet check valve housings 4 Reconnect the cable to the pump PC board 5 5 8 Completing the Procedure 1 Follow the instructions o...

Page 87: ...ubing is disconnected 5 6 2 Removing the Pump Follow the instructions in Removing the Pump on page 75 5 6 3 Replacing the Piston High Pressure Seal 1 Use a 3 mm hex driver P N 060154 or wrench to loos...

Page 88: ...e wooden end of a cotton tipped swab and pry out the seal Discard the seal 6 Hold the new high pressure seal P N 066162 with the smaller diameter ringed side of the seal facing down and drop it into t...

Page 89: ...seal properly 8 Reinstall the pump head onto the pump 5 6 4 Replacing the Piston Air Seal 1 Remove the PC board from the side of the pump see Figure 5 13 view A 2 Loosen the two bolts that hold the tw...

Page 90: ...air seal P N 066163 with the closed end facing down into the end plate Gently press the seal into place with a cotton tipped swab or other tool with a soft tip Figure 5 15 Removing the Pump Left End P...

Page 91: ...he pump should sit evenly on the flat surface without rocking 10 Tighten the two bolts evenly 11 Reattach the PC board to the side of the pump 5 6 5 Reinstalling the Pump and Completing the Procedure...

Page 92: ...ting on the valve To disconnect a press fitting use your fingers or a small open end wrench to press the ring on the fitting in while at the same time pulling the tubing out 3 Use a 1 4 inch open end...

Page 93: ...n the old valve by removing the two Phillips screws on the valve 9 Attach the splash guard to the new pressure relief valve P N 048889 10 Lower the new pressure relief valve onto the valve base Tighte...

Page 94: ...068115 each time the valve requires rebuilding Order a Static Valve Tool Kit P N 068116 only the first time the valve requires rebuilding Figure 5 19 illustrates each tool Part Number Item Quantity 0...

Page 95: ...rench 5 8 in open end wrench or socket Large flathead screwdriver Cotton tipped swabs or other tool with a soft tip Isopropyl alcohol IPA or acetone Figure 5 19 Static Valve Tools Piston Side Seal Ins...

Page 96: ...20 3 Using a 1 4 inch open end wrench disconnect the two Hastelloy fluid lines from the valve 4 Disconnect the dark yellow and orange tubing from the press fittings on the valve To disconnect a press...

Page 97: ...ston from the static valve a Locate the slot in the piston holder If necessary rotate the piston holder so that the opening in the slot faces up b Guide the piston out of the piston holder by lifting...

Page 98: ...move the nut on the inlet side of the valve body b Remove the seal backup ring and the filter from the inlet side they may fall out on their own Save the seal backup ring You can discard the filter c...

Page 99: ...ert the pointed end of the seal removal tool into the valve body Slide the tool between the valve body and O ring and pull the O ring out of the valve body 6 Using a cotton tipped swab or other tool w...

Page 100: ...5 Rest your thumbs on the back of the tool and press down firmly with equal pressure on the left and right sides of the tool You should hear a snap as the new seal is seated in the valve body Remove t...

Page 101: ...ling the Static Valve 1 Place the seal backup ring with the flat side facing up on top of the seal in the inlet gland When correctly installed the backup ring completely covers the mounting surface NO...

Page 102: ...f the valve body and tighten with a 5 8 in open end wrench or socket Use another open end wrench to hold the valve body in place while tightening the nut 5 Reinstall the nut on the piston side of the...

Page 103: ...screw them loosely into the valve body to secure the body to the base plate Do not fully tighten the screws yet 9 Slide the spacer tool P N 068118 between the valve body and the piston ferrule 10 Scre...

Page 104: ...ion P N 057395 to connect the piece of orange extension tubing P N 049293 to the end of the line 13 The gas pressure will extend the cylinder shaft fully and hold the spacer tool firmly in place betwe...

Page 105: ...valve Refer to the label on the inside of the right side panel 3 Reconnect the gas source and turn on the gas supply 4 Turn on the ASE 150 main power switch 5 Follow the steps below to test the syste...

Page 106: ...lace while tightening the nut During the static cycle also check the tip of the source needle the needle with the smaller diameter near the front of the needle assembly in the collection vessel If liq...

Page 107: ...d remove the right side panel 3 Use a 2 5 mm hex wrench to remove the two screws on the top of the needle block see Figure 5 22 Figure 5 22 Removing the Needle Block Screws 4 Slide the cover of the ne...

Page 108: ...rear of the needle assembly Figure 5 24 Removing the Source Needle from the Needle Block 6 Use a 1 4 inch open end wrench to disconnect the fitting on the side of the static valve see Figure 5 25 7 R...

Page 109: ...he cover on the needle block and reinstall the screws 11 Connect the free end of the source needle tubing to the side of the static valve 12 Follow the instructions on page 74 to reinstall the right s...

Page 110: ...ays replacing both fuses 4 Insert two new 10 amp IEC127 fast blow fuses P N 954746 into the springs in the fuse drawer Press gently to fully insert the fuses into the drawer Figure 5 27 Fuse Drawer 5...

Page 111: ...of 264 Vac Typical Operating Power 500 W Maximum Operating Power 1000 W Maximum Line Draw 8 A at 110 Vac Oven Power Requirements Two switches set the oven voltage to 110 for power source voltages bet...

Page 112: ...een parameters Stainless Steel Sample Cells Stainless steel cell bodies and end caps with PEEK seals and stainless steel frits Cells are available in the following sizes 1 mL actual volume 1 0 mL 5 mL...

Page 113: ...psi Valves High pressure valves pressure relief and static Low pressure valves purge prime and pneumatics Bottle Sensor When the needles are in the down position sensors detect whether a collection v...

Page 114: ...ASE 150 Operator s Manual 106 Doc 065207 02 9 08...

Page 115: ...se power source of 100 to 240 Vac 50 60 Hz The oven voltage switches must be set to match the voltage from the power source at the installation site 110 for voltages between 100 and 120 Vac or 220 for...

Page 116: ...the blue 4 mm 0 156 in OD tubing P N 049296 into the elbow fitting 3 Push the other end of the tubing into the NITROGEN connector on the ASE 150 rear panel see Figure B 1 ASE 150 Startup Kit Part Numb...

Page 117: ...1 6 Optional Route the free end of the vent tubing to a vent hood Figure B 1 ASE 150 Rear Panel Do not obstruct or pressurize the vent outlet Ne bouchez ni ne mettez sous pression la sortie d a ration...

Page 118: ...at the installation site either 110 for voltages between 100 and 120 Vac or 220 for voltages between 220 and 240 Vac 2 If you need to change an oven voltage switch setting a Verify that the main power...

Page 119: ...on at AC input levels outside of the specified operating voltage range may damage the ASE 150 DANGER D LECTROCUTION Pour viter toute lectrocution il faut utiliser une prise de courant avec prise de te...

Page 120: ...eading does not meet specification contact Dionex Figure B 3 Diagnostics Screen Figure B 4 Regulators Screen Field Function Specification SYSTEM Internal system pressure 0 34 0 02 MPa 50 3 psi COMPRES...

Page 121: ...the bottle Use only Dionex solvent reservoirs These are glass bottles with a plastic shatterproof coating To prevent personal injury make sure the pressure applied to the bottles does not exceed 0 07...

Page 122: ...nnector To disconnect the line push the small latch at the top of the connector toward the center of the connector NOTE Always connect the solvent line to the solvent connector first and then the gas...

Page 123: ...ition it below the built in bottle cap 3 While being careful not to bend the tubing that extends from the bottle cap insert the bottle into the bottle cap 4 Tilt the cap and bottle toward you and scre...

Page 124: ...46253 securing the lower latch to the cell door see Figure B 7 If the ASE 150 has recently finished a run the inside of the cell door will be hot Put on thermal gloves P N 060372 before adjusting the...

Page 125: ...two extra hex screws in case the original screws are misplaced NOTE When the latch is correctly installed the small tab is on the underside of the latch see Figure B 7 Figure B 8 Mounting Sites for t...

Page 126: ...e cursor to the first parameter that you want to change for example CELL SIZE b Press ENTER The cursor moves to the editing field NOTE If you decide not to edit this field press MENU to return the cur...

Page 127: ...open residual pressure is released from the sample cell The default setting OFF is recommended PREHEAT TIME Specifies for how long the oven heats up without solvent 0 to 99 minutes The default setting...

Page 128: ...using the O ring insertion tool P N 049660 Figure B 10 Inspecting Cell O Rings If an O ring is missing install a new one see Figure B 11 If any O ring has a hole size of less than 0 5 mm replace it I...

Page 129: ...2 While holding the cell at a slight angle position the bottom end cap under the bottom latch of the cell holder 3 Raise the cell so that the bottom end cap lifts the bottom latch 4 Straighten the cel...

Page 130: ...pr sence de f lure ou d gratignures sur les flacons de collecte doit tre v rifi e avant chaque extraction N utilisez jamais un flacon endommag Les flacons non gradu s sont usage unique Les flacons gra...

Page 131: ...e the rinse cycle is in progress 6 When the rinse cycle is complete after about 1 minute three beeps are emitted and the RINSE button LED turns off 7 Remove the rinse cell a If the oven is hot put on...

Page 132: ...ASE 150 Operator s Manual 124 Doc 065207 02 9 08...

Page 133: ...lect certain default parameters for the ASE 150 run the methods that control a run and create and edit custom methods Diagnostic screens let you monitor input from sensors monitor pressure settings ad...

Page 134: ...access to the ASE 150 operational and diagnostics screens To display the MENU screen press the MENU button on the front panel To display a screen listed on the MENU 1 Press an up or down arrow button...

Page 135: ...at Heat Oven Wait Oven Ready Static Rinse Purge Relief Unload Rinse or Abort If the status is Static or Rinse the cycle number is indicated METHOD The name or number of the current method VOL The appr...

Page 136: ...ted cell size UNITS Specifies the unit of measure for pressure displays psi MPa bar or atm REDUCE RELIEF Determines whether the pressure relief valve is open for a reduced period ON or the normal peri...

Page 137: ...on and off the beep that sounds when an error occurs Figure C 5 Method Editor Screen All Parameters Shown Parameter Description METHOD Displays the number 1 through 24 or name of the method currently...

Page 138: ...ex recommends the following settings 40 to 80 seconds for a 1 mL 5 mL 10 mL or 22 mL cell 70 to 110 seconds for a 34 mL cell 160 to 200 seconds for a 66 mL cell 250 to 290 seconds for a 100 mL cell ST...

Page 139: ...DIAGNOSTICS MENU 1 Press MENU to display the MENU screen see Section C 1 1 2 Press an up or down arrow button to move the cursor to the DIAGNOSTICS option and then press ENTER To display a diagnostics...

Page 140: ...this screen Figure C 7 Sensors Screen Parameter Description CELL DETECT When the cell door is closed the sensor can detect whether a cell is installed in the cell holder The sensor cannot identify whi...

Page 141: ...scription Specification SYSTEM Indicates the internal system pressure 0 34 0 02 MPa 50 3 psi COMPRESSION Indicates the pressure applied when the oven is compressed 0 90 0 03 MPa 130 5 psi BOTTLE Indic...

Page 142: ...vapor threshold if necessary Figure C 9 Hydrocarbon Sensor Screen Parameter Description ACTUAL Indicates the hydrocarbon level detected by the hydrocarbon sensor THRESHOLD Selects the solvent vapor th...

Page 143: ...ndicates the number of extractions performed since the ASE 150 was installed or the extraction counter was last reset PUMP STROKE Indicates the number of pump strokes performed since the ASE 150 was i...

Page 144: ...en The MODULEWARE screen indicates which version of ASE 150 Moduleware is currently installed The MODULEWARE screen is also displayed for a few seconds when the ASE 150 power is turned on Figure C 11...

Page 145: ...steel sample cell 10 mL assembled 1 068088 Stainless steel sample cell 22 mL assembled 1 068089 Stainless steel sample cell 34 mL assembled 1 068090 Stainless steel sample cell 66 mL assembled 1 06809...

Page 146: ...ell end caps Viton Pkg 50 049660 O ring insertion tool 1 068093 Cellulose filters 27 mm Pkg 100 056780 Cellulose filters 30 mm Pkg 100 068092 Glass fiber filters 27 mm Pkg 100 056781 Glass fiber filte...

Page 147: ...clear 60 mL includes lids and septa Pkg 72 048781 Collection vials amber 60 mL includes lids and septa Pkg 72 068226 Collection vial clear 60 mL graduated Class A includes lid and septum 1 068248 Coll...

Page 148: ...w pressure air seal 1 Static Valve 068115 Static Valve Repair Kit 1 068116 Static Valve Tool Kit 1 066165 Static valve seal 1 067381 Static valve piston 1 Miscellaneous 954746 Fast blow IEC127 fuse 10...

Page 149: ...to the costs associated with sample preparation studies have shown that the biggest bottleneck and source of errors in any analytical process are found in sample preparation If we want to have the bi...

Page 150: ...tions boil at relatively low temperatures This is one limitation of techniques such as Soxhlet or automated Soxhlet The highest temperature at which extractions take place in these techniques is the b...

Page 151: ...in the collection vessel holder The oven is maintained at the chosen operating temperature throughout the extraction room temperature to 200 C The cell design and associated fluid apparatus allow oper...

Page 152: ...vary from 0 to 99 minutes After the static time fresh solvent is pumped through the cell to remove extracted analytes while the sample and solvent are still hot The amount used for the rinse can vary...

Page 153: ...on to occur In general the same sample preparation that is done prior to Soxhlet or sonication extraction should be done prior to extraction by ASE This section discusses three sample preparation tech...

Page 154: ...ample was extracted with a mixture of hexane 2 propanol 3 2 using the following ASE conditions 1000 psi 125 C 6 min heat up 3 x 10 min static cycle 100 rinse 60 s purge and one 11 mL cell containing o...

Page 155: ...and make the sample easier to handle Drying Samples do not have to be completely dry to achieve efficient extractions with ASE This depends on the analytes and the solvent used for extraction High lev...

Page 156: ...ble to solubilize the target analytes while leaving the sample matrix intact The polarity of the extraction solvent should closely match that of the target compounds The common adage of like dissolves...

Page 157: ...As the temperature is increased the viscosity of the solvent is reduced thereby increasing its ability to wet the matrix and solubilize the target analytes The added thermal energy also assists in bre...

Page 158: ...d a critical experimental parameter ASE extractions are performed at 1500 psi 10 MPa Cycles The use of static cycles was developed to introduce fresh solvent during the extraction process which helps...

Page 159: ...e on sample preparation Select the sample cell size that most closely matches the sample size The sample cells do not need to be filled completely however a full cell will use less solvent in the extr...

Page 160: ...ASE process The choice of temperature alone can affect selectivity The higher the temperature for the extraction the less selective the results Lowering the temperature will make ASE more selective b...

Page 161: ...t would interfere in the determinative step Next the samples were extracted with hexane ethyl acetate to remove the steroid compounds Solvent fractionation using ASE is an area that needs to be explor...

Page 162: ...gnated silica gel and ion exchange resins Table E 2 shows a summary with related references There are a few interesting things to note from this table Acid impregnated silica gel has the highest capac...

Page 163: ...involved in projects to determine perchlorate in soils and vegetation samples Water at 80 C was used as the extraction solvent Alumina was used to remove colored compounds such as chlorophyll Ion exc...

Page 164: ...hat was superior to conventional SPE after exhaustive extraction This work demonstrated the fractionation of lipid classes using sequential extractions Unmodified silica and cyanopropyl silica were us...

Page 165: ...ompounds in Soil American Laboratory 27 4 24 28 1995 2 F H fler J Ezzell and B Richter Beschleunigte L semittelextraktion ASE Teil 1 LaborPraxis 19 3 62 67 1995 3 F H fler J Ezzell and B Richter Anwen...

Page 166: ...iver J Chromatogr B Anal Technol Biomed Life Sci 753 217 223 2001 13 J Ezzell B Richter and E Francis Selective Extraction of Polychlorinated Biphenyls from Fish Tissue Using Accelerated Solvent Extra...

Page 167: ...lfur Cleanup U S Environmental Protection Agency Cincinnati OH 1996 24 M Nording S Sporring K Wiberg E Bj rklund and P Haglund Monitoring Dioxins in Food and Feedstuffs Using Accelerated Solvent Extra...

Page 168: ...of Organochlorine Pesticides in Soil J Chromatogr A 1152 247 253 2007 32 Dionex Corporation Fast Determination of Acrylamide in Food Samples Using Accelerated Solvent Extraction ASE Followed by Ion Ch...

Page 169: ...140 Autoignition point of solvents 25 AutoSeal Function 8 Inspecting tips for damage 55 Location 8 Pressure when actuated 112 133 B Basic solvents Shutdown procedure 55 Blueberry extracts 153 BNA met...

Page 170: ...h 24 Editing 49 52 Parameters 49 129 D Daily maintenance 54 Danger icon 3 Degassing solvents 26 Diagnostics 2 Diagnostics screen 131 Displaying 131 Diatomaceous earth DE 31 32 140 Dimensions of ASE 15...

Page 171: ...ose 34 Part number 138 Filters glass fiber 34 Part number 138 Fittings Gas leaks 67 Liquid leaks 65 Nitrogen 108 Replacing 69 Solvent reservoir 29 Tightening 69 Flush See Rinse cycle during a method F...

Page 172: ...2 Parameters 49 129 Methods preprogrammed 20 Chlorinated herbicides HRB 20 21 Dioxins and furans PDF 20 22 Organochlorine pesticides OCP 20 21 Organophosphorous pesticides OPP 20 22 Polychlorinated bi...

Page 173: ...lacing 79 83 Pneumatic specifications 104 Post run procedures 46 PPE method parameters 23 Preparing the sample 31 Preparing to run 25 Preprogrammed methods 20 Chlorinated herbicides HRB 20 21 Dioxins...

Page 174: ...gnostics 2 Safety icons 3 4 Safety messages 3 4 Safety standards and labels 5 Sample Difficult to extract 53 Dry 32 Liquid 32 Loading into cell 37 Wet 31 32 Sample cell end cap 11 O rings Teflon 138 O...

Page 175: ...level required 29 113 Solvent sample equilibrium 53 Solvents Autoignition points 25 Degassing 26 Reducing usage 37 Rinsing after a change 48 Selecting 25 26 Selection guidelines 26 Source needle 8 Liq...

Page 176: ...al cables 67 Error messages 57 Excessive cell pressure 58 Liquid leaks 65 67 System stopped 67 Tubing Vent 109 U Up Down switch 7 8 V Valves Pressure relief 17 84 Static 17 86 Vapor threshold exceeded...

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