AccuPyc 1330

Quick Reference Guide

(mtmicromeritics" -----'
USING THE KEYS

To select the primary To select the alternate

function on the face of - - - - function printed above
the key, press only that the key, fIrst press the
key. For example: _ _ __ white key, then press
press l ir· l to enter the kiY' For Ip~Ts"l;:.1
the number 6. press""" """
to print areport.

STANDARD KEYS - - - - - - - - - - - - - - - - - - -

Enter the numbers 0 through 9.

Enter a decimal point or a dash for sampie ID.

Complete an entry or begin an action.

Display the next message when in display mode. Display the

next multiple choice item when in a command mode.

Clear a message when in display mode. Clear an entry when

in a command mode.

Save the information you entered and return to display mode.

Change the keypad mode. The keypad may be used in either

primary function mode or alternate function mode.

When you press the white key to enter alternate function

mode, a plus sign (+) appears in the upper right corner of
the displayand the commands written above the keys
become available.

To exit alternate function mode, press the white key again.

The plus sign (+) will be removed from the display.
KEYCOMBINATIONS-------------------

ZERO ,----------,11Hol Zero the pressure transdueer.

CALIBRATE '----------'I li~ nl Calibrate the pyenometer.

MANUAL Manually eontrol the valves. Mter pressing

the Manual key, you may use the FILL,
EXPAND, and VENT keys to open and
c10se the valves.

SET UP Display or edit analysis parameters, report

options, calibration volumes, data transmis-
sion parameters, unit types, and operating
language.

TRANSMIT Transmit analysis or calibration data over the

serial line. If an automatie operation is in
progress, transmit a partial report.

ESCAPE Delete all data entered in the eurrent mode

and return to display mode. If an automatie
operation is in progress, eancel it.

ANALYZE I I i! i l Perform an analysis.

REVIEW I I (i! ( I Review or edit eompleted analysis or calibra-

tion data.

PRINT I I i! nil Print analysis or ealibration report. If an auto-

matie operation is in progress, print a partial
report.

FILL I i7il Open and c10se the fill valve. The indieator
(when in above the FILL key is on when the valve is
Manual Mode) open and off when the valve is elosed.

EXPAND kIä'l Open and c10se the expansion valve. The

(whenin indicator above the EXPAND key is on
Manual Mode) when the valve is open and off when the
vaIVe is c1osed.

VENT l /g .Il Open and c10se the vent valve. The indicator
(when in above the VENT key is on when the valve
Manual Mode) is open and off when the valve is elosed.
PERFORMING AN ANALYSIS - - - - - - - - - - - - - - - -

1. Weigh the empty sampie cup and record the weight

2. Place sampie in the cup and dry it thoroughly in an oven.

3. After preparing the sampie. weigh the cup and sampie and record the weight. Subtract
the empty sampie cup weight from the sampie cup plus sampie weight to determine the
sampie weight Record the sampie weight.

4. Remove the cell chamber cap.

5. Insert the sampie cup into the cell chamber and replace the cell chamber cap.

6. Press IL_-----'I [ @liNnonthepycnometerkeypad.

7. If Sampie ID is displayed. enter the ID and press lEl'tltill. If not, skip to step 8.
8. If Sampie Weight is displayed. enter the weight and press l'Ii!rtli'~I. If not. skip to step 9.

9. Press IEl'tltä I to start the analysis.

10. As the analysis is perforrned. status messages are displayed. When the analysis is com-
plete. the pycnometer beeps three times. Remove the sampie from the cell chamber.

11. The Reload prompt is displayed. Press tooolOEI to cycle through the error messages and
repon data.

CHANGING THE OPERATING LANGUAGE - - - - - - - - - - - - -

1. If an automatie operation is in progress. wait until it is complete.

2. Press _---'lljjwill
LI to return to display mode if you are in another mode of operation.

3. Press L.I_-,lllmä:;nI.

4. Press ICHOlCEI until Unit type? is displayed.

5. Press I mll~1 until Language? is displayed.

6. Press I~I until the desired language is displayed. Then press 1: ~AYl!) I.

Part No. 133-429()3.()()

 ACCUPYC 1330

Kurzbedienungsanleitung

'---- Iffif micromeritics~

Benutzung der Tastatur Um die zweite Tasten-Belegung
zu aktivieren, die über der
Um die Standard-Belegung zu jeweiligen Taste angegeben ist,
erhalten, drücken Sie die Taste drücken Sie die weiße Taste und
mit dem entsprechenden anschließend die gewünschte
Symbol-Aufdruck. Funktionstaste.
Zum Beispiel: Drücken Sie Zum Beispiel: Drücken Sie
D:::J ,um die Zahl ,,6" c==J D:::J, um ein Meßproto-
einzugeben. koll ausdrucken zu lassen.

Standard-Belegung

Taste Wirkung

Eingabe der Ziffern 0 - 9.

Dezimal-Punkt oder Bindestrich bei der

Eingabe der Proben bezeichnung.

I ENTERI Beenden der Eingabe oder Starten einer

(Eingabe) Messung.

ICHOiCIj Auswahl der nächsten Meldung im Anzeige-

(Auswahl) Modus, Anzeigen der nächsten Auswahlmög-
lichkeit im Programmier-Modus.

I CLEARI Löschen einer Meldung im Anzeige-Modus

(Löschen) oder einer Eingabe im Programmier-Modus.

I SAYE I Sichern der eingegebenen Angaben und

(Sichern) Rückkehr in den Anzeige-Modus.

Wechsel der Tastatur-Belegung zwischen

Standard- und Kombinationsbelegung. Die
Tastatur kann in einem der bei den Modi
betrieben werden.
Nach dem Drücken der weißen Taste erscheint
ein Plus-Zeichen (" +") in der oberen rechten
Ecke der LCD-Anzeige und die über den
Tasten angebrachte Belegung wird wirksam.
Durch erneutes Drücken der weißen Taste wird
das Plus-Zeichen gelöscht und die Standard-
belegung wird wirksam.
Tasten-Kombinationen

Funktion Tasten Wirkung

NULL.abgleich c:::J c::I:J Nullabgleich des Druckaufnehmers.

CAL.ibrieren Starten des Kalibrationsprogramms.

MANUELL Manuelle Bedienung der drei Ventile. Nach dem

Drücken dieser Tastenkombination können die
drei Tasten der ersten Reihe benutzt
werden (s. unten).

SETUP Anzeigen oder Ändern der voreingestellten

(Voreinstellungen) Analysenbedingungen, der Protokoll-Optionen,
der Kalibrations-Volumina, der verwendeten
Druckeinheit oder der Bedienungs-Sprache.

SENDEN c:::J o::J Übertragen von Analysen- oder Kalibrations-

Daten über die serielle Schnittstelle. Wenn eine
automatische Messung läuft, wird ein Teilbericht
gesendet, ohne die Messung zu unterbrechen.

ESCAPE c:::J I CLEAR I Löschen aller eingegebenen Daten in der g\lrade

(Verlassen) gewählten Funktion und Rückkehr in den An-
zeige-Modus (Gegenteil von ENTER). Wenn
eine automatische Messung läuft, wird sie
abgebrochen.

ANALYS.ieren c:::J ~ Beginn einer automatischen Messung.

EDIT c:::J c::::I=:J Editieren einer beendeten Messung oder der

(Verändern) Kalibrationsdaten.

DRUCKEN c:::J c::::I=:J Drucken eines Analysen- oder Kalibrations-

Protokolls über die parallele Schnittstelle.
Wenn eine automatische Messung läuft, wird
ein Teilbericht gedruckt, ohne die Analyse zu
unterbrechen.

Tasten der oberen Reihe (Orange-farbene Beschriftung):

Aktiv, wenn die manuelle Betriebsart eingestellt ist (c:::J MANUELL):

FÜLLEN o::J Öffnen und Schließen des Füll-Ventils.

EXPAND.ieren CCJ Öffnen und Schließen des Expansions-Ventils.

BELÜFTEN CCJ Öffnen und Schließen des Belüftungs-Ventils.

Die Leuchtdiode über der jeweiligen Taste leuchtet auf, wenn das betreffende
Ventil geöffnet ist und erlischt nach dem Schließen.
Durchführen einer Analyse

1. Wiegen Sie den leeren, sauberen Proben becher.

2. Füllen Sie die Probe in den Becher und trocknen Sie sie gründlich.

3. Die vorbereitete, abgekühlte Probe wird mit dem Probenbecher erneut

gewogen. Die Differenz zwischen diesem Gewicht und dem leeren Becher
ergibt die Einwaage (nur für Dichtebestimmung erforderlich).

4. Öffnen Sie die Probenkammer.

5. Setzen Sie den Probenbecher ein und verschließen Sie die Probenkammer.

6. Drücken Sie die Tastenkombination für ANALYS.ieren (c::::::J ~)

7. Wenn die Probenbezeichnung erfragt wird, geben Sie sie über die Tastatur
ein und drücken ! ENTER!. Wenn nicht, weiter bei Punkt 8.

8. Wenn das Probengewicht erfragt wird, geben Sie es über die Tastatur ein
und drücken ! ENTERI Wenn nicht, weiter bei Punkt g.

g. Drücken Sie ! ENTER! zum Starten der Analyse. Mit ESCAPE (c::::::J !CLEAR!)
kann abgebrochen werden.

10. Während der Analyse werden auf der LCD-Anzeige Statusmeldungen

angezeigt. Das Ende der Messung wird durch drei helle Töne signalisiert.
Entfernen Sie die Probe aus der Probenkammer.

11. Die Meldung "NEULADEN" wird angezeigt. Drücken Sie mehrmals

!CHOIC!l (Auswahl), um eventuell vorhandene Fehlermeldungen sowie die
Meßdaten auf der LCD-Anzeige anzuzeigen.

Ändern der Bedienungssprache (Englisch -+ Deutsch)

1. Warten Sie das Ende einer laufenden automatischen Messung ab.

2. Stellen Sie mit ESCAPE (c::::::J !CLEAR!) den Anzeige-Modus ein.

3. Drücken Sie SET UP (c::::::J c::I::l).

4. Drücken Sie CHOICE, bis die Anzeige "Unit Type" erscheint.

5. Drücken Sie ENTER, bis "Language?" erscheint.

6. Drücken Sie CHOICE, bis die gewünschte Sprache angezeigt wird.

7. Drücken Sie SAVE; die LCD-Anzeige zeigt die Aufforderung "Neu laden" an.
lffif'micromeritics@

AccuPyc 1330 Pycnometer

Operator's Manual

Part Number: 133-42801-01

22 August 1990
 WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instru-
ment manufactured by it to be free from defects in material and workmanship impairing its usefu1ness under normal
use and service conditions except as note<! herein.

Our liability under this warranty is limite<! to repair, servicing and adjUSbnent, free of charge at our plant, of any instru-
ment or defective parts, when returned prepaid to us, and wbich our examination discloses to have been defective. The
purchaser is responsible for a11 transportation charges involving the sbipment of materials for warranty repairs. Failure
of any instrument or product due to operator error, improper installation, unauthorized repair or alteration, failure of
utilities, or environmental contamination will not constitute a warranty claim. The Materials of construction used in
MICROMERITICS instruments and o!her products were chosen after extensive testing and experience for !heir
reliability and durability. However, these materials cannot be totally guaranteed against wear and/or decomposition by
chemical action (corrosion) as a result of normal use.

Repair parts are warrante<! to be free from defects in material and workmansbip for 90 days from the date of shipmenL

No inslrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authoriza-
tion to return the inslrument or product. All repairs or replacements are made subject to factory inspection of returned
parts.

MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are
made by persons other than its own authorized service personnel unless such work is authorized in writing by
MICROMERITICS.

The obligations of this warranty will be limite<! under the following conditions:

1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under!heir respec-
tive brand narnes or Irade narnes. We, therefore, make no express or irnplied 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 bis products that may prove defective in workmanship or materials. Service charges
made by such manufacturer are the responsibility ofthe ultimate purchaser. This states ourentire liability in respect
to such products, except as an authorized person of MICROMERITICS may otherwise agree to in writing.

2. If an instrument or product is found defective during the warranty period, replacemenl parts may, al the discre-
tion of MICROMERITICS, be sent to be instalied by the purchaser, e.g., printe<! circuit boards, check valves,
seals, etc.

3. Expendable items, e.g., sarnple tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and stems,
seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such items
which perforrn satisfactorily during the first 45 days after the date of shipment are assumed to be free of manufac-
turing defects.

Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against
MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufac-
tures a special product to the purchaser' s specifications.

MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its
products other than the liability state<! above. This warranty is in lieu of allother warranties, express or irnplied, includ-
ing, but not limite<! to the implied warranties of merchantability or fitness for use.

One Micromeritics Drive • Norcross, GA 30093-1877 • Telex: 682-7018

Domestic Sales - (404) 662·3633 Domestic Repair Service - (404) 662-3666
International Sales - (404) 662·3660 Customer Service - (404) 662-3636

Form No. ~l04-OO

280d 1988
AccuPyc 1330 TABLE OF CONTENTS

Table of Contents

1. GENERAL DESCRIPTION

Organization of the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

Equipment Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Pycnometer Keypad . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7

2. INSTALLATION

Unpacking and lnspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1

Equipment Damage or Loss During Shipment . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Equipment Return . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Selecting the Location . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Gas Requi,rements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Equipment Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Selecting the Input Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Rear Panel Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Turning on the Pycnometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-10
Entering Analysis and Report Parameters . . . . . . . . . . • . . . . . . . . . . . . . . . . 2-11
Selecting Units ofPressure Measurement and Operating Language . . . . . . . . . . . . . . 2-12
Greasing the ChamberCap O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
Verifying Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14

3. PERFORMING AN ANALYSIS

Setting Regulator Pressure .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

Preparing and Loading a Sampie . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Starting the Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Using the Default Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Using Modified Analysis Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
Viewing or Printing Analysis Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5

4. GENERAL OPERATING INSTRUCTIONS

Monitoring the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1

Status Messages Displayed During an Automatie Operation . . . . . . . . . . . . . . . . . . 4-1
Error and Report Messages .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3

15 Dec 89
TABLE OF CONTENTS AccuPyc 1330

Canceling an Automatie Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-4 a

Entering Commands . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-5 '. .
Perfonning an Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-6
Reviewing and Editing Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-7
Reviewing and Editing Analysis Results and Parameters . . . . . . . . . . . . . . . . .4-7
Reviewing and Editing Calibration Results and Parameters ...............4-8
Printing Repons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-9
Transmitting Repons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-13
Calibrating tbe Pyenometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-14
Zeroing tbe Pressure Transdueer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-15
Manually Controlling tbe Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-16
Editing tbe Set-Up Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-17
Analysis or Calibration Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-18
Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 - 2 1
Calibration Volumes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-23
Data Transmission . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 - 2 4
Unit Types and Operating Language . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-25

5. TROUBLESHOOTING AND MAINTENANCE

Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Error and Status Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 - 4
Queued Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 - 4
Messages Displayed During an Automatie Operation . . . . . . . . . . . . . . . . . . . . . 5-10
Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-12
Greasing tbe Chamber Cap O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 - 1 2
Replaeing tbe Chamber Cap O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-13
Cheeking tbe Cell and Expansion Chambers for Leaks . . . . . . . . . . . . . . . . . . . . . 5-15
Cleaning tbe Pyenometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 - 1 7
Recovering from aPower Failure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17
Replaeing Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 - 1 7

6. ORDERING INFORMATION

APPENDICES

Appendix A: Changing tbe Analysis Module

Appendix B: Analysis Theory
Appendix C: Calibration Theory
Appendix D: Format of Transmitted Data

ii 15 Dec 89
 CHAPTER 1

GENERAL DESCRIPTION

• Organization of the Manual

• Equipment Description

• Pycnometer Keypad

• Specifications
AccuPyc 1330 GENERAL DESCRIPTION

GENERAL DESCRIPTION

ORGANIZATION OF THE MANUAL

This manual describes how 10 iosta1l, operate, and maintain the AccuPyc 1330 Pycnometer. The
manual is divided into six chapters.

Chapter 1 Provides a general description and specifications of the pycnometer.

Chapter 2 Provides unpacking and iospection information, and iosta1lation iostructioos.

Chapter 3 Provides iostructioos for performing an analysis.

Chapter 4 Provides detailed operating iostructioos.

Chapter 5 Provides troub1eshooting and maintenance procedures and error messages.

Chapter 6 Provides information on ordering parts and accessories for the pycnometer.

Several appendices are also inc1uded.

EQUIPMENT DESCRIPTION
The AccuPyc 1330 Pycnometer is an easy-to-use, fully-automatic gas displacement pycnometer.
Analyses are initiated with a keystroke. Once an analysis is initiated, data are collected, calcula-
tions performed, and results displayed without further operator intervention. The pycnometer may
be operated in any of four languages: English, German, Spanish, or French. The language used
may be changed by a simple keystroke sequence.

The AccuPyc 1330 Pycnometer's unique run precision feature increases the precision of analysis
results by reporting data from five consecutive runs that are within a user-specified tolerance.
This feature allows early termination of analyses, thereby decreasing the number of runs needed
for accurate results.

The AccuPyc 1330 Pycnometer, shown in the following illustration. contaios 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 continu-
ally monitored on the display. The optional printer prints out complete analysis and calibration re-
sults. In addition. aserial port is provided for data transmission 10 other devices.

15 Dec 89 1-1
GENERAL DESCRIPTION AccuPyc 1330

Cell Chamber Cap Display Area

Keypad

Figure 1-1. AccuPyc 1330 Pycnometer

The AccuPyc 1330 Pycnometer determines density and volwne by measuring the pressure change
of heliwn in a calibrated volwne. The schematic diagram. which is included above the keypad.
indicates system status. The three indicators show the current state of the fill. expansion, and
vent valves. The indicator is lit when a valve is open.

Gell Chamber Expansion Chamber

1 /

Fill Valve Expansion Vent Valve

Indicator Valve Indicator Indicator

Figure 1-2. Schematic Diagram

1-2 15 Dec 89
AccuPyc 1330 GENERAL DESCRIPTION

In addition to analysis, there are two other automatie operations performed by the pyenometer:
calibration and transducer zero reset.

Analysis measures sampIe volume, from which density ean be derived automatically if sampIe
weight has been entered. The unit comes pre-programmed with default conditions and ready to
perform analyses. It ean be easily reprogrammed to meet your speeifie needs. You ean modify
your own analyses by entering the following parameters: number of purges, purge fill pressure,
number of runs, run fill pressure, equilibration rate, and run precision. The run precision option
allows early termination of the analysis if the last five runs are all within a user-specified toler-
anee. By modifying these parameters, you retain control over the two main sections of the analy-
sis: purge and run.

A purge is used strietly for sampIe clean up and air and moisture removal from the ehamber's in-
side. It is aecomplished by c10sing off the pyenometer bloek and filling the cell chamber to the
designated purge fill pressure. The ehambers are then vented to atmosphere, resulting in elimina-
tion of water vapor or other contaminants. A run is used for eollecting the preeise, accurate data
used in repon caleulations.

Calibration is used to determine the size of the eell and expansion chambers within the instru-
ment. After ealibration, the cell and expansion ehamber volumes are automatically stored in the
set-up parameters.

The zero funetion is used to caleulate a new zero pressure offset. It is measured when the system
is at atmospherie pressure and thermal equilibrium and is subtraeted from all subsequent pressure
readings in order to obtain a true gauge pressure.

22 Aug 90 1-3
GENERAL DESCRIPTION AccuPyc 1330

PYCNOMETER KEYPAD

FlLL EXPAND VENT

ANALVZE REVIEW PRINT

o
MANUAL SETUP TRANSMIT ESCAPE

ZERO CALIBRATE

Figure 1-3. Pycnometer Keypad

Most keys on the keypad perfonn one primary and one alternate funetion. The primary funetion
of any key is indieated by the number or command on the face of the key. The alternate funetion
is indieated by the command above the key.

To se1eet the alternate funetion printed above the key,

P R I NT - - lfirst Pi~.I............. I, ~en press the key. For examp1e: press
L. ... .6.........J to poot. Refer to Tab1e 1-2.
I ___ To seleet the primary funetion on the face of the key,
........... press only that key. For examp1e: press niilllIl to enter
the number 6. Refer to Tab1e 1-1.

1-4 15 Dec 89
ACcuPyc 1330 GENERAL DESCRIPTION

Tables I-I and 1-2 describe how the keys are used to control and monitor the pycnometer.

Table 1-1. Standard Keys

Enter the numbers 0 through 9.

Enter a decimal point or a dash for sampie ID.

Complete an entry or begin an action.

lellöl~1 Display the next message when in display mode. Display the next
multiple choice item when in a command mode.

Clear a message when in display mode. Clear an entry when in a

command mode.

Save the information you entered and return to display mode.

Change the keypad mode. The keypad may be used in either pri-
mary function mode or alternate function mode.

When you press the white key to enter alternate function mode, a
plus sign (+) appears in the upper right corner of the displayand
the commands written above the keys become available.

To exit alternate function mode, press the white key again. The
plus sign (+) will be removed from the display.

15 Dec 89 1-5
GENERAL DESCRIPTION AccuPyc 1330

Tabte 1-2. Key Combinations

ZERO Zero the pressure transducer.

CALffiRATE Calibrate the pyenometer.

MANUAL Manually contral the valves. After pressing the

Manual key, you may use the PUL, EXPAND,
and VENT eommands to open and elose the
valves.

SEfUP Display or edit analysis parameters, repon

. options, ealibration volumes, data transmission
parameters, unit types, and operating language.

TRANSMIT Transmit analysis or ealibration data over the

serial line. If an automatie operation is in prog-
ress, transmit a partial repon.

ES CAPE Delete a1l data entered in the eurrent mode and

return to display mode. If an automatie opera-
tion is in progress, eancel the operation.

ANALYZE Perform an analysis.

REVIEW Review or edit completed analysis or ealibration

data.

PRINT Print analysis or ealibration report If an auto-

matie operation is in progress, print a partial
report

FILL )7:il (when in Open and elose the fill valve. The indicator
manual above the FILL key is on when the valve is
mode) open and off when the valve is elosed.

EXPAND I ;)'III\tl (when in Open and elose the expansion valve. The indica-
manual tor above the EXPAND key is on when the
mode) valve is open and off when the valve is elosed.

VENT lJ :1 (when in Open and elose the vent valve. The indicator
manual above the VENT key is on when the valve is

1-6
mode) open and off when the valve is elosed.

15 Dec 89
•
ÄCCUPyc 1330 GENERAL DESCRIPTION

SPECIFICATIONS

Tab1e 1-3. AccuPyc 1330 Pycnometer Speci(lCations

Temperature Stable between 15 and 35 °C (59 to 96 0F)

Humidity 20 to 80% relative, non-eondensing

Vo1tage 100/120 or 220/240 VAC ±1O%

Current 0.5A (100/120 VAC); 0.25A (220/240 VAC)

Frequeney 50/60 Hz

Sample Volume 0.5 - 100 mL

Standard Sample Holder 19 mm OD x 39.8 mm long x 0.254 mm wall (0.750 in. OD x

1.570 in. long ±O.OO5 in. x omo in. wall) for standard (10 mL)
holder

Optional Sample Modules Provide ranges of 1 to 100 mL

Precision Reprodueibility typieally to within ±O.OI % of the nominal full-

seale ce11 ehamber volume. * Reproducibility guaranteed to within
±O.02% of the nominal full-seale volume on clean, dry, thermally
equilibrated samples.

Aeeuraey Aeeurate to within 0.03% of reading plus 0.03% of nominal full-

seale ce11 ehamber volume. *

Cabinet 311 mm W x 173 mm H x 357 mm D

(12 in. W x 7 in. H x 14 in. D)

Gases . Research grade helium is recommended. If unavailable, use helium

with a dewpoint of -67 °C (-88 0F) or lower.

*Nominal full-seale ee11 ehamber volume is the samp1e eapaeity..

15 Dec 89 1-7
 CHAPTER 2

INSTALLATION

• Unpacking and Inspection

• Selecting the Location

• Gas Requirements

• Equipment Setup

• Verifying Operation
AccuPyc 1330 INSTALLATION

INSTALLATION

This chapter describes how to unpack, inspect, and install the AccuPyc 1330 Pycnometer.

UNPACKING AND INSPECTION

When you receive the shipping cartons, carefully compare the Packing List with the equipment
actually received and check the equipment for any damage during shipment. Be sure to sift
through all packing materials before declaring equipment missing.

NOTE
If you need to declare equipment as damaged or lost, save the
shipping cartons. The claims investigator must examine the cartons
in order to cornplete 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 oc·
curling during shipment. If you discover damage or loss of equipment during shipment, repon
the condition to the carrier immediately.

EQUIPMENT RETURN

Micromeritics strives to ensure that all items arrive safely and in working order. Occasionally,
due to circumstances beyond. our control, a customer may receive equipment which is not in
working order. When equipment has been damaged (either during shipment or in use) and you
wish to return \he equipment to Micromeritics for repair or replacement, please follow the steps
below:

1. Tag or otherwise identify the defective equipment, noting the defect and, if possible, the cir-
cumstances under which the defect occurs.

2. Make reference to the sales order 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 instruc-
tions. The Service Department will assign a Return Material Authorization (RMA) number to
your retum and provide shipping information.

15 Oec 89 2·1
INSTALLATION AccuPyc 1330

SELECTING THE LOCATION

When seleeting the loeation of the pyenometer. keep the following in mind:

• The pyenometer performs best in a eonstant temperature environment.

• It should be installed on a workbeneh about 36 in. high in a loeation free of drafts from
either a foreed-air heating or eooling system.

• The slots in the baseplate. which provide ventilation. should not be blocked.

• The pycnometer should not be placed near a wiodow; exposure to sunlight may cause the
temperature to vary.

GAS REQUIREMENTS
The pyenometer uses helium (99.995% pure or better) to provide rapid. aeeurate analyses. The
eylioder eontaioiog helium must be fitted with a gas regulator and the regulator set for 15 to 23
psig (we reeommend 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 proteetion deviee contained in the
pyenometer that vents the pyenometer to atmospherie pressure if pressure exeeeds 25 psig.

2-2 15 Dec 89
AccuPyc 1330 INSTALLATION

EQUIPMENT SETUP
The pycnometer should be checked to make sure it is operating properly before actual analyses
are anempted. The remainder of this chapter describes how to install the pycnometer and verify
operation.

SELECTING THE INPUT POWER

All instruments leave the factory set for 120 VAC and with the line fuse removed. The correct
setting of the universal power entrance must be checked and the appropriate fuse installed before
the pycnometer can be operated. The pycnometer is designed to operate with either 100. 120. 200
or 240 VAC at 50 or 60 Hz. Voltage selection and fusing are made at the power connector.
which is located on the rear panel of the unit

1. Make sure the power cord is disconnected from the pycnometer.

2. Using a pointed object, remove the fuse block and cover assembly from the power connec-
tor at the rear of the pycnometer.

Pointed Object Fu.e Block and

Cover A.&embly

/ I
OtW( VlITH
.US e FU SES
250 V

Figure 2-1. Removing Fuse Block and Cover Assembly

15 Dec 89 2-3
INSTALLATION AccuPyc 1330

3. Pull the voltage selector card straight out of the power connector housing.

Pointed Objsct _ _ _ _ __

Figure 2-2. Removing Voltage Selector Card

4. Orient the voltage selector card so that the desired voltage is indicated at the bottom. Orient
the indicator pin so that it points upward as shown in the following illustration.

100V 120" 220V 240V

Figure 2-3. Voltage Selection

2-4 15 Dec 89
AccuPyc 1330 INSTALLATION

5. Insert the voltage selector card into the power connector housing with the edge containing
the desired voltage first and with the printed side facing the POWER ON/OFF switch.

Voltage Seleetor
Card

Figure 24. lnserting Vo1lllge Selector Card

6. Fuse the input power line according to loeal safety practices. The input power connector can
be used with either a single-fuse arrangement or a double-fuse arrangement, as shown in the
following illustration.

FUße Block

~_~=:::::!:!::==>~cover

~~
Cover _ __ "- FUGe
DOUBLE-FUSE ARRANGEMENT SINGLE-FUSE ARRANGEMENT

Figure 2-5. Fusing Arrangements

15 Dec 89 2-5
INSTALLATION AccuPyc 1330

a. Observe the position ofthe fuse block, using Figure 2-5 for reference. Ifthe single-fuse ar-
rangement is desired, the fuse block should be positioned such that the side with the single
fuse slot and the jumper bar is away from the cover.

Ifthe double-fuse arrangement is desired, the fuse block should be positioned such that the
side with the double fuse slots is away from the cover.

b. If the fuse block is positioned properly for the fusing desired, proceed to Step c.

If the fuse block is not positioned properly for the fusing desired:

1. Remove the fuse block retaining screw.

2. Lift the fuse block from the cover.

3. Rotate the fuse block.

4. Mount the fuse block to the cover.

5. Replace the retaining screw.

c. Insert appropriate fuse(s) for the input power source. Refer to the chart below for the appro-
priate fuse rating.

Power Source Fuse

100-120VAC 0.5 Amp Slo-Blo

220-240VAC 0.25 Amp Slo-Blo

2-6 15 Dec 89
AccuPyc 1330 INSTALLATION

7. Insert fuse block and cover assembly into input power connector and snap it into place.
Once the fuse block and cover assembly are in place. the position of the indicator pin shows
the input power selected.

Voltage Indicator Pin

Indicator Pin
Visible Here

fOOY 0
Use ONLY WITH ,20Y 0
250V FUSES ZZOY 0
NEer FOWER Z40V
OISCOH,PLAClN6 FUSE5
BeF"R~ R

Figure 2-6. Inserting Fuse Block anti Cover Assembly

15 Dec 89 2-7
INSTALLATION AccuPyc 1330

REAR PANEL CONNECTIONS

1. Anach an appropriate regulator to the gas supply cylinder. Leave the gas cylinder shut-off
valves closed until instructed otherwise.

Two-Stage Pressure
Reducing Regulator

&jO Regulator
Gas Cylinder

~y
~ B~Reducer Fitting
Shut-Off Valve

Copper
Tubing

Figure 2-7. Connecting Gas Supply Cylinder to the Regulator

2. Anach the supplied brass reducer fitting to the outlet of the regulator shut-off valve.

3. Turn the shut-off valve nut clockwise until it is finger tight. Then use a 9/16-in. open-ended
wrench (or an adjustable wrench) to tighten the nut an additional 1/4 turn.

2-8 15 Oec 89
AccuPyc 1330 INSTALLATION

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/l6-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 INLEf connector on the back
of the pycnometer.

Parallel
Printer

AccuPyc 1330

Pycnomete:r~~~~~~~~~~~~~

Gas Cylinder

Figure 2-8. Rear Panel Connections

7. Turn the nut on the tubing cJockwise until it is finger-light Then use a 7/16-in. open-ended
wrench (or an adjustable wrench) to tighten the nut an additional 1/4 turn.

8. A port labeled VENT is provided on the rear panel. If you are using a gas other than helium
and wish to vent the system, use this port Connect one end of 1/8-in. ID flexible tubing to
the rigid tubing labeled VENT and the other end to a venting system.

9. If aserial line is to be used for data transmission, connect one end of the RS-232 cable to
the connector labeled SERIAL 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 PARAlLEL on the back of
the pycnometer. Connect the other end to the input connector on the printer.

11. Plug in the printer power cord and the pycnometer power cord.

22 Aug 90 2-9
INSTALLATION AccuPyc 1330

TURNING ON THE PYCNOMETER

To turn on the pycnometer. plaCt< the power ON/OFF switch on the rear panel in the ON ( I )
position. The system is automaticaIly vented and the following prompt is displayed:

Reload is displayed on the first line. indicating that the system is idle. The current pressure is
shown on the second line. There may be messages containiog the results of a previous analysis
or the status of the pycnometer. If there are any error messages. an asterisk appears in the right
corner of the first line. When this occurs. press I~~I to display the first message. Continue
pressing li$ölCiiI to cycle through aIl messages and return to the Reload prompt.

NOTE
When the system is turned on the first time or after aperiod 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.

2·10 15 Dec 89
•
ACcuPyc 1330 INSTALLATION

ENTERING ANALYSIS AND REPORT PARAMETERS

The pycnometer is shipped with the following default values for analysis parameters:

Number of purges 3
Purge fill pressure 19.5 psig
Number of runs 3
Run fill pressure 19.5 psig
Equilibration rate 0.005 psig/min

If you wish to 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 options:

Request sample ID no
Analysis display mode volume
Report destination display

If you wish to use these values. no further action is necessary. If you wish to change the values.
refer to Report Options in Chapter 4.

15 Dec 89 2-11
INSTALLATION AccuPyc 1330

SELECTING UNITS OF PRESSURE MEASUREMENT AND OPERATING LANGUAGE

The units of measurement for pressure may be displayed in pounds-per-square-inch gauge (psig)
or kilopascal gauge (kPag). In this manual, psig is used in the examples shown. The pycnometer
may be operated in any of four languages: English, Gennan, Spanish, and French. The default
for units is psig and the default language is English. If you wish to use these defaults, no further
action is necessary; proceed to Greasing the Chamber Cap O-Ring. If you wish to change the
defaults:

1. Press LI_-,I l~lI, then press !blji:lii!j\l until Unit types is displayed. Press 1;'Ri\ijI.
2. Press Icll!:jiCiil then I~] to change the value to kPag.

3. The Lanl!lJ. :~~~1mpt is displayed. Press Illlli:l!Cill until the desired language is displayed,
then press ...$Ä~lt. .

NOTE
If there are error messages in the message queue (indicated by an
asterisk next to the Reload prompt), delete the messages before
chan ging languages. Refer to "Error, Report,and System Status
Messages," Chapter 4. Make sure you press 1'!lAiiIiÜI after changing
languages.

4. Place the appropriate template (inc1uded in the accessory kit) over the pycnometer keypad.

2-12 15 Dec 89
•
AccuPyc 1330 INSTALLATION

GREASING THE CHAMBER CAP O-RING

A greasing disk is included in the accessory kit shipped with the pycnometer. Use the disk to
grease the O-ring as described below.

1. Remove the chamber cap by turning it counterclockwise then lifting off.

2. Using your fmgertip, apply a !hin layer of Dow Corning high vacuum grease (or equivalent)
to the greasing disko

3. Insert the greasing disk into the chamber cap and turn slightly to apply a very light coating
of grease to the O-ring.

Greasing
Disk

O-ring

Chamber
cap

Figure 2-9. Greosing the O-Ring in Chamber Cop

4. Replace the chamber cap.

15 Dec 89 2-13
INSTALLATION AccuPyc1330

VERIFVING OPERATION
Before perfOIming an analysis, verify that the pycnometer is operating properly by performing
tbe following steps.

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

10000.00

Note that aperiod is used to denote a decimal fraction. In some

languages, commas are used instead.

1. Zero the transducer by pressing LI_---'II}J!!']. The pressure display will show approxi-
mately zero.

2. Press I Ilitl on tbe keypad to enter manual mode.

3. Use the I Dfulll I, IEXPANi!I, and F~}I keys to elose 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.

2-14 15 Dec 89
•
AccuPyc 1330 INSTALLATION

FILL EXPAND VENT

ANALVZE REVIEW PRINT

o
MANUAL SETUP TRANSMIT ESCAPE

ZERO CALIBRATE

Figure 2-10. Front Panel

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

NOTE
Da not exceed 19!) psig. If the pressure exceeds 20 psig the transducer
may overrange and Im 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. elose 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.

15 Dec 89 2-15
INSTALLATION AccuPyc 1330

8. Observe the pressure display. After equilibration, the pressure should not vary more than
0.005 psig/min. Open the vent valve. After aperiod of time, the pressure should again stabi-
lize.

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

2-16 15 Dec 89
 CHAPTER 3

PERFORMING AN ANALYSIS

• Setting Regulator Pressure

• Preparing and Loading a Sampie

• Starting the Analysis

• Viewing or Printing Analysis Results

AccuPyc 1330 PERFORMING AN ANALYSIS

PERFORMING AN ANALYSIS

This chapter briefly describes how to perfonn an analysis. Chapter 4 describes in detail how
to use a1l the functions of the AccuPyc 1330 Pycnometer.

SETTING REGULATOR PRESSURE

Before beginning an analysis, check the regulator pressure. Fill pressure is separately speci-
fied for purge and run; set the regulator pressure at the higher of the two (plus about 2.0
psig) as folIows:

1. Press L..I_--,I WHli}1 to enter manual mode.

2. Press t tüV t l (EXPAND) and I'NIPpl (VENT) to open the expansion and vent valves. When
the valves are open, the indicators above the keys are turned on.

3. Press UV7ini') (FlLL) to open the fill valve.

4. Set the regulator pressure control knob on the cylinder to the desired pressure and then in-
crease it about 2.0 psig.

5. Press IWtt lU (FlLL) to close the fill valve.

6. Press [isiivit) to return to display mode.

15 Dec 89 3-1
PERFORMING AN ANALYSIS AccuPyc 1330

PREPARING AND LOADING A SAMPLE

Preparing the sampie is the first step in obtaining accurate results from the pycnometer. Sam-
pies must be free of moisture in order to obtain true sampie weight and to avoid the distort-
ing effect of water vapor on the volume measurement. The following procedures are
recommended; however, modifications may be necessary for some materials. Heat sensitive
materials may have to be dried by long-time exposure to silica gel, freeze drying, etc. Mate-
rials having a low melting point may be dried using the purge process. In this case, do not
weigh the sampie and cup until after the purge and analysis have been completed.

The important point to keep in mind is that each step should be conducted to avoid exposure
of the dried sampie to atmospheric moisture. This means weighing as rapidly as possible and
installing in the instrument without unnecessary delay.

1. Weigh the empty sampie cup. (If volume only is to be measured, you may skip this step).

2. Place a quantity of sampie in the cup. Use as large a quantity of sampie as possible; we rec-
ommend that the cup be at least two-thirds full. Pack powders and fluffy materials (if permis-
sible) to obtain maximum sampie weight in the cup.

3. Place the sampie cup with sampie in a drying oven. The amount of time the sampie must be
heated depends on the material and the temperature it will tolerate; this may have to be es-
tablished by other tests.

4. Remove the sampie cup from the oven and transfer it to a desiccator provided with active
desiccant Allow it to cool until near room temperature. In the steps which follow, minimize
air exposure of the sampie.

5. Weigh the cup and sampie and record the weight. Subtract the empty sampie cup weight
from the sampIe cup plus sampie weight to determine the sampie weight. (If volume only is
to be measured, you may skip this step.)

6. Remove the cell chamber cap.

3·2 15 Dec 89
AccuPyc 1330 PERFORMING AN ANALYSIS

7. Insert the sampie cup with sampie into the cell chamber.

Figure 3-1. Inserting Sample Cup Into Cell Chamber

8. Replace the cell chamber cap.

15 Dec 89 3-3
PERFORMING AN ANALYSIS AccuPyc 1330

STARTING THE ANALYSIS

USING THE DEFAULT PARAMETERS

To start an analysis using the analysis and report parameters shipped with the pycnometer:

1. Press LI_---'I 14'1.

2. The following prompt is displayed:

Press I'emifl to begin the analysis.

USING MODIFIED ANALYSIS PARAMETERS

To start an analysis using analysis parameters that have been modified:

1. Press LI_ ---'I kwl.

2. The following prompt is displayed if Sampie 10 was enabled in the Report Options function.

Using sampie lOs can help you keep track of data from various analyses. You may. for ex-
ample. use the sampie 10 as a date and time stamp. The sampie 10 can contain from I to
20 numbers and dashes.

Enter the sampie 10 and press I~Ntl(ill.

3. The following prompt is displayed if density was selected for Analysis display mode in the
Report Options function.

Enter the sampie weight and press IEilTEifl. The range of valid entries is 000.0000 to
999.9999 g.

3-4 22 Aug 90
AccuPyc 1330 PERFORMING AN ANALYSIS

4. The fOllowing prompt is displayed.

Press !&NTSIi] to begin the analysis.

VIEWING OR PRINTING ANALYSIS RESULTS

1. As the analysis is perfonned, operational status messages are displayed. (Refer to Monitor-
ing the System in Chapter 4 for adescription of the messages.)

2. When the analysis is complete, the pycnometer beeps three times. Remove the
the cell chamber. If there were any errors, the first error message is displayed. Press ....
to cycle through the error messages.

3. After the error messages are diSIJlay: average volume or density and the deviation
from the mean are displayed. Press :.

4.

5. When the Reload prompt is displayed, you may begin another operation.

15 Dec 89 3-5
 CHAPTER4

GENERAL OPERATING INSTRUCTIONS

• Monitoring the System

• Caneeling an Automatie Operation

• Entering Commands
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

GENERAL OPERATING INSTRUCTIONS

The pyenometer remains in the display mode until you enter a eommand by pressing the ap-
propriate keys. This ehapter deseribes how to read the displayand enter eommands.

MONITORING THE SYSTEM

STATUS MESSAGES DlSPLAYED DU RING AN AUTOMATie OPERATION

When an automatie operation is in progress, operational status messages are eontinually dis-
played. You may not enter eommands until the operation is f"mished. You may:

• Press ,-I_ .....1!cmltl to eancel the automatie operation.

• Press IL_...JI ! :Wl ttl to print a partial report of analysis or ealibration results.
• Press 1.. 1_ .....llt3 tii to transmit a partial report of analysis or ealibration results.
The following example shows a typical status message for an automatie operation. Refer to
Table 4-1 for a detailed deseription.

Operation Pressure
Display Units of
Type Measure

No. of Seconds
Action Performed

Action Being
Perfonned
No. limes of limes
eurrenl Mode Currenl Mode
has been was Requested
Perfonne<f

When the operation is fmished, the pycnometer beeps three times.

15 Dec 89 4-1
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

Table 4-1. Automatie Operation Status Messages

Operation Type Anls Analysis

Cal 1 Calibration Pass I, which is the first pass during calibra-

tion with the cell chamber empty.

Cal 2 Calibration Pass 2, which is the second pass during cali-

bration with the calibration standard in the cell chamber.

zero zero offset

Pressure Display P Current pressure in system

PI Pressure for data point PI t

pz Pressure for data point pzt

Operation Mode Purg Purge in progress

zero Transducer zero reset in progress

Run Run in progress

Action fill F'illing the cell chamber or expansion chamber

equil Equilibrating

wait Wait the displayed number of seconds

t Refer to Appendices B and C.

4-2 15 Dec 89
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

ERROR AND REPORT MESSAGES

Error and report messages generated during the operation are plaeed in a queue in ehronologi-
ea! order, with eITor messages having the highest priority (refer to Figure 4-1). the au-
tomatie operation is eomplete, the Reload promret is d/sPlayed. You may press 1" " •. ' to
display the first message and eontinue pressing ClIQIl;l\ to eyc1e through the messages. You
may press f;CUi.ltl while a message is displayed to delete the message.

Operation Error Messages - - - 1st Priority

~~------~~

~_R_epo:....-rt_E_rro_r_M_e_s_sa..::g~es_-I - - - 2nd Priority

L-_ _ _R_e.:,.po_rt_D_a_ta_ _- - - I - - - 3rd Priority

Figure 4-1. Message Queue

After the operation eITor 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 automatie operation is begun, at whieh time they
are automatieally deleted.

15 Dec 89 4·3
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

CANCELING AN AUTOMATIC OPERATION

You may cancel an automatie operation that is in progress by pressing 1"-------,llewRlI. The
following message is displayed:

Press ltillfltM within five seconds to cancel the operation.

When you cancel an operation, messages are displayed indicating that termination is in prog-
ress. The te~i~ation process, whiCh. vents the sR~~~~~1 tak~s abou~ 30 seconds. You may can-
cel the termmatlOn process, by pressmg I I ·CU\Alt agam, but If you do, you must
manually vent the system.

If no runs were completed and there are not enough data to compute, the following message
is displayed:

If there are enough data to compute and reports were requested, they are printed.

4-4 15 Dec 89
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

ENTERING COMMANDS
The pyenometer remains in display mode until you enter a eommand by pressing the appropri-
ate keys on the keypad. Commands start an analysis or other automatie operations and allow
you to modify operating parameters. The eommands available are:

Perform an Analysis
Review and Edit Analysis or Calibration Data
Print or Transmit Reports
Calibrate the Pyenometer
Zero the Pressure Transdueer
Edit Set-Up Parameters
Manually Control the Valves

NOTE
You may not enter a command while an automatie operation is in
progress.

When you enter a eommand, most funetions will display prompts. A prompt is arequest for
you to enter information. A prompt generally eontains two lines. The first line contains a
deseription of the requested information and the displays adefault value (when
lapplien!:~'!.l use the d:fault value,. jus~ press the . .. . key. For example, when you press
{;};~!;. •••;.;.; the followmg prompt IS dlsplayed:

Description of Requested Information

Defauf! Vafue

To seleet analysis parameters, whieh is the default value, press tmmw .

If you do not wish to use the default value, you ean use the keypad to enter other responses.
There are two types of prompts: data entry and multiple ehoice. Prompts that require you to
enter data are followed by a colon (:). Use the keypad to enter the desired value, then press
IEIlT!I!I. If you enter an invalid value, you will hear a beep. Try again.

Multiple ehoice prompts eontain a fixed set of respor are followed by a question
mark (?). To seleet a multiple ehoice response, press .... until the desired value is dis-
played, then press !~N!tf;RI.

At any time while entering information you may:

Press I:$AV~:I to save the information you entered and return to display mode.

Press LI__II~t,,*jjl to delete the information you entered and return to display mode.

The remainder of this ehapter deseribes the eommands used to begin automatie operations,
review, edit, and print results, and edit operating parameters.

15 Dec89 4-5
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

PERFORMING AN ANALYSIS
Press LI_-,I V/lN;1to perform an analysis.

Display Entry

This prompt is displayed only when Sampie ID was en-

abled in the Set-Up function (refer to Report Options later
in this chapter).

The sampie ID can contain from 1 to 20 numbers and

dashes.

Enter the sampie ID and press Ill\lttilitl.

NOTE

Press ItIW Mto insert a dash.

This prompt is displayed only if density was selected for

Analysis display mode (refer to Report Options later in
this chapter.)

Enter the sampie weight and press li!iir!!~ :J.

Range: 000.0000 to 999.9999 g

Choose ODe of the following:

• Press 1l!i'lfElIl to start the analysis.

The analysis begins and operational status messages are

continually displayed .

• Press 1'·!iÄVi\'d to store the data you ente red and return to
display mode.

• Press LI_-,l lt tUIl.l to cancel the analysis.

4-6 22 Aug 90
•
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

REVIEWING AND EDITING DATA

The Review function enables you to review and edit the results of the last analysis or calibra-
tion along with its entered parameters.

Revlewlng and Edltlng Analysis Results and Parameters

Press I IIIla 'tl I to review or edit analysis results.

Display Entry

The sampie ID is displayed if it is enabled in the Set-Up

funCtirnJ~~er to Report Options later in this chapter).
Press ".tm\!l. .

This prompt is displayed only if density is selected for

Analysis display mode (refer to Report Options).

The sampie weight entered in the Start Analysis function is

displayed. Press !ittÜ'jjiil.

Either density or volume is displayed depending on the se-

lection made for display mode (refer to Report Options).
[N] is replaced with the number of the run. The deviation
from the mean is also displayed.

You may choose to exclude the or volume

from the calculated average by pressing When a
density or volume is excluded from the average, an asterisk
appears next to it.

Likewise, a density or volume that was previously excluded

from the calculated avera~e m~r be included by pressing
L I . When you press il!1o~
d!ötcS · j·· , a new deViation
.. . calcu-
IS
lated and displayed.

Press iiliiffiilll to display values for the next ron.

Press F:$~NJ:itl when you wish to exit review and edit mode
and return to display mode. When you press Itf!~i;iJiM, all
collected data are automatically recalculated and all data re-
duction messages are added back into the queue.

15 Dec 89 4-7
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

Revlewlng and Edltlng Callbratlon Results and Parameters

Press LI_--,II.Mtl to review or edit calibration results.

Display Entry

The volume of the calibration standard is displayed.

Select either cell chamber or expansion chamber, then press

liiNtelil.

Either cell or expansion volume is displayed depending on

the selection made at the previous prompt. [N] is replaced
with the number of the run. The deviation from the mean is
also displayed.

You may choose to exclude the displayed cell or@eXl.!jSiOn

volume from the calculated average by pressingl!l:!~il .
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 Ijjjjpi($\l.

When you press I!lIiQiQ~I, a new deviation is calculated and

displayed.

Press f~M to display values for the next run.

Press lif.i(wJl when you wish to exit review mode

and return to display mode. When you press:: , all col-
lected data are automatically recalculated and all data reduc-
tion messages are added back into the queue.

4-8 15 Dec 89
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

PRINTING REPORTS
Reports are generated after analysis and ealibration and remain available for viewing or print-
ing until another automatie operation (other than zero) is performed. When you perform an
automatie operation, reports from the previous operation are deleted.

The Report Options funetion enables you to seleet the destination of the report that is auto-
matically generated after an analysis or ealibration. The destination may be: display, printer,
or transmission line. A display report is always ealeulated regardless of the specified destina-
tion. The display report for analyses eontains average density or volume, depending on the op-
tion seleeted (refer to Report Options), and the deviation from the mean. The printed report
eontains volume, density, and deviation for eaeh run, as weil as an average of all runs. Note
that if you do not enter a sampie weight, the value shown for density will be ineorrect.
When sampie weight is not entered, 1.0000 g is used.

The display report for ealibration eontains average eell or expansion volume, depending on
the option seleeted (refer to Report Options), and the deviation from the mean. The printed
report eontains cell and expansion volumes for eaeh run, as weil as an average of all runs.
A run with an asterisk next to the run number is not ineluded in the ealeulations.

Figure 4-2 shows a ealibration report. Figure 4-3 shows areport for an analysis performed
using the same ealibration standard. Figure 4-4 shows areport for an analysis performed with
run preeision enabled.

To display reports, press lliilö\Clil to eycle through messages until the report messages are dis-
played.

Press I Ilnt:&rwl to print reports. Reports are immediately sent to the printer. If you press
I I itül!iWI during an automatie operation, a partial report is printed.
You may eaneel reports sent to the printer or serial line by pressing I IICil&i\ill. You may
eancel partial reports that were requested during an automatie operation when the following
message is displayed:

15 Dec 89 4-9
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

The following is 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.

PaO'_ 1

AccuPyc 1338 UX.XX

Serlal Hll .. ber XXXXX
CIlUbratlDn RepDrt

Volume of Callbratlon Standarda 5.5775 ce

Nunber of purgesl 10 Equl11bratlon Rate. 0.0050 palg/.1n

Ce 11 Expansion
Volulle Deviation Volua. Devlat Ion
Run PaIr. ce ce ce ce
---------
1
--------
12.3844
--------
0.0008 7.998e 0.0003
2 12.3841 0.0004" 7.9988 0.0003
3 12.3841 0.0004 7.9993 0.0008
•
5
12.3634
12.3844
-0.0003
0.0007
7.9984
7.9991
-0.0001
0.0006
6 12.3839 0.0002 7.9987 0.0002
7 12.3835 -0.0001 7.9984 -0.0002
8 12.3831 -0.0006 7.9979 -0.0006
9 12.3830 -0.0006 7.9980 -0.0011'5
10 12.3828 -0.0009 7.9977 -0.0008

Average Cell.Volumel 12.3837 ce Standard Deviation. 0.0006 cc

Average Expansion Volume. 7.9965 ce Standard DeViation: 0.0005 ce

Figure 4-2. Calibration Report

4-10 22 Aug 90
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

The following report represents an analysis that was perfonned on the calibration standard
used for the previous report.

page 1

AccuPyc 1338 VX.XX

Serial "IIoMber XXXXX
Denalty and Uol ..... ., Report

sa.ple 101 11-6-S9--1Z-55 Sampie Welgbt I 42.6966 q

Number of Purqes. 20 Equl11bratlon Rate. 0.0eS0 palg/111n
Cell Volu... 12.3837 ce Expansion Volume, 7.9995 ce

Volulle Deviation Oens1ty Deviation

Run. ce ce g/ce qlcc
1 5.5767 -0.0005 7.6562 0.0007
2 5.5772 -0.0001 7.6556 0.0001
3 5.5771 -0.0001 7.6557 0.0002
4 5.5771 -0.0001 7.6557 0.0002
5 S.S777 0.0004 7.6549 -&.0006
6 5.5775 0.0003 7.6551 -0.00.'
7 5.5776 0.0003 7.6550 -0.0005
8 5.5779 0.0006 7.6546 -0.0009
9 S.S77. 0.0001 7.6553 -0.0002
10 5.5775 0.0002 7.6552 -9.0003
11 5.5773 0.0001 7.6554 -0.0001
12 5.5770 -0.0002 7.6558 0.0803
13 5.5776 0.0003 7.6550 -0.0005
14 5.5776 0.0004- 7.6549 -0.0006
15 5.5770 -0.0002 7.6558 0.0003
16 5.5776 0.000' 7.6550 -0.0085
17 5.5766 -0.0007 7.6564 0.0009
18 5.5765 -0.0007 7.6565 0.0010
19 5.5766 -0.0006 7.6563 0.00eS
20* 5 . 5762 -0.0010 7.6569 0.0014

Average VOlu... 5.5772 ce Standard Deviation. e.000. ce

Average Danslty. 7.6555 g/cc Standard Deviation. 0.0006 Q/cc

Figure 4-3. Analysis Report

22Aug 90 4-11
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

The following report represents an analysis that was perfonned on an untreated (not dried)
sampIe with run precision enabled. The run precision feature 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.

Pa;. 1

AccuPyc 1338 VX.XX

Sari" NUMber XXXXX
Den.lty .nd VDlu.e Report

5allple lD. 11-06-89--14-45 Sallple Welqht I 5.8293 0-

NUllber of PurlJes I 20 Equllibratlon Ratet 0.0050 pelo'a1n
CeU Volume I 12.3637 ce Expansion Volumel 7.9985 ce

Volume Deviation Dens1 ty Deviation

Run. ce ce q/ce g/ee
--------
1.4081
--------
0.0000
------
4.1397
---------
-0.0000
l'
2' 1.4072 -0.0010 4.1425 0.0028
3' 1.4072 -0.0009 4.1425 0.0026
••
5'
1.4072
1.4111
-0.0010
0.0030
4.1426
.. .1319
0.0029
-0.0087
6' 1.4083 0.0001 ... 1393 -0.0004
7' 1.4074 -0.0007 4.1419 0.0021
O' 1.4076 -0.0005 " .1412 0.0015
9' 1.4070 -0.0011 ... 1431 0.0033
10' 1.4059 -0.0023 4.1464 0.0067
11' 1.4070 -0.0011 4.1429 0.00'32
12' 1.4076 -0.0006 4.1414 0'.00'17
13' 1.40'74 -0.00'07 4.1419 9.0'0'22
1.4197 9.0'025 4.1323 -0'.0'0'75
'"
15'
16'
1.40'68
1.40'62
-0.0013
-0.0'0'26
4.1436
... 1455
0.0'0'39
0'.0'0'58
17' 1.40'82 0'.0'0'0'0' 4.1396 -0'.0'0'0'1
10 1.4083 0'.0'0'0'2 4.1393 -6.0'0'05
19 1.40'84 0'.0'00'3 4.1389 -0'.60'0'9
20 1.40'85 0.0'0'0" 4.1387 -0'.0'0'11
21 1.40'73 -0.0'0'0'8 4.1421 0'.0'0'24
22 1.40'81 -0'.00'0'0 4.1397 6.0'600

AveraQe Voluraea 1.40'81 ce Standard Devia.tion. 0.00'0'5 ce

Average DensitYI ... 1397 q/cc Standa.rd DeViatIon, 0.0014 g/ce

Figure 44. Analysis with Run Precision Report

4-12 22 Aug 90
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

TRANSMITTING REPORTS
The AeeuPye RS-232 interface transmits report data to a computer using the standard ASCII
file format. Once eaptured with an asynehronous serial eommunieations program such as
COTERM, whieh is available from Mieromerities (part no. 003-20632-00), the report data
can be used in popular spreadsheet and data manipulation programs.

Press I II M,äMiI to transmit report data over the serialline. If you press LI_...JI [mi HM
during an automatie operation, a partial report is transmitted.

You may eaneel report data sent to the serial line by pressing I IloWiU. You may ean-
cel partial reports that were requested during an automatie operation when the following mes-
sage is displayed:

15 Dec 89 4-13
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

CALIBRATING THE PYCNOMETER

You should check or calibrate the pycnometer anytime you restart it. For a quick check, ron
an analysis with an empty cup to see how dose the average volume is to O. It should be
±O.05% of full-scaie. To calibrate the pycnometer, follow the instructions beiow. When you
calibrate the pycnometer, cell volume and expansion volume in the set-up parameters are
updated automatically.

Press _---'11: i~(1 to begin the calibration procedure.

LI

Display Entry

volume of the calibration standard and press

Range: 0.1 to 999.0000 ce

Press 1~t((!!1 to begin the calibration or LI_...JII!:Wt~1 to

cancel the calibration.

Status messages are dispIayed as the first phase of calibra-

tion progresses. When the first phase is finished, you will
hear three beeps and the following prompt is dispIayed.

Insert the calibration standard in the cell chamber. Then

press I~iitiilil.

When you press IElifilill, calibration continues and opera-

tional status messages are continually dispIayed.

4-14 22 Aug 90
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

ZEROING THE PRESSURE TRANSOUCER

The transducer offset may be reset to zero in order to perform diagnostics or to operate the
pycnometer manually.

NOTE
The transducer is automatically set to zero for each run in an analysis
or calibration.

Press 1..._--,lln@!:nltozerothepressure transducer.

Display Entry

Press [_Itl to zero the transducer or <-I_---'I ti~l!1j to can·

cel the operation.

The transducer is zeroed and the pycnometer returns to dis-

play mode.

15 Dec 89 4-15
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

MANUALLY CONTROLLING THE VALVES

This function enables you to perfonn a manual analysis by controlling the valves.

Press LI_-liitttl to enter manual mode.

Display Entry

When Manual is shown in the display, you can manually

open and elose the fill, expansion, and vent valves by press-
ing the appropriate keys.

7 - Opens and eloses the fill valve

8 - Opens and closes the expansion valve
9 - Opens and closes the vent valve

Observe the indicators above the In~iti;;"'I, !iixPAmil, and

IWJ!~'fH keys. When a valve is open, the indicator is on.
When a valve is elosed, the indicator is off.

Press nlll\liiÜI when you wish to exit manual mode and re-
turn to display mode.

CAUTION

Prolonged opening of all three valves at one

time may cause excessive loss of helium.

4-16
•
15 Dec 89
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

EDITING THE SET-UP PARAMETERS

The set-up function enables you to enter parameters to be used for analysis, calibration, re-
porting, and data transmission. There are five sets of parameters:

Analysis or calibration parameters

Report options
Calibration volumes
Data transmission
Unit types and Operating Language

The pycnometer is shipped with default values entered for analysis parameters; it is not neces-
sary to edit these values in order to perform an analysis. However, you may modify an analy-
sis to meet your own particular needs by changing the parameters, which include number of
purges and runs (0 to 99), fill pressures (0 to 19.850 psig), and equilibration rate (0.0001 to
9.0000 psig/min) .

Default values are also entered for calibration parameters. These may be edited in the same
manner as analysis parameters. The only difference is that for calibration the maximum num-
ber of purges and runs that will be performed by the system is ten.

Report options specify the report mode (density or volume for analysis) and the report desti-
nation.

Calibration volumes specify the sampie volume and the expansion volume to be used for cali-
bration.

Data transmission specifies transmission parameters such as baud rate, parity, etc.

Unit types specify either pounds-per-square-inch gauge (psig) or kilopascals gauge (kPag) to
be used as the pressure measurement unit type. It also specifies the language to be used.

The parameters you enter are stored and used to control the pycnometer until new parameters
are entered. Instructions follow for each set of parameters.

15 Dec 89 4·17
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

AnalysIs or C8l1bratlon Parameters

Press IL_-----'IIFil to display or edit analysis or calibration parameters.

Display Entry

Press ... .•• .••.••..• until Analysis parameters is displayed. Then

press

number of purges to be performed and press

Range: o to 99
Purging cleans the cell and expansion chambers i)efore an
analysis begins. The greater the number of purges, the
cleaner the sampIe will be when analyzed.

Enter the fill pressure and press n'iNtlillil.

Range: o to 19.850 psig

o 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 sampIes.

Enter the number of runs to be performed and press Iml!äl.

Range: 1 to 99

Enter the fill pressure and press lliiiii'tillil.

Range: o to 19.850 psig

o to 136.86 kPag

4-18 15 Dec 89
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

Display Entry

Enter the equilibration rate and press li ldiiilf! .

Range: 0.0001 to 9.0000 psiglmin

0.0007 to 62.05 kPaglmin

A high rate will produce faster results, but results may not
be as precise as desired. The lowest rates may cause errors
when some materials (such as materials with appreciable
vapor pressures, closed cell foams, or organics) are ana-
lyzed.

The run precision feature enables early termination of the

analysis when certain criteria are met. When you select run
precision, the analysis will be terminated after five consecu-
tive runs are within the specified tolerance.

If you select run precision, you should request a large num-

ber (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
met.

Select yes or no, then press li~M.

NOTE

This prompt applies for analysis only.

This prompt is displayed only if the number of runs is

greater than five.

Enter the run precis~on volume tolerance which IS~llPlessed

as apercent of nommal cell volume, then press ,~I(tf;!I:, .

Range: 0.01% to 50%

NOTE

Nominal cell volume is the sampie capacity.

15 Dec 89 4-19
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

Display Entry

Choose one of the following options:

• Press li$4vtll to save the information you entered and

return to display mode.

• Enter another set-up type.

• Press I I !ctlUlltJ to discard the information you

entered and return to display mode.

4-20 15 Dec 89
AccuPyc1330 GENERAL OPERATING INSTRUCTIONS

Report Options
Press IL_~IIHH2m l to display or edit report options.

Display Entry

until Report options is displayed. Then press

Seleet the mode, either density or volume, in which the

analysis report will be displayed, then press !~I.

NOTE
80th density and volume will be shown on
the printed report, but density will be
correct only if sampIe weight was entered.

A sampIe ID is a unique identifier of the sampIe. It can eon-

tain from I to 20 numbers or dashes.

Using sampIe IDs ean help you keep track of data from var-
ious analyses.

Por example, you can use the sampIe ID as a date and time
stamp.

Select either yes or no, then press IErlillij'l .

Seleet the destination of the report that is automa~~ilgen­

erated after an analysis or ealibration, then press i~i .

Choices: display, printer, transmission /ine.

NOTE
A display report is always calculated regardless
of the destination.

15 Dec 89 4-21
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

Display Entry

Choose one of the following options:

• Press I";(V~I to save the information you entered and

return to display mode.

• Enter another set-up type .

• Press I I UiituiRl to discard the information you

entered and return to display mode.

4-22 15 Dec 89
AccuPyc 1330 GENERAL OPERATING INSTRUCTIONS

Callbratlon Volumes
Press LI_-,IIRlfFI to display or edit calibration volwnes.

Display Entry

Press: . until Calibration volumes is displayed. Then

press

NOTE

When the pycnometer is calibrated, cell

volume and expansion volume are auto-
matically updated.

Enter the cell volume and press !Mt!'l$:I.

Range: 0.5 to 999.0000 ce

Enter the expansion volume and press liiffiiii'l.

Range: 0.5 to 999.0000 ce

Choose one of the following options:

• Press loll:iül to save the information you entered and

return to display mode.

• Enter another set-up type.

• Press I I !Q!iQ1iil to discard the information you

entered and return to display mode.

15 Dec89 4-23
GENERAL OPERATING INSTRUCTIONS AccuPyc 1330

Data Transmission
Press L.. .I_---'11:}:2::1 to display or edit data transmission parameters.

Display Entry

Press @llOiCEiI until Data transmission is displayed. Then

press IliNtER I.

Baud rate specifies data transmission. Select the

baud rate, then press

Choices: 9600 600

110 1200
150 2400
300 4800

Select either 8 or 7, then press telttelil.

Select either I or 2, then press 11ii'rtEl!1.

Select the parity, then press f~ä;l.

Choices: none, even, odd.

Select either disabled or enabled, then press I~:I.

Choose one of the following options:

• Press IlJAV!ÜI to save the information you entered and

return to display mode .

• Enter another set-up type .

• Press 1 IlcWRI to discard the information you

entered and return to display mode.

4-24 15 Dec 89
AccuPyc1330 GENERAL OPERATING INSTRUCTIONS

Unlt 'TYpes and Operating Language

Press LI_...JIIKKällU to display or edit unit types or the operating language.

Display Entry

until Unit types is displayed. Then press

S~lect either psig (pounds-per-r9~~iinCh gauge) or kPag

(ldlopascal gauge), then press 1!mEiR, •

Select the desired language, then press I!:ldillil .

Cho/ces: Engl/sh, German, Span/sh, or French

NOTE
If there are error messages in the message
queue (indicated by an asterisk next to the
Reload prompt), delete the messages before
changing languages. Refer to "Error, Report,
and System Status Mjssaget" Chapter 4.
Make sure you press '"$li.Vilt'
,k . . . ,.. ,:: after changmg
•
languages.

Choose one of the following options:

• Press H.,j(jljl to save the information you entered and

return to display mode.

• Enter another set-up type.

• Press I I rQ@A~1 to discard the information you

entered and return to display mode.

15 Dec 89 4-25
 CHAPTER 5

TROUBLESHOOTING AND MAINTENANCE

• Troubleshooting

• Error and Status Messages

• Maintenance
AccuPyc 1330 TROUBLESHOOTlNG AND MAINTENANCE

TROUBLESHOOTING AND MAINTENANCE

This chapter describes common operational problems and their solutions, error and status mes-
sages, and maintenance procedures. If further assistance is needed after following the procedures
in this chapter, contact a Micromeritics Service Representative.

TROUBLESHOOTING
Operating problems encountered with the pycnometer are usually easily corrected. Typical prob-
lems and the steps required to correct them are described in the following table.

Table 5-1. Common Operational Problems

Unit does not work Power cord not fully inserted Insert power plug firmly into
when power switch is at one end or the other. outlet socket; insert unit con-
turned on. nector firmly into power con-
nector opening.

No power at outlet. Plug in lamp or small appli-

ance to test outlet. If there is
no power, contact electrician.

Plug prongs bent so that con- Wiggle power plug at outlet

tact not made at outlet. while watching display. If dis-
play comes on, have electri-
cian adjust prongs or replace
outlet or plug.

Power cord damaged. Have electrician check cord

using test meter. Replace if
defective.

Wrong voltage selected. Unplug unit. Check voltage

selection board. If wrong volt-
age selected. correct the volt-
age and re-insert board.

15 Dec 89 5·1
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

Unit does not work Fuse blown. Unplug unit. Check fuse.
when power switch is Check the voltage selected; it
turned on. (continued) must be appropriate for the
fuse: 100-120 VAC, 0.5 Amp
Slo-BIo fuse; 220-240 VAC,
0.25 Amp Slo-Blo fuse.
Have an electrician check the
wall outlet. Replace the fuse
if blown.

Loose interna! connection or Contact a Micromeritics Ser-

broken wire. vice Representative for repair
or replacement information.

Specified pressure not Chamber cap not properly Oose chamber cap by turning
reached or not main- closed. clockwise.
tained.
Chamber cap contains dust or Oean both the chamber cap
debris or the O-ring is not and the rim of the cell cham-
properly greased. ber by wiping with lint-free
tissue. Lightly grease the
chamber cap O-ring (refer to
Greasing the Chamber Cap
O-Ring later in this chapter).

0- ring in chamber cap not Check the chamber cap. En-

properly seated. sure that the 0- ring is prop-
erly seated and !hat it
contains no scratches or cuts.

O-ring in chamber cap is cut Repace the O-ring in the

or scratched. chamber cap (refer to Replac-
ing the Chamber Cap 0-
Ring later in this chapter).

Gas leaks in the cell chamber Check the pycnometer for

or expansion chamber. leaks (refer to Checking the
Cell and Expansion Cham-
bers for Leaks later in this
chapter).

5-2 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

Heliwn drained fmm Leaks in the gas line connec- Pressurize the system. Close,
tank. tion. then open the Cylinder Shut-
Off Valve. If the needle on
the pressure gauge on the gas
cylinder jwnps abruptly, a
leak in the gas line connec-
tions may be indicated.
Check all gas line connections
(refer to Rear Panel Connec-
tions in Chapter 2 for connec-
tion instructions).

Pycnometer was left in man- Close all valves, then attach a

ual mode with all the valves new tank of heliwn.
open or the fill valve open
and the chamber cap off.

15 Dec 89 5-3
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

ERROR AND STATUS MESSAGES

The following error messages may appear in the display area of the pycnometer. Some of the
messages contain the statement: "NN/ZZ runs completed." When this appears, NN will be re-
placed with the number of runs completed when the error occurred and z:z will be replaced with
the number of runs requested.

The messages are organized into two categories: Queued Messages and Messages Displayed Dur-
ing an Automatie Operation.

QUEUED MESSAGES
Messages placed in a queue are displayed in chronological order when you press !bilRI. When
the queue contains eITor messages, an asterisk is shown next to the Reload prompt.

ANLSERR: Eq failure
NN/ZZ runs completed
Cause: The sampie being analyzed failed to equilibrate in 1000 seconds.
Action: Check the system carefully for leaks as described in Checking the Cell and Ex-
pansion Chambers for Leaks later in this chapter. Make sure the sampie is
properly prepared before performing an analysis.

Cause: Sampie (foams, organies, etc.) absorbs helium slowly:

Action: Set the equilibration rate to progressively higher values until reasonable equilibra-
tion times (15 sec to 120 sec) are achieved.

ANLSERR: Fill failure

NN/ZZ runs completed
Cause: There was insufficient pressure to allow filling within five minutes during an
analysis.
Action: Increase the regulator pressure or, if there is insufficient helium in the tank, ob-
tain a new tank of helium.

ANLSERR: Overrange
NN/ZZ runs completed
Cause: Apressure overrange occurred during an analysis because the regulator pressure
is set too high.
Action: Adjust the pressure so that it is equal to the higher of the two fill pressures speci-
fied in the analysis parameters plus 2.0 psig.

5-4 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

Cause: Apressure overrange occurred during an analysis because an error occurred in

the pressure measurement electronics.
Action: Call a Micromeritics Service Representative.

ANLSERR: Underrange
NN/ZZ runs completed
Cause: Apressure underrange occurred during an analysis because an error occurred in
the pressure measurement electronics.
Action: Call a Micromeritics Service Representative.

CALIERR: Eq faDure
NN/ZZ runs completed
Cause: The empty cell chamber failed to equilibrate in 1000 seconds during the first pass
of calibration.
Action: Check the system for leaks as described under Checking the Cell and Expan-
sion Chambers for Leaks later in this chapter.

CALIERR: FiU failure

NN/ZZ runs completed
Cause: There was insufficient pressure to allow fiUing within five minutes during the
first pass of calibration.
Action: Open the tank valves if shut, increase the regulator pressure or, if there is insuffi-
cient helium in the tank, obtain a new tank of helium.

CALIERR: Overrange
NN/ZZ runs completed
Cause: Apressure overrange occurred during the first pass of calibration because the reg-
ulator pressure is set too high.
Action: Adjust the pressure so that it is equal to the higher of the two fiU pressures speci-
fied in the analysis parameters plus 2.0 psig.

Cause: Apressure overrange occurred during the first pass of calibration because an
error occurred in the pressure measurement electronics.
Action: Call a Micromeritics Service Representative.

15 Dec 89 5-5
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

CALIERR: Underrange
NN/ZZ runs completed
Cause: Apressure underrange occurred during the first pass of calibration because an
error occurred in the pressure measurement electronics.
Action: Call a Micromeritics Service Representative.

CAL2ERR: Eq failure
NN/ZZ runs completed
Cause: The calibration standard failed to equilibrate in I{)()() seconds during the second
pass of calibration.
Action: Check the system for leaks as described under Checking the Cell and Expan-
sion Chambers for Leaks later in this chapter.

CAL2ERR: Fill failure

NN/ZZ runs completed
Cause: There was insufficient pressure to allow filling within five minutes during the sec-
ond pass of calibration.
Action: Open the tank valves if shut, increase the regulator pressure or, if there is insuffi-
cient helium in the tank, obtain a new tank of helium.

CAL2ERR: Overrange
NN/ZZ runs completed
Cause: Apressure overrange occurred during the second pass of calibration because the
regulator pressure is set too high.
Action: Adjust the pressure so that it is equal to the higher of the two fill pressures speci-
fied in the analysis parameters plus 2.0 psig.

Cause: Apressure overrange occurred during the second pass of calibration because an
error occurred in the pressure measurement electronics.
Action: Call a Micromeritics Service Representative.

CAL2ERR: Underrange
NN/ZZ runs completed
Cause: Apressure underrange occurred during the second pass of calibration because an
error occurred in the pressure measurement electronics.
Action: Call a Micromeritics Service Representative.

5-6 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

DATA ERR:
No data to cornpute
Cause: An automatie operation was canceled before aIl necessary data could be collected.
Action: Restart the automatie operation.

Cause: All the runs have been exc1uded in review mode.

Action: Return to review mode and inc1ude some runs.

DTA WRN: Ca! std

10% of full-scale
Cause: The system Uied to generate a calibration repon. but the calibration standard used
was less than 10% of the nominal cell chamber volume. Resulting data may be
inaccurate.
Action: Use a calibration standard of sufficient size (calibration standards are available
from Micromerities). The calibration standard should occupy at least 10% of the
nominal cell chamber volume and the more nearly filled the cell iso the better the
calibration.

DTA WRN: Volurne

10% of full-scale
Cause: The amount of sampIe placed in the sampIe cup was so small that the percentage
of precision may be inferior.
Action: Rerun the sampIe using enough material to occupy the maximum amount of the
nominal cell chamber volume.

HW ERR: AID J10

faHure
Cause: An error in the pressure measurement electronics has occurred.
Action: Call a Micromerities Service Representative.

HW_ERR; BB RAM has

been initialized
Cause: Battery backed RAM has failed.

Action: Call a Micromerities Service Representative.

15 Dec 89 5-7
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

HW ERR: Valve I10

failure
Cause: An error in the valve control electronics has occurred.
Action: Call a Micromeritics Service Representative.

MAN ERR:
Pressure overrange
Cause: The fill valve was left open until the maximum system pressure was exceeded.
Action: Close the fill valve and open the vent and expansion valves. Allow the pressure
to stabilize.

PRT ERR: Timeout

failed to respond
Cause: The printer took longer than 10 seconds 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.

SYS ERR: Power Fail

NN/ZZ Runs Complet~d
Cause: Apower failure occurred and when power resumed, the automatie operation was
canceled.
Action: Restart the automatie operation if desired.

TRN_ERR: Timeout
failed to respond
Cause: The receiving device took longer !han 10 seconds to acknowledge 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 1/0 parameters controlling the receiv-
ing device correspond with the data transmission parameters in the set up mode.

USR ERR: Cal std

10% of full-scale
Cause: You tried to enter a calibration standard volume that is less than 10% of the nomi-
nal full-scale volume.
Action: Enter a volume that represents at least 10% of the nominal cell chamber volume.

5-8 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

USR ERR:
No data to review
Cause: You tried 10 review data for an automatie operation when there were no data to
review.
Action: Abandon request.

USR_ERR: Number of
runs must be = 5
Cause: You tried to enable run precision without increasing the number of runs to at
least five.
Action: Increase the number of runs 10 five or abandon request.

USR_ERR:
Out of range
Cause: You tried to enter a value that is out of the valid range.
Action: Enter a value in the specified range (refer to Chapter 4).

USR_ERR:
Pressure overrange
Cause: Apressure 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 pycnometer has been placed in a
draft-free environment.

ZEROERR: Overrange
Cause: Apressure overrange occurred while zeroing.
Action: Check for a fill valve leak. If there is none, contact a Micromeritics Service Rep-
resentative.

15 Dac 89 5-9
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

MESSAGES DISPLAYED DURING AN AUTOMATie OPERATION

When an automatie operation is in progress, status messages are continually displayed.

Automatie operation
has been canceled
Cause: The automatie operation has been canceled by the user.
Action: Wait for the termination process to complete or end the termination process by
pressing I I Jblütll two more times.

Print in progress
[ESCAPEj to cancei
Cause: Status message displayed when areport is being printed.
Action: None; this is a status message only.

Printer port
not responding
Cause: The printer took longer than five seconds 10 acknowledge receipt of data from
the pycnometer.
Action: Check 10 make sure the printer is properly connected 10 the pycnometer, is turned
on, and is on line.

Sending line (line number)

[ESCAPEj to cancei
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 acknowledge receipt of
data from the pycnometer.
Action: Make sure the receiving device is properly connected 10 the pycnometer RS-232
port and is turned on. Verify that the serial 1/0 parameters controlling the receiv-
ing device correspond with the data transmission parameters in the set up mode.

5-10 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

Transmission port
waiting ror Xon
Cause: The receiving device stopped transmission by sending an Xoff, and hasn't re-
sumed the transmission by sending an Xon.
Action: None; when the receiving device is ready for more data, it should send the pyc-
nometer an Xon.

The following message is displayed on the printer or on the screen for transmitted data

No collected data to report, or all runs excluded

Cause: This message is printed or transmitted if you requested areport but there is either
no data available or data has been excluded via review mode.
Action: Initiate an automatie operation or retum to review mode and include at least one
run.

15 Dec 89 5-11
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

MAINTENANCE

GREASING THE CHAMBER CAP O·RING

The cell chamber cap contains an O-ring that requires routine maintenance because it is so often
exposed. The chamber cap O-ring should be greased at the beginning of each period of use.

1. Remove the chamber cap by turoing it counterclockwise then lifting off.

2. Wipe off the old grease using lint-free tissue.

3. Using your fingertips. apply a !hin layer of Dow Coroing high vacuum grease (or equiva-
lent) to the greasing disko

4. Insert the greasing disk into the chamber cap and turn slightly to apply a very light coating
of grease to the O-ring.

5-12
Figure 5-1. Greastng Chamber Cap O-Rtng

15 Dec 89
•
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

5. Wipe the mating surface in the cell chamber with lint-free tissue.

6. Replace the chamber cap.

REPlACING THE CHAMBER CAP Q-RING

Fine fibers and particles between the O-ring and its sealing surfaces can cause leaks, as can
scratches or cuts in the O-ring or in the metal surfaces. Wben 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.

Figure 5-2. Removing the Chamber Cap O-Ring

15 Dec 89 5-13
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

2. Clean the groove in the chamber cap using a small brush or lint-free tissue and isopropyl al-
cohol.

Figure 5-3. Cleaning the Chamber Cup

3. Allow the chamber cap to dry thoroughly.

4. Grease the O-ring using Dow Coming vacuum grease (or equivalent).

5. Replace the 0-ring, being careful not to nick or scratch il

5-14 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

CHECKING THE CELL AND EXPANSION CHAMBERS FOR LEAKS

To check the cell and expansion chambers for leaks perfonn the following procedure.

NOTE
Thls procedure should be performed In a temperature-stable envi-
ronment 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
partides, the O-ring should be properly seated, and it should not
contain excessive grease.

1. Allow the pycnometer to equilibrate thennally in a room having a stable temperature.

2. Press ,--I_--,I WqMM to enter manual mode.

3. If the system has been open, manually pUlge the system before proceeding as follows:

a. Open the EXPAND valve and close the VENT valve. ('The indicator above the key is tumed
on when the valve is open.)

b. Open the FILL valve and fill the sampie chamber to the desired pressure.

c. Close the FILL valve and open the VENT valve.

Repeat this procedure two or three times.

4. Press Mtiit%m to open the fill valve.

5. Fill the sampie chamber to 19.5 psig.

6. Press I!ditJiti to elose the fill valve.

7. ObseIVe the pressure display. After an equilibration period (about 20 to 30 seconds), the pres-
sure should not vary more than 0.0005 psig/min.

• If the pressure does not vary more than 0.0005 psig/min, proceed to step 8.

• If the pressure varies more than 0.0005 psig/min., temperature instability or a leak may be
indicated. Vent the system, then repeat steps 4 through 7 several times to verify !hat a
leak is indicated. If a leak is indicated, call a Micromeritics SeIVice Representative.

8. Press nWänfl to open the expansion valve and Inntwl to open the fill valve.

9. Fill the chambers to 19.5 psig.

10. Press I min l to elose the fill valve.

15 Dec 89 5-15
TROUBLESHOOTING AND MAINTENANCE AccuPyc 1330

11. ObseIVe the pressure display. After an equilibration period (about 20 to 30 seconds), the
pressure should not vary more than 0.0005 psig/min.

If the pressure varies more than 0.0005 psig/min, temperature instability or a leak may be in-
dicated. Vent the system, then repeat steps 8 through 11 several limes to verify that a leak is
indicated. If a leak is indicated, call a Micromeritics Service Representative.

5-16 15 Dec 89
AccuPyc 1330 TROUBLESHOOTING AND MAINTENANCE

CLEANING THE PYCNOMETER

The exterior casing of the pycnometer may be cleaned using a clean cloth, dampened with isopro-
pyl alcohol (IPA), a mild detergent solution, or a 3% hydrogen peroxide solution.

RECOVERING FROM APOWER FAllURE

The pycnometer has a battery back-up feature that saves entered data in case of apower failure.
Set up parameters and any other data entered will still be present when power is restored. If an
automatie operation was in progress when the power failure occurred, it will be eaneeled when
the pycnometer restarts. Any data collected during the automatie operation will still be present,
but the operation should be started again in order to produce complete results.

REPLACING FUSES

The pycnometer incorporates a fuse in the power connection slot to protect the unit from dam-
age. If the fuse is blown, it must be replaced with another of the same type and the correet rat-
ing. Refer to Selecting the Input Power in Chapter 2 for fuse requirements and replaeement
procedures.

15 Dec 89 5-17
 CHAPTER 6

ORDERING INFORMATION
AccuPyc 1330 ORDERING INFORMATION

ORDERING INFORMATION

133-()()()()()-00 AccuPyc 1330, fully-automatic gas displacement pycnometer with lO-mL

sampie capacity.

133-00001-00 AccuPyc 1330, fully-automatic gas displacement pycnometer with I-mL

sampie capacity.

133-00002-00 AccuPyc 1330, fully-automatic gas displacement pycnometer with l00-mL

sampie capacity.

133-34803-00 Sampie Module, I-mL

133-34802-00 Sampie Module, 10-mL

133-34804-00 Sampie Module, l00-mL

133-25855-00 Sampie Cup, I-mL capacity

133-25805-00 Sampie Cup, 100mL capacity

133-25845-00 Sampie Cup, l00-mL capacity

003-51135-00 Fuse, 3AG Slo-Bl0, 0.5 Amp

003-51141-00 Fuse, 3AG, Slo-Blo, 0.25 Amp

004-25076-00 Chamber Cap O-ring, I-mL

004-25575-00 Chamber Cap O-ring, lO-mL

004-25577-00 Chamber Cap O-ring, l00-mL

004-25633-00 Calibration Standard, lO-mL

004-25632-00 Calibration Standard, l00-mL

004-25549-00 Reducer, l/8-in. tube x 1/4-in. tube

004-62014-01 Regulator

230-02001-00 Gas Inlet Line Assembly

004-27042-00 Inlet Filter

004-25469-00 Inlet Transducer Filter O-ring

008-16045-00 Vacuum Grease, Dow Coming

15 Dec 89 6-1
ORDERING INFORMATION AccuPyc 1330

133-25825-00 Greasing Disk

130-25643-00 Magnet, 1/4 x 2 inches

003-20603-04 RS-232 Cable

004-54011-00 Tool for removal of sampIe cup

133-42701-01 French Template

133-42701-02 German Template

133-42701-03 Spanish Template

133-42801-00 Operator's Manual

Optional Equipment
003-33004-00 Control Module. lncludes 80386SX CPU with 80387SX math coprocessor,
40 Mb hard disk, amber monitor, dot-matrix printer and cables (100/120V,
50/60 Hz)

003-33004-01 Same as P/N: 003-33004-00 except 230V, 50/60 Hz.

003-20632-00 COTERM/220 Software Kit, includes RS-232 cable and diskette.

003-20631-00 Printer

003-20615-03 Printer Ribbon

6-2 15 Dec 89
 APPENDIXA

CHANGING THE ANALYSIS MODULE

AccuPyc 1330 APPENDIXA

CHANGING THE ANALYSIS MODULE

Analysis modules, which house the cell chamber, are available in various sizes, enabling you to
analyze different size sampies with precision. Ta change the analysis module:

1. Turn off the gas supply at the regulator mounted to the gas cylinder by turning the Cylinder
Shut-Off Valve fully counterclockwise.

Cylinder
Shut.Qff Valve

Inlet J

Figure A-l. Tuming Off Gas Supply

2. Press I I !)1 )tl on the pycnometer keypad to enter manual mode. Then press VENT to
open the vent valve, EXPAND to open the expansion valve, and FlLL to open the fill valve.

22 Aug 90 A-1
APPENDIXA AccuPyo 1330

FILL EXPAND VENT

ANALVZE REVIEW PRINT

o
MANUAL SETUP TRANSMIT ESCAPE

ZERO CALIBRATE

Figure A-2. Pycnometer Keypad

3. ObselVe the pressure reading. When the pressure drops to less than I psig, place the power
switch on the back of the pycnometer in the off (0) position. Remoye the power cord.

4. Disconnect the gas supply line from the rear panel of the pycnometer by tuming the nut on
the INLET connector counterclockwise with a 7/16 in. open-end wrench (refer to Figure
A-l).

5. Disconnect the gas yent line (if attached) by gently pulling the flexible tubing from the rigid
tubing labeled VENT at the rear of the pycnometer.

6. Remoye the printer cable and the serial cable (if used) from the rear panel of the pycnome-
ter.

7. Remoye the cap from the cell chamber.

A-2 15 Deo 89
AccuPyc 1330 APPENDIXA

8. Remove the rear panel by removing the five retaining screws !hat hold the panel in place.

Figure A-3. 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.

A B

FIgure A-4. Rotating Top Panel

22 Aug 90 A-3
APPENDIXA AccuPyc 1330

10. Remove the four screws securing the module mounting ralls to the baseplate.

Figure A-S. Module Mounting RaUs

11. Grasp the module and pull it straight up. A convenient method of removing the module is
to replace the 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 ralls.

12. Disconnect the cable assemblies going to the valves mounted to the block.

Disconnect Valve Disconnect

Gables Here Electronics Module
Gables Here

Figure A-6. Disconnecting Cable AssembUes

A-4 22 Aug 90
ACcuPyc 1330 APPENDIXA

13. Remove the cable from the electronics module at the point it attaches to the printed circuit
board undemeath the module.

14. Attach the cable removed in step 13 to the new module 's printed circuit board.

15. Attach cables from the Vent, Expand, and Vent valves to J4, J5, and J6 as shown in
Figure A-7.

Yen! Valve

Expand Valve

Fill Valve

Figure A-7. Connecting CabU! Assemblies

16. Place the new module into the pycnometer. Make sure the standoffs fit into the correspond-
ing recesses in the ralls. Note that the transducer sbould be on the rear face of the module.

17. Reassemble the pycnometer by reversing steps 1 through 10. Be sure to remove the cap be-
fore closing the cover and to reconnect all cables and the gas supply line. Check the gas con-
nection for leaks.

18. Set the regulator pressure as described in Setting Regulator Pressure in Chapter 3.

19. Calibrate the pycnometer as described in Calibrating the Pycnometer in Chapter 4.

22 Aug 90 A-5
 APPENDIX B

ANALYSIS THEORY
 AccuPyc 1330 APPENOIXB

ANALYSIS THEORY

The AccuPyc 1330 Pycnometer is a gas displacement pycnometer, a type of instrument which
measures the volume of solid objects of irregular or regular shape whether powdered or in one
piece. A greatly simplified diagram of the instrument is shown in Figure B-l.

Assume that both VCELL and VEXP are at ambient pressure Pa' are at ambient temperature Ta' and
that the valve is then closed. VCELL is then charged to an elevated pressure PI. The mass balance
equation across the sampie cell, VCELL, is

(1)

where

nc = the number of moles of gas in the sampie cell,

R = the gas constant, and
Ta = the ambient temperature.

Calibrated Sampie Calibrated

Cell Volume Valve Expansion Volume
VCELL VEXP

Figure B-1. Simplified Block Diagram

The mass equation for the expansion volume is

(2)

where

nE = the number of moles of gas in the expansion volume.

e·
15 Oec 89 B·l
APPENDIX B AccuPyc 1330

When the valve is opened. the pressure will fall to an intennediate value. P2. and the mass bal-
ance equation becomes

(3)

Substituting from equations (1) and (2) into (3):

(4)

or

(5)

then

p.-P2 (6)
VCELL - VSAMP = P P VEXP
2- I

Adding and subtracting p. in the denominator and rearranging gives

(7)

Dividing by (P. - Pv in both the numerator and denominator

VEXP (8)
VSAMP = VCELL- P _P
-1- I •
p.-P2

or

(9)

Since Pb P2 • and p. are expressed in equations (1) through (9) as absolute pressures and equa-
tion (9) is arranged so tbat p. is subtracted from both PI and P2 before use. new Pig and P2g
may be redefined as gauge pressures

(10)

(11)

B-2 15 Dec 89
ACcuPyc 1330 APPENDIX 8

and equation (9) rewritten as

VEXP (12)
VSAMP = VCEll.- P
.:1& _ 1
Pzg

Equation (12) then becomes the working equation for the pycnometer. Calibration procedures are
provided to determine V CEll. and V EXP and the pressures are measured by a gauge pressure trans-
ducer. Provisions are made for conveniently 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 would render equations (1), (2), and (3) inadequate to describe
behavior.

15 Dec 89 8·3
 APPENDIX C

CALIBRATION THEORV
AccuPyc 1330 APPENDIXC

CALIBRATION THEORY

Prior to running samples on the AccuPyc 1330 Pycnometer, the volume of the sample cell and
the expansion volume must be known. The derivation that follows permits these internal volumes
to be measured with respect to a removable, accurately known standard volume. A simplified dia-
gram of the instrument is shown in Figure C-l.

Assume that, V CAllB is removed, V CELL is charged 10 an elevated gauge pressure PI and VEXP is
at zero gauge (ambient) pressure but sealed and that the valve is closed. Upon opening the valve,
the condition established is

(1)

where Pz is the resulting intermediate pressure. The use of gauge pressures is permissible be-
cause it is equivalent 10 having subtracted a constant ftom both sides of the equation.

Sampie Cell Volume Expansion Volume

Valve
VCEll VEXP

G
Figure C-l. Simplified Diagramfor CaUbration

Placement of VCAllB into V CELL and repetition of the charging and expansion yields

(2)

Where PI * and Pz* are the before and after expansion pressures with VCAllB in place.

VCAllB, PI> Pz, PI*, and Pz* are assurned to be known or measurable. V CELL and Vsxp are 10 be
found. Solving equation (1) for VHXP yields

(3)

15 Dec 89 C-1
APPENDIXC AccuPyc 1330

Substitution of equation (3) into equation (2) yields

(4)

Gathering tenns and solving for VCBLL further yields

(5)

Substitution of experimental and known values into equation (5) yields VCBLL which when used
in equation (3) yields VEXP. the desired result.

C-2 15 Dec 89
 APPENDIX D

FORMAT OF TRANSMITTED DATA

AccuPyc 1330 APPENOIXO

FORMAT OF TRANSMITTED DATA

The following tables describe the fonnat and meaning of data in transmitted reports. Each re-
cord is tenninated by a carriage return and line feed.

Table D-l. Calibration Report F0111Ult

Record
Information Conveyed Form
Number

1 Carriage retum/linefeed
2 Version number of the AccuPyc software 20 characters
3 Serial Number 1 integer
4 Report type = calibration 11 characters
5 Calibration standard size 1 floating pt.
6 Number of purges 1 integer
7 Equilibration rate 1 floating pt. +
9 characters
8 Average cell volume 1 floating pt.
9 Cell volume standard deviation 1 floating pt.
10 Average expansion volume 1 floating pt.
11 Expansion volume standard deviation 1 floating pt.
12 Number of runs 1 integer
13 Raw data - Pressure of data points
PI P2 Pl* P2* I floating pt.
Units (psig or kPag) each
xxx.xxxxbxxx.xxxxbxxx.xxxxbxxx.xxxxbcccc 4 characters
b = blank
14 Reduced data
Cell volume 1 floating pt.
Cell volume deviation 1 floating pt.
Expansion volume 1 floating pt.
Expansion volume deviation 1 floating pt.
xxx.xxxxcxxx.xxxxbxxx.xxxxcxxx.xxxx
c = * or blank
b = blank

An asterisk after the cell or expansion volume indi-

cates that the value is excluded from the average
calculation.

Records 12 and 13 are repeated for each run.

15 No data message 40 characters

22 Aug 90 0-1
APPENOIXO AccuPyc 1330

Table D-2. AfUllysis Report Format

Record
Information Conveyed Form
Number

1 Carriage return/linefeed
2 Version number of the AccuPyc software 20 characters
3 Serial Number 1 integer
4 Report type = aoalysis 8 characters
5 Sampie 10 20 characters
6 Sampie weight 1 floating pt.
7 Number of purges 1 integer
8 Equilibration rate I floating pt. +
9 characters
9 Cell volume I floating pt.
10 Expansion volume I floating pt.
11 Average volume 1 floating pt.
12 Volume standard deviation I floating pt.
13 Average density 1 floating pt.
14 Density standard deviation I floating pt.
15 Number of runs 1 integer
16 Raw Data - Pressure of data points
PI P2 1 floating each
Units (psig or kPag) 4 characters
xxx.xxxxbxxx.xxxxbcccc
b = blank
17 Reduced Data
Volume 1 floating pt.
Volume deviation I floating pt.
Density 1 floating pt.
Density deviation 1 floating pt.
xxx.xxxxcxxx.xxxxbxxx.xxxxcxxx.xxxx
c = * or blank
b = blank

An asterisk after the density or volume value indi-

cates that the value is excluded from the average
calculation.

Records 15 and 16 are repeated for each run.

0-2 22 Aug 90