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Verifying Operation

Before performing an analysis, verify that the pycnometer is operating prop-
erly by performing the following steps.

Numbers are displayed on the pycnometer as shown in the following
example:
10000.00

Note that a period is used to denote a decimal fraction.

1.

Press

to zero the transducer.

2.

Once the zeroing process is complete (the pressure display shows ap-

proximately zero), press

on the keypad to enter manual

mode.

3.

Use the

,

, and

keys to close all valves. A valve

opens and closes when you press the appropriate key. The valve is open
when the indicator above the key is on and closed when the indicator is
off.

4.

Open the fill valve. Wait until the pressure reaches 15 to 19 psig.

Do not exceed 19.9 psig. If the pressure exceeds 20 psig the transducer
may overrange and an error message will be displayed. If this occurs,
open the expansion and vent valves and allow the transducer to drift
back down, then start the procedure over.

5.

Close the fill valve.

6.

Observe the pressure display. After an equilibration period, the pressure
should not vary more than 0.005 psig/min.

7.

Open the expansion valve.

8.

Observe the pressure display. After equilibration, the pressure should not
vary more than 0.005 psig/min. Open the vent valve. After a period of
time, the pressure should again stabilize.

If the pycnometer responds as described above, it is ready to operate. If it
does not, check installation procedures, then repeat the verification proce-
dures. If it still does not respond as described above, service to the system or
operational assistance may be required. Contact a Micromeritics Service Rep-
resentative.

0

1

FILL

EXPAND

VENT

AccuPyc 1330

Verifying Operation

September 1996

2-11

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Summary of Contents for AccuPyc 1330

Page 1: ...AccuPyc 1330 Pycnometer Operator s Manual V3 03 Part No 133 42808 01 January 2005 ...

Page 2: ... Instrument Corporation Micromeritics Instrument Corporation 2005 All rights reserved The software described in this manual is furnished under a license agreement and may be used or copied only in ac cordance with the terms of the agreement ...

Page 3: ...rtain products sold by MICROMERITICS are the products of reputable manufacturers sold under their respective brand names or trade names We therefore make no express or implied warranty as to such products We shall use our best efforts to obtain from the manufacturer in accordance with his customary practice the repair or replacement of such of his products that may prove defective in workmanship o...

Page 4: ...nometer 2 7 Entering Report and Analysis Parameters 2 8 Selecting Units of Pressure Measurement and Operating Language 2 9 Greasing the Chamber Cap O Ring 2 10 Verifying Operation 2 11 3 PERFORMING AN ANALYSIS Setting Regulator Pressure 3 1 Preparing and Loading a Sample 3 2 Starting an Analysis 3 4 Using the Default Parameters 3 4 Using Modified Analysis Parameters 3 4 Viewing or Printing Analysi...

Page 5: ...on 4 26 Unit Types Operating Language Date and Time 4 27 5 TROUBLESHOOTING AND MAINTENANCE Troubleshooting 5 1 Error and Status Messages 5 5 Queued Messages 5 5 Messages Displayed During an Automatic Operation 5 12 Maintenance 5 14 Replacing the Chamber Cap O Ring 5 15 Checking the Cell and Expansion Chambers for Leaks 5 16 Replacing the Gas Inlet Filters 5 18 Cleaning the Pycnometer 5 21 Recoveri...

Page 6: ...CHAPTER 1 GENERAL INFORMATION Organization of the Manual Conventions Equipment Description ...

Page 7: ...nstructions Chapter 5 Provides troubleshooting and maintenance procedures and error messages Chapter 6 Provides information on ordering parts and accessories for the pycnometer Several appendices are also included Conventions This manual uses the icons shown below to identify notes of importance cautions and warnings Notes contain information to help you operate the instrument more effectively Cau...

Page 8: ...lowing illustration contains a keypad a display area and an analysis chamber referred to as the cell chamber The pycnometer is controlled by commands entered through the keypad The operational status of the pycnometer can be continually moni tored on the display The optional printer prints out complete analysis and calibration results A serial port is provided for electronic data transmission Figu...

Page 9: ... and run A purge is used strictly for sample clean up and air and moisture removal from the chamber s inside It is accomplished by closing off the pycnometer block and filling the cell chamber to the designated purge fill pressure The chambers are then vented to atmosphere resulting in elimination of water va por or other contaminants A run is used for collecting the precise accurate data used in ...

Page 10: ...e the key To select the alternate function printed above the key first press then press the key For ex ample press to print Refer to Ta ble 1 2 To select the primary function on the face of the key press only that key For example press to enter the number 6 Refer to Table 1 1 FILL ANALYZE EXPAND VENT REVIEW PRINT MANUAL SETUP TRANSMIT ESCAPE ZERO CALIBRATE 8 9 5 6 1 2 3 0 7 4 SAVE CLEAR ENTER CHOI...

Page 11: ... when in display mode Clear an entry when in a command mode Save the information you entered and return to display mode Blank Change the keypad mode The keypad may be used in either primary function mode or alternate function mode When you press the Blank key to enter alternate function mode a plus sign appears in the upper right corner of the display and the commands written above the keys become...

Page 12: ... display mode If an automatic operation is in progress cancel the operation ANALYZE Perform an analysis REVIEW Review or edit completed analysis or calibration data PRINT Print analysis or calibration report If an automatic operation is in progress print a partial report FILL when in manual mode Open and close the fill valve The indicator above the FILL key is on when the valve is open and off whe...

Page 13: ...les Provide ranges of 1 to 100 cm3 Precision Reproducibility typically to within 0 01 of the nominal full scale cell chamber volume Reproducibility guaranteed to within 0 02 of the nominal full scale volume on clean dry thermally equilibrated samples Accuracy Accurate to within 0 03 of reading plus 0 03 of nominal full scale cell chamber volume Cabinet 3ll mm W x 173 mm H x 357 mm D 12 in W x 7 in...

Page 14: ...CHAPTER 2 INSTALLATION Unpacking and Inspection Selecting the Location Gas Requirements Equipment Setup Verifying Operation ...

Page 15: ...gator must examine the cartons in order to complete the inspection report Equipment Damage or Loss During Shipment If equipment is damaged or lost in transit you are required to make note of the damage or loss on the freight bill The freight carrier not Micromeritics is responsible for all damage or loss occurring during shipment If you dis cover damage or loss of equipment during shipment report ...

Page 16: ...der or purchase order for the equipment and provide the date the equipment was received 3 Notify a Micromeritics Service Representative of the defect and request shipping instructions The Service Department will assign a Return Mate rial Authorization RMA number to your return and provide shipping in formation Unpacking and Inspection AccuPyc 1330 2 2 September 1996 ...

Page 17: ...99 995 pure or better to provide rapid accu rate analyses The cylinder containing helium must be fitted with a gas regu lator and the regulator set for 15 to 23 psig we recommend 20 22 psig In no instance should the pressure input to the pycnometer be greater than 23 psig Excessive pressures waste gas due to a protection device contained in the pycnometer that vents the pycnometer to atmospheric p...

Page 18: ...onal 1 4 turn Do not overtighten the fittings Doing so can collapse the brass fitting and cause a leak 4 Attach the copper tubing to the brass reducer fitting 5 Turn the nut on the tubing clockwise until it is finger tight Then use a 7 16 in open ended wrench or an adjustable wrench to tighten the nut an additional 1 4 turn 6 Attach the other end of the copper tubing to the fitting on the INLET co...

Page 19: ...m 9 If a serial line is to be used for data transmission connect one end of the RS 232 cable to the connector labeled RS 232 on the back of the pycnometer Connect the other end to the output device 10 Connect one end of the printer cable to the connector labeled with the printer icon on the back of the pycnometer Connect the other end to the input connector on the printer Refer to Appendix E Print...

Page 20: ...t into the connector on the rear panel of the pycnometer and press firmly to lock into place The software card must be properly inserted in the pycnometer connec tor during operation It is best to keep it installed at all times even when power to the unit is turned off Figure 2 9 Inserting Software Card 12 Plug in the printer power cord and the pycnometer power cord Notched End of Software Card Eq...

Page 21: ...first message Continue pressing to cycle through all mes sages and return to the Reload prompt When the system is turned on the first time or after a period of non use it should be allowed to warm up for at least 30 minutes before analyses are performed For analyses that require very precise results it should warm up for two hours It is important that a constant temperature be maintained inside th...

Page 22: ... use these values no further action is necessary If you wish to change the values refer to Analysis or Calibration Parameters in Chapter 4 The pycnometer is shipped with the following default values for report op tions Request sample ID no Analysis display mode volume Report destination display Transmission format Single column If you wish to use these values no further action is necessary If you ...

Page 23: ...he Chamber Cap O Ring If you wish to change the defaults 1 Press then press until Unit types is displayed Press 2 Press then to change the value to kPag 3 The Language prompt is displayed Press until the desired lan guage is displayed then press If there are error messages in the message queue indicated by an aster isk next to the Reload prompt delete the messages before changing lan guages Refer ...

Page 24: ...n imperfect seal and leaks 1 Remove the chamber cap by turning it counterclockwise then lifting off 2 Using your fingertip apply a thin layer of Dow Corning high vacuum grease or equivalent to the greasing disk 3 Insert the greasing disk into the chamber cap and turn slightly to apply a very light coating of grease to the O ring Apply a VERY LIGHT coating of grease to the O ring There should be no...

Page 25: ...s 20 psig the transducer may overrange and an error message will be displayed If this occurs open the expansion and vent valves and allow the transducer to drift back down then start the procedure over 5 Close the fill valve 6 Observe the pressure display After an equilibration period the pressure should not vary more than 0 005 psig min 7 Open the expansion valve 8 Observe the pressure display Af...

Page 26: ...CHAPTER 3 PERFORMING AN ANALYSIS Setting Regulator Pressure Preparing and Loading a Sample Starting the Analysis Viewing or Printing Analysis Results ...

Page 27: ... sample to be inadequately saturated resulting in inaccurate data or termination of analysis Before beginning an analysis check the regulator pressure Fill pressure is user specified for purge and run using the AccuPyc 1330 Set Up function re fer to Analysis or Calibration Parameters in Chapter 4 Set the regulator pressure at the higher of the two plus about 2 0 psig as follows 1 Press to enter ma...

Page 28: ...rting or re moving a sample If the chamber remains uncapped temperature insta bility will occur which could affect analysis results 1 Weigh the empty sample cup If volume only is to be measured you may skip this step 2 Place a quantity of sample in the cup Use as large a quantity of sample as possible we recommend that the cup be at least two thirds full Pack powders and fluffy materials if permis...

Page 29: ... If the cap is placed on a dirty surface analysis errors may result 7 Insert the sample cup with sample into the cell chamber Figure 3 1 Inserting Sample Cup Into Cell Chamber 8 Replace the cell chamber cap Do not remove the cell chamber cap when the pycnometer is pressur ized Sample may be discharged from the chamber AccuPyc 1330 Preparing and Loading a Sample September 1996 3 3 ...

Page 30: ...in the Re port Options function Using sample IDs can help you keep track of data from various analyses You may for example use the sample ID as a date and time stamp The sample ID can contain from 1 to 20 numbers and dashes Enter the sample ID and press 3 The following prompt is displayed if density was selected for Analysis display mode in the Report Options function Enter the sample weight and p...

Page 31: ... move the sample from the cell chamber Press to cycle through the error messages 3 After the error messages are displayed the average volume or density and the deviation from the mean are displayed Press 4 A report is automatically printed if report destination was set to printer If not you may print a report by pressing You may transmit a report by pressing 5 When the Reload prompt is displayed y...

Page 32: ...TIONS Monitoring the System Canceling an Automatic Operation Entering Commands Printing Reports Transmitting Reports Calibrating the Pycnometer Zeroing the Pressure Transducer Manually Controlling the Valves Editing the Setup Parameters ...

Page 33: ...ther than the follow ing until the operation is finished Press to cancel the automatic operation Press to print a partial report of analysis or calibration results Press to transmit a partial report of analysis or calibra tion results Analysis is suspended until printing or transmission is complete The following example shows a typical status message for an automatic opera tion Refer to Table 4 1 ...

Page 34: ...tion with the calibration standard in the cell chamber Zero Zero offset Pressure Display P Current pressure in system P1 Pressure for data point P1 P2 Pressure for data point P2 Operation Mode Purg Purge in progress Zero Transducer zero reset in progress Run Run in progress Action fill Filling the cell chamber or expansion chamber equil Equilibrating wait Wait the displayed number of seconds Refer...

Page 35: ...gh the messages You may press while a message is displayed to delete the messsage Operation Error Messages Report Error Messages Report Data After the operation error messages report error messages then report data average density or volume and deviation from the mean are displayed The messages remain in the message queue until you delete them or until another automatic operation is begun at which...

Page 36: ...ination process which vents the system takes about 30 seconds You may cancel the termination process by pressing again but if you do you must manually vent the system If no runs were completed and there are not enough data to compute the fol lowing message is displayed If there are enough data to compute and reports were requested they are printed CLEAR Press ENTER to cancel automatic operation EN...

Page 37: ...e the default value just press the key For example when you press the following prompt is displayed To select analysis parameters which is the default value press If you do not wish to use the default value you can use the keypad to enter other responses There are two types of prompts data entry and multiple choice Prompts that require you to enter data are followed by a colon Use the keypad to en...

Page 38: ...if density was selected for Analysis display mode refer to Report Options later in this chapter Enter the sample weight and press Range 000 0000 to 999 9999 g Choose one of the following Press to start the analysis The analysis begins and operational status messages are continually displayed Press to store the data you entered and return to display mode Press to cancel the analysis 4 Sample ID ENT...

Page 39: ...nalysis results Display Entry The sample ID is displayed if it is enabled in the Set Up function refer to Report Options later in this chapter Press This prompt is displayed only if density is selected for Analysis display mode refer to Report Options The sample weight entered in the Start Analysis function is displayed Press 5 Sample ID sample ID ENTER Sample Weight weight ENTER AccuPyc 1330 Revi...

Page 40: ... to it Similarly a density or volume that was previously excluded from the calculated average may be included by pressing When you press a new deviation is calculated and displayed Press to display values for the next run Press when you wish to exit review and edit mode and return to display mode When you press all collected data are automatically recalculated and all data reduction messages are a...

Page 41: ...y pressing When a volume is excluded from the average an asterisk appears next to it Likewise a cell or expansion volume that was previously excluded from the calculated average may be included by pressing When you press a new deviation is calculated and displayed Press to display values for the next run Press when you wish to exit review and edit mode and return to display mode When you press all...

Page 42: ...ns the date and time the analy sis was started and completed and the temperature of the cell chamber The display report for calibration contains average cell or expansion volume depending on the option selected refer to Report Options and the devia tion from the mean The printed report contains cell and expansion volumes for each run as well as an average of all runs A run with an asterisk next to...

Page 43: ... a calibration report The calibration standard used must be at least 10 of nominal cell volume We recommend 60 to 70 for the best results Figure 4 1 Calibration Report AccuPyc 1330 Printing Reports September 1996 4 11 ...

Page 44: ...The following report represents an analysis that was performed on the calibra tion standard used for the previous report Figure 4 2 Analysis Report Printing Reports AccuPyc 1330 4 12 September 1996 ...

Page 45: ...sion enabled The run precision fea ture eliminates data from all but five runs that are within a specified tolerance An asterisk next to a run indicates that the data from the run were eliminated from the calculations Figure 4 4 Analysis with Run Precision Report AccuPyc 1330 Printing Reports September 1996 4 13 ...

Page 46: ...nsmit report data over the serial line If you press during an automatic operation a partial report is transmitted You may cancel report data sent to the serial line by pressing You may cancel partial reports that were requested during an automatic opera tion when the following message is displayed Reports may be transmitted in one of two formats single column or spread sheet Refer to Appendix D Fo...

Page 47: ...nter the volume of the calibration standard and press Range 0 1 to 999 0000 cm3 Press to begin the calibration or to cancel the calibration Status messages are displayed during the first phase of calibration When the first phase ends the pycnometer beeps three times Place the calibration standard in the cup in the cell chamber In most cases use one ball for the 100 cm3 pycnometer two balls for the...

Page 48: ...r is automatically set to zero for each run in an analysis or calibration Press to zero the pressure transducer Display Entry Press to zero the transducer or to cancel the operation The transducer is zeroed and the pycnometer returns to display mode 0 Enter to start Escape to cancel ENTER CLEAR Zeroing the Pressure Transducer AccuPyc 1330 4 16 September 1996 ...

Page 49: ...7 Opens and closes the fill valve 8 Opens and closes the expansion valve 9 Opens and closes the vent valve Observe the indicators above the and keys When a valve is open the indicator is on When a valve is closed the indicator is off Press when you wish to exit manual mode and return to display mode Prolonged opening of all three valves at one time may cause excessive loss of helium 1 Manual p pre...

Page 50: ...re also entered for calibration parameters These may be ed ited in the same manner as analysis parameters The only difference is that for calibration the maximum number of purges and runs that will be per formed by the system is ten Report options specify the report mode density or volume for analysis and the report destination Calibration volumes specify the sample volume and the expansion volume...

Page 51: ...er the fill pressure and press Range 0 to 19 850 psig 0 to 136 86 kPag Generally the greater the fill pressure the easier it is to measure the volume precisely However a lower pressure may be desirable for some samples Enter the number of runs to be performed and press Range 1 to 99 Enter the fill pressure and press Range 0 to 19 850 psig 0 to 136 86 kPag 2 Set up type Analysis parameters CHOICE E...

Page 52: ...of the analysis when certain criteria are met When you select run precision the analysis will be terminated after five consecutive runs are within the specified tolerance If you select run precision you should request a large number 50 to 99 of runs If you select a small number of runs the analysis will stop when the number you entered is reached even though the specified tolerance has not been me...

Page 53: ...ange 0 01 to 50 Nominal cell volume is the sample capacity Choose one of the following options Press to save the information you entered and return to display mode Enter another set up type Press to discard the information you entered and return to display mode Percent full scale 0 05 ENTER Set up type Analysis parameters SAVE CLEAR AccuPyc 1330 Editing the Setup Parameters September 1996 4 21 ...

Page 54: ...p track of data from various analyses For example you can use the sample ID as a date and time stamp Select either yes or no then press Select the format of data to be used when transmitting reports Refer to Appendix D for a description of the formats Choices Single column Spreadsheet Select the destination of the report that is automatically generated after an analysis or calibration then press C...

Page 55: ...e of the following options Press to save the information you entered and return to display mode Enter another set up type Press to discard the information you entered and return to display mode Set up type Report options SAVE CLEAR AccuPyc 1330 Editing the Setup Parameters September 1996 4 23 ...

Page 56: ... cm3 The temperature offset is pre set at the factory and is entered on the Calibration Sheet shipped with the instrument It should not be changed unless the battery backed RAM is reinitialized If battery backed RAM is reinitialized enter the value from the calibration sheet and press Range 0 to 100 00 C 2 Set up type Calibration data CHOICE ENTER Cell volume value from calibration ENTER Expansion...

Page 57: ...he information you entered andreturn to display mode Enter another set up type Press to discard the information you entered and return to display mode Set up type Calibration data SAVE CLEAR AccuPyc 1330 Editing the Setup Parameters September 1996 4 25 ...

Page 58: ...hen press Choices none even odd Select either disabled or enabled then press Choose one of the following options Press to save the information you entered and return to display mode Enter another set up type Press to discard the information you entered and return to display mode 2 Set up type Data transmission CHOICE ENTER Baud rate 9600 baud ENTER Number of data bits 8 ENTER Number of stop bits 1...

Page 59: ...oad prompt delete the messages before changing lan guages Refer to Error Report and System Status Messages in Chapter 4 Make sure you press SAVE after changing languages The date is included in all printed and transmitted reports If the date shown is incorrect you may enter the correct date as follows day month year Note that each entry must contain two digits For example to enter September 1 1992...

Page 60: ...ntry must contain two digits For example to enter 1 05 P M enter 13 05 00 and press The key is used to enter a colon Choose one of the following options Press to save the information you entered and return to display mode Enter another set up type Press to discard the information you entered and return to display mode Time HH MM SS pre set time ENTER Set up type Unit types SAVE CLEAR Editing the S...

Page 61: ...CHAPTER 5 TROUBLESHOOTING AND MAINTENANCE Troubleshooting Error and Status Messages Maintenance ...

Page 62: ...s What Happened Why What To Do Nothing happens when power switch is turned on ie no lights on schematic display noth ing on LCD screen Power cord not fully inserted at one end or the other Insert power plug firmly into outlet socket insert unit connector firmly into power connector opening No power at outlet Plug in lamp or small appliance to test outlet If there is no power contact electrician Pl...

Page 63: ...y closed Close chamber cap by turning clockwise Chamber cap contains dust or debris or the O ring is not properly greased Using a lint free tissue clean the chamber cap and the rim of the cell chamber Lightly grease the chamber cap O ring refer to Greasing the Chamber Cap O Ring later in this chapter O ring in chamber cap not properly seated Check the chamber cap Ensure that the O ring is properly...

Page 64: ...p If offset is negative run new zero offset Zeroing the Pressure Transducer Chapter 4 Helium drained from tank Leaks in the gas line connection Pressurize the system Close then open the Cylinder Shut Off Valve If the needle on the pressure gauge on the gas cylinder jumps abruptly a leak in the gas line connections may be indicated Check all gas line connections Refer to Rear Panel Connections in C...

Page 65: ...om sample Refer to Preparing and Loading a Sample Chapter 3 Pycnometer leaks Check cap O ring for defects Regrease or replace the O ring if necessary While in Manual Mode with the cap installed open all valves With helium flowing through the pycnometer actuate the expansion valve repeatedly for approximately 1 minute This will remove lint which could cause a leak from the valve seat Repeat the pro...

Page 66: ...pt ANLSERR Eq failure NN ZZ runs completed Cause The sample being analyzed failed to equilibrate in 1000 seconds Action Check the system carefully for leaks as described in Checking the Cell and Expansion Chambers for Leaks later in this chapter Make sure the sample is properly prepared before performing an analysis Cause Sample foams organics etc absorbs helium slowly Action Set the equilibration...

Page 67: ...rred in the pressure measurement elec tronics Action Call a Micromeritics Service Representative CAL1ERR Eq failure NN ZZ runs completed Cause The empty cell chamber failed to equilibrate in 1000 sec onds during the first pass of calibration Action Check the system for leaks as described under Checking the Cell and Expansion Chambers for Leaks later in this chapter CAL1ERR Fill failure NN ZZ runs ...

Page 68: ...tion because an error occurred in the pressure meas urement electronics Action Call a Micromeritics Service Representative CAL2ERR Eq failure NN ZZ runs completed Cause The calibration standard failed to equilibrate in 1000 sec onds during the second pass of calibration Action Check the system for leaks as described under Checking the Cell and Expansion Chambers for Leaks later in this chapter CAL...

Page 69: ... urement electronics Action Call a Micromeritics Service Representative CAL2ERR Underrange NN ZZ runs completed Cause A pressure underrange occurred during the second pass of calibration because an error occurred in the pressure meas urement electronics Action Call a Micromeritics Service Representative DATA_ERR No data to compute Cause An automatic operation was canceled before all necessary data...

Page 70: ...full scale Cause The amount of sample placed in the sample cup was so small that the percentage of precision may be inferior Action Rerun the sample using enough material to occupy the maximum amount of the nominal cell chamber volume HW_ERR A D I O failure Cause An error in the pressure measurement electronics has occurred Action Call a Micromeritics Service Representative HW_ERR BB RAM has been ...

Page 71: ...matic operation was canceled Action Restart the automatic operation if desired TRN_ERR Timeout failed to respond Cause The receiving device took longer than 10 seconds to ac knowledge receipt of data from the pycnometer Action Make sure the receiving device is properly connected to the pycnometer RS 232 port and is turned on Verify that the serial I O parameters controlling the receiving device co...

Page 72: ...e Cause A pressure overrange occurred but was left uncorrected Action Return to manual mode and vent the system ZEROERR Eq failure Cause The system failed to equilibrate within 1000 seconds Action Check the pycnometer for leaks Make sure the pycnome ter has been placed in a draft free environment ZEROERR Overrange Cause A pressure overrange occurred while zeroing Action Check for a fill valve leak...

Page 73: ...s to acknowledge receipt of data from the pycnometer Action Check to make sure the printer is properly connected to the pycnometer is turned on and is on line Sending line line number ESCAPE to cancel Cause Status message displayed when data are being transmitted Action None this is a status message only Transmission port not responding Cause The receiving device took longer than five seconds to a...

Page 74: ...an Xon The following message is displayed on the printer or on the screen for trans mitted data No collected data to report or all runs excluded Cause This message is printed or transmitted if you requested a report but there is either no data available or data has been excluded via review mode Action Initiate an automatic operation or return to review mode and include at least one run AccuPyc 133...

Page 75: ...seal 1 Remove the chamber cap by turning it counterclockwise then lifting off 2 Wipe off the old grease using lint free tissue 3 Using your fingertips apply a thin layer of Dow Corning high vacuum grease or equivalent to the greasing disk 4 Insert the greasing disk into the chamber cap and turn slightly to apply a very light coating of grease to the O ring Apply a VERY LIGHT coating of grease to t...

Page 76: ...he metal surfaces When it is necessary to replace the O ring follow these steps 1 Remove the O ring from its groove by pushing a sharp tool into the ring and prying it out Be careful not to scratch the metal surface of the chamber cap Scratches could result in an imperfect seal Figure 5 2 Removing the Chamber Cap O Ring AccuPyc 1330 Maintenance September 1996 5 15 ...

Page 77: ... and expansion chambers for leaks perform the following procedure This procedure should be performed in a temperature stable environ ment after the pycnometer has been warmed up for at least two hours Before performing this procedure check the chamber cap to ensure that it is not the source of leaks It should be free from particles the O ring should be properly seated and it should not contain exc...

Page 78: ...ary more than 0 005 psig min proceed to step 8 If the pressure varies more than 0 005 psig min temperature instability or a leak may be indicated Vent the system then repeat steps 4 through 7 several times to verify that a leak is indicated If a leak is indicated call a Micromeritics Service Representative 8 Press to open the expansion valve and to open the fill valve 9 Fill the chambers to 19 5 p...

Page 79: ...n sion valve and FILL to open the fill valve The power cord should be disconnected from the unit before disconnect ing the gas supply Failure to do so could result in electrical shock 3 Observe the pressure reading When the pressure drops to less than 1 psig place the power switch on the back of the pycnometer in the off 0 position Remove power cord 4 Disconnect the gas supply line from the rear p...

Page 80: ...g screws that hold the panel in place Figure 5 5 Removing Rear Panel 8 Lift the side panels at the rear of the pycnometer and rotate forward The cover should lock in an upright position as shown below Figure 5 6 Rotating Top Panel 9 Remove the two screws that secure the gas inlet entrance assembly AccuPyc 1330 Maintenance September 1996 5 19 ...

Page 81: ... gas entrance block with lint free cloth to remove any grease that may still be present 12 Very lightly grease the new O ring with high vacuum grease Apply only a very light coating of grease Too much grease can clog the filter or disrupt gas flow Filter and O ring Gas Inlet Entrance Assembly Maintenance AccuPyc 1330 5 20 September 1996 ...

Page 82: ...could result in electrical shock to personnel or damage to the unit Do not allow liquid to penetrate the casing of the pycnometer Doing so could result in damage to the unit Recovering from a Power Failure The pycnometer has a battery back up feature that saves entered data in case of a power failure Set up parameters and any other data entered will still be present when power is restored If an au...

Page 83: ...CHAPTER 6 ORDERING INFORMATION ...

Page 84: ...mbly 10 cm3 133 25863 00 Filtered cup assembly 100 cm3 004 25575 00 Chamber Cap O ring 10 cm3 004 25577 00 Chamber Cap O ring 100 cm3 133 34900 00 Calibration Standard Kit contains two 10 cm3 calibration standards and one 10 cm3 sample cup 133 34902 00 Calibration Standard Kit contains one 100 cm3 calibration standard and one 100 cm3 sample cup 004 25633 00 Calibration Standard 10 cm3 004 25632 00...

Page 85: ...ing Disk 003 20616 01 RS 232 Cable F F 10 ft shielded 133 42701 01 French Template 133 42701 02 German Template 133 42701 03 Spanish Template 133 42701 04 Italian Template 133 42808 00 Operator s Manual Ordering Information AccuPyc 1330 6 2 January 2005 ...

Page 86: ...APPENDIX A CHANGING THE ANALYSIS MODULE ...

Page 87: ...pply 2 Press on the pycnometer keypad to enter manual mode Then press VENT to open the vent valve EXPAND to open the expansion valve and FILL to open the fill valve The power cord should be disconnected from the unit before disconnect ing the gas supply Failure to do so could result in electrical shock 3 Observe the pressure reading When the pressure drops to less than 1 psig place the power switc...

Page 88: ...as vent line if attached by gently pulling the flexible tub ing from the rigid tubing labeled VENT at the rear of the pycnometer 6 Remove the printer cable and the serial cable if used from the rear panel of the pycnometer 7 Remove the cap from the cell chamber FILL ANALYZE EXPAND VENT REVIEW PRINT MANUAL SETUP TRANSMIT ESCAPE ZERO CALIBRATE 8 9 5 6 1 2 3 0 7 4 SAVE CLEAR ENTER CHOICE APPENDIX A A...

Page 89: ... Removing Rear Panel 9 Lift the side panels at the rear of the pycnometer and rotate forward as shown in Figure A 4A After about 100 degrees rotation the assembly should lock in an upright position as shown in Figure A 4B Figure A 4 Rotating Top Panel A B AccuPyc 1330 APPENDIX A September 1996 A 3 ...

Page 90: ...cap completely and use the knob as a handle to pick up the module Observe the standoffs mounted to the baseplate and the corresponding recesses in the rails 12 Disconnect the cable assemblies going to the valves mounted to the block Figure A 6 Disconnecting Cable Assemblies Mounting Rails Standoffs Disconnect Valve Cables Here Disconnect Electronics Module Cables Here APPENDIX A AccuPyc 1330 A 4 S...

Page 91: ...ake sure the standoffs fit into the corresponding recesses in the rails Note that the transducer should be on the rear face of the module 17 Reassemble the pycnometer by reversing steps 1 through 10 Be sure to re move the cap before closing the cover and to reconnect all cables and the gas supply line Check the gas connection for leaks 18 Set the regulator pressure as described in Setting Regulato...

Page 92: ...APPENDIX B ANALYSIS THEORY ...

Page 93: ...ure Ta and that the valve is then closed VCELL is then charged to an elevated pressure P1 The mass balance equation across the sample cell VCELL is P1 VCELL VSAMP ncRTa 1 where nc the number of moles of gas in the sample cell R the gas constant and Ta the ambient temperature Figure B 1 Simplified Block Diagram The mass equation for the expansion volume is Pa VEXP nERTa 2 where nE the number of mol...

Page 94: ...o 3 P2 VCELL VSAMP VEXP P1 VCELL VSAMP PaVEXP 4 or P2 P1 VCELL VSAMP Pa P2 VEXP 5 then VCELL VSAMP Pa P2 P2 P1 VEXP 6 Adding and subtracting Pa in the denominator and rearranging gives VSAMP VCELL Pa P2 VEXP P2 Pa P1 Pa 7 Dividing by Pa P2 in both the numerator and denominator VSAMP VCELL VEXP 1 P1 Pa Pa P2 8 or VSAMP VCELL VEXP P1 Pa P2 Pa 1 9 APPENDIX B AccuPyc 1330 B 2 September 1996 ...

Page 95: ...n 12 then becomes the working equation for the pycnometer Calibra tion procedures are provided to determine VCELL and VEXP and the pressures are measured by a gauge pressure transducer Provisions are made for conven iently charging and discharging gases at controlled rates for optimizing the relative sizes of the sample chambers and expansion volumes and for cleans ing the samples of vapors which ...

Page 96: ...APPENDIX C CALIBRATION THEORY ...

Page 97: ... pressure but sealed and that the valve is closed Upon opening the valve the condition established is P1 VCELL P2 VCELL VEXP 1 where P2 is the resulting intermediate pressure The use of gauge pressures is permissible because it is equivalent to having subtracted a constant from both sides of the equation Figure C 1 Simplified Diagram for Calibration Placement of VCALIB into VCELL and repetition of...

Page 98: ...n of equation 3 into equation 2 yields P1 VCELL VCALIB P2 VCELL VCALIB P2 VCELL P1 P2 P2 4 Gathering terms and solving for VCELL further yields VCELL VCALIB P1 P2 P1 P2 P2 P2 P1 P2 5 Substitution of experimental and known values into equation 5 yields VCELL which when used in equation 3 yields VEXP the desired result APPENDIX C AccuPyc 1330 C 2 September 1996 ...

Page 99: ...APPENDIX D FORMAT OF TRANSMITTED DATA ...

Page 100: ...Column Record Number Information Conveyed Form 1 Version number 20 characters 2 Serial number 1 integer 3 Report type calibration 11 characters 4 Start 4a Date 8 characters 4b Time 8 characters 5 Stop 5a Date 8 characters 5b Time 8 characters 6 Temperature 1 floating point 7 Calibration standard size 1 floating point 8 Number of purges 1 integer 9 Equilibration rate 1 floating point 10 Average cel...

Page 101: ...ure D 1 Single Column Format AccuPyc 1330 VX XX 625 Calibration 18 08 92 07 59 43 18 08 92 08 22 48 25 799398 6 371870 3 0 005000 12 247808 0 000417 8 432275 0 000547 3 19 580629 19 564293 19 553852 11 296484 11 587052 11 580896 19 627428 19 618446 19 600245 8 060401 8 056624 8 049247 1 1 1 APPENDIX D AccuPyc 1330 D 2 June 1997 ...

Page 102: ...e 1 floating point 11 Cell volume standard deviation 1 floating point 12 Average expansion volume 1 floating point 13 Expansion volume standard deviation 1 floating point 14 Number of runs 1 integer 15 Carriage return line feed 16 Carriage return line feed 17 Carriage return line feed 18 Run number and pressure reported on one line as ASCII comma delimited data 18a Run number 1 integer 18b P1 1 fl...

Page 103: ...1870 3 0 005000 12 247808 0 000417 8 432273 0 000547 3 1 19 580629 11 296484 19 627428 8 060401 1 12 248280 0 000472 8 432904 0 000631 2 19 564293 11 587052 19 618446 8 056624 1 12 247489 0 000319 8 431926 0 000347 3 19 553852 11 580896 19 600245 8 049247 1 12 247654 0 000154 8 431990 0 000283 APPENDIX D AccuPyc 1330 D 4 June 1997 ...

Page 104: ...ate 1 floating point 11 Cell volume 1 floating point 12 Expansion volume 1 floating point 13 Average volume 1 floating point 14 Volume standard deviation 1 floating point 15 Average density 1 floating point 16 Density standard deviation 1 floating point 17 Number of runs 1 integer 18 Run precision 0 Disabled 1 Enabled 1 integer 19 Percent full scale 1 floating point 20 P1 all P1 data 1 floating po...

Page 105: ...Analysis 18 08 92 07 12 41 18 08 92 07 20 19 25 7685642 6 10 97 12 57 40 5110 3 0 005000 12 249167 8 432934 6 372971 0 000332 0 000000 0 000000 3 0 0 050000 19 570705 19 555931 19 544651 8 037209 8 030797 8 025983 0 0 0 145 250 352 APPENDIX D AccuPyc 1330 D 6 June 1997 ...

Page 106: ...n rate 1 floating point 11 Cell volume 1 floating point 12 Expansion volume 1 floating point 13 Average volume 1 floating point 14 Volume standard deviation 1 floating point 15 Average density 1 floating point 16 Density standard deviation 1 floating point 17 Number of runs 1 integer 18 Run precision 0 Disabled 1 Enabled 1 integer 19 Percent full scale 1 floating point 20 Carriage return line feed...

Page 107: ...Format for Analysis AccuPyc 1330 VX XX 625 Analysis 18 08 92 07 12 41 18 08 92 07 20 19 25 685642 6 10 97 12 57 40 5110 3 0 000000 0 005000 12 249167 8 432934 6 372971 0 000332 0 000000 0 000000 3 0 0 050000 1 19 570705 8 037209 0 145 6 372611 0 000360 0 000000 0 000000 2 19 555931 8 030797 0 250 6 373038 0 000067 0 000000 0 000000 3 19 544651 8 025983 0 352 6 373264 0 000293 0 000000 0 000000 APP...

Page 108: ...APPENDIX E PRINTER CHARACTER SET ...

Page 109: ...hat your printer supports these characters Decimal Value Character Decimal Value Character 33 59 34 60 35 61 36 62 37 63 38 64 39 65 A 40 66 B 41 67 C 42 68 D 43 69 E 44 70 F 45 71 G 46 72 H 47 73 I 48 0 74 J 49 1 75 K 50 2 76 L 51 3 77 M 52 4 78 N 53 5 79 O 54 6 80 P 55 7 81 Q 56 8 82 R 57 9 83 S 58 84 T AccuPyc 1330 APPENDIX E September 1996 E 1 ...

Page 110: ...9 m 87 W 110 n 88 X 111 o 89 Y 112 p 90 Z 113 q 91 114 r 92 115 s 93 116 t 94 117 u 95 _ 118 v 96 119 w 97 a 120 x 98 b 121 y 99 c 122 z 100 d 123 101 e 124 102 f 125 103 g 126 104 h 129 ü 105 i 132 ä 106 j 164 ñ 107 k 225 ß APPENDIX E AccuPyc 1330 E 2 September 1996 ...

Page 111: ...INDEX ...

Page 112: ...nging the analysis module A 1 Checking for leaks 5 16 Cleaning the pycnometer 5 21 Cylinder shut off valve 2 4 D Damaged or lost equipment 2 1 Data bits editing the parameters 4 26 Data transmission parameters editing 4 26 Date setting 4 27 Default values 2 8 Density sample weight required for 4 6 Dewpoint specification for gases 1 7 E Editing analysis and calibration parameters 4 19 calibration r...

Page 113: ...eue 4 3 Minimum helium tank pressure 2 3 Monitoring the system 4 1 N Notes 1 1 Number of purges editing parameters 4 19 system default 2 8 Number of runs editing parameters 4 19 system default 2 8 O O ring 5 15 replacing 5 15 ON turning the instrument ON 2 7 P Parallel port printer location 2 5 Parity editing the parameters 4 26 Percent full scale editing the parameters 4 21 system default 2 8 Per...

Page 114: ...9 4 27 units of measurement 2 9 Serial Port RS 232 2 5 Setup parameters editing 4 18 Shut off valve A 1 Single column report format 4 14 Software card installing 2 6 Specifications 1 7 Spreadsheet report format 4 14 Starting a calibration 4 15 Starting an analysis using default parameters 3 4 using defaults 3 4 using modified parameters 3 4 Status messages 4 1 5 5 Stop bits editing the parameters ...

Page 115: ... Warm up period 2 7 Warnings 1 1 Weighing the sample 3 2 X Xon Xoff 4 26 Z Zero function defined 1 3 Zero pressure offset 1 3 Zeroing the pressure transducer 4 16 Index AccuPyc 1330 Index 4 January 1999 ...

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