4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C.

V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

Mercury Porosimeter
Standard Operating Procedure
Revision: 3.0 Last Updated: Mar.31/2015, Revised by Nathanael Sieb

Overview
This document will provide a detailed operation procedure of the Micromeritics Autopore IV Porosimeter. Formal Training is required for all users prior to using the system.

Revision History
#

Revised by:

Date

Modification

Nathanael Sieb

2014-03-27

Initial Release

Nathanael Sieb

2014-08-26

Added details on weighing penetrometer

Nathanael Sieb

2015-03-31

Added comments on independent penetrometer cleaning

4
5

Document No. 4DSOP000X

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

Table of Contents

General Information ................................................................................................................................. 3

Operation ................................................................................................................................................ 4
1. System Description ........................................................................................................................... 4
2. Sample Loading ............................................................................................................................... 5
3. Low Pressure Analysis ...................................................................................................................... 8
4. High Pressure Analysis ................................................................................................................... 10
5. Cleaning Penetrometer ................................................................................................................... 14
6. Data Collection .............................................................................................................................. 16
7. Penetrometer calibration (staff only) ............................................................................................... 17
References and Files ............................................................................................................................... 17
Contact Information ............................................................................................................................... 17

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

General Information
The Autopore IV uses pressurized mercury to measure the pore sizes in materials. This 9500 model
has two low-pressure ports and one high-pressure port. Mercury is injected into the materials at increasing
pressures up to 33,000 psi. The intrusion volume is measured at each pressure, which corresponds to the
volume of pores for various pore sizes. This is a destructive testing method, and the sample must be disposed of in the mercury waste after testing.
Mercury is a hazardous material. Please make sure you read the MSDS for mercury, which is
with the tool. The primary risks of exposure using this tool are inhalation and skin contact. Every effort
has been made to minimize the risks, but as with all laboratory practices, the user must follow safe procedures. All users are required to complete training prior to using this equipment. All users must wear
gloves (latex or nitrile), lab coats, and safety glasses when handling the penetrometer. Only staff is permitted to refill the mercury or perform maintenance on the tool. Cleaning the penetrometer must be done in
the fume hood with a trained buddy present. If there are any spills or other problems, inform a
staff member immediately.
Users may be allowed to clean the penetrometers independently during regular working hours if
they have run more than 5 samples with a buddy and use the system at least twice per month. Please contact 4D LABS staff if you are interested in permission to clean penetrometers without a buddy present.
This system produces high pressures up to 33,000 psi. Do not attempt to open any ports unless
the Pressurized indicator lights are off (more details in procedure).

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

Operation
1. System Description
The Autopore IV 9500 has two low pressure ports and one high pressure port. The low pressure
port is primarily used for filling the penetrometer with mercury. The high pressure port collects the majority
of the data.

low
pressure
ports

high
pressure
port

If there is an emergency, power to the entire system can be shut-off by turning off the power bar.

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

The status lights tell you if any of the ports are pressurized, and the level of mercury in the degasser chamber.

The cart contains all supplies including the penetrometer, Mercury QuikVac, and mercury spill kit.

2. Sample Loading
1. Create an entry in the log book for the tool.
2. If necessary, turn on the porosimeter with the switch at the back of the system (staff only).
3. Weigh the sample material to be analyzed. Aim for ~300 mg if possible, but this number ultimately be determined by the material and expertise of the user.

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

4. IMPORTANT: Put on gloves, goggles, and a lab coat. Take out a Ziploc bag and label
it for mercury waste.

5. Remove the penetrometer from the case and prepare the wrench set.
penetrometer

stem

head
6. Place the penetrometer in the holder and use the wrench to release the locking ring.

loosen

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

7. Open the penetrometer and place the sample in it.

8. Use a tiny amount of vacuum grease and apply it around the edge of the penetrometer.

9. Close the penetrometer, place it in the holder, and tighten the locking ring.

tighten
10. Remove the metal rod from the low pressure port and put it on a paper towel on the porosimeter.
Insert the penetrometer into the low pressure port and tighten it so that it is well restrained.

11. IMPORTANT: Remove gloves and dispose of them in mercury waste bag before using
computer.

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

3. Low Pressure Analysis

1. Start Autopore IV 9500.
2. Select Open Sample Information (or F2) Click ok to create a new file.

3. Select replace and choose a similar sample.

4. Update the weight of the sample and choose the analysis conditions.

5. Select the correct penetrometer s/n.

6. Check the pressure values (nothing greater than 30,000 psi!). Save and close.

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

7. Select Unit 1 Low pressure analysis

8. For appropriate port, select the file to run.

9. Click next to check the setup values.

10. Press start when ready.
11. The system will evacuate the penetrometer to 50 umHg and wait 5 minutes. The entire evacuation
process may take 30 minutes or more. If the pressure does not reach 50 umHg after 1 hour but is
less than 100, then the user press Skip to go to the next step.

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

12. The system will fill the penetrometer with mercury and begin the analysis. During the analysis, the
system will measure the intrusion volume at each pressure specified in the analysis conditions.
13. IMPORTANT: Put on gloves, goggles, and a lab coat.
14. The analysis is complete when the Status of the tool returns to Idle.

15. When complete, remove the penetrometer from the low-pressure port and place in the Rubbermaid tub. IMPORTANT: Keep the penetrometer stem pointing UP to avoid spilling any
mercury.

4. High Pressure Analysis

1. Measure the weight of the penetrometer, sample, and mercury. Use the black weighing support.

10

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

2. Load the sample in the high-pressure port. (remember to wear gloves, goggles, and a lab coat)

3. The vent valve should be open when tightening. Work slowly and move forward and backward to
remove air bubbles.

vent valve

open
close
4. IMPORTANT: Remove gloves and dispose of them in mercury waste bag before using computer.

11

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

5. Select Unit 1 High pressure analysis

6. Select the file to run, input the Assembly Weight, and press start.

7. Open the vent valve when prompted and close it when prompted.
8. System will analyze samples at the pressures defined in the Analysis Conditions to complete the
report.

9. Wait for the system status to return to Idle and the red Pressurized light to turn off.
LED
off

10. IMPORTANT: Put on gloves, goggles, and a lab coat.

11. Open the vent valve.

12

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

12. Open the high pressure port.

13. Place the grey tray on the deck top.

14. Remove the penetrometer and allow most of the oil to drain off the outside of the penetrometer
back into the high pressure port. IMPORTANT: Keep the penetrometer stem pointing UP to avoid
spilling any mercury.

15. Wipe the majority of the oil off using paper towels. Dispose of the paper towels in the mercury
waste bag.
16. Place the penetrometer in the case.

13

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

17. Dispose of gloves in the mercury waste bag and return the high-pressure port to a closed condition.

5. Cleaning Penetrometer
1. REQUIRED: You must have a buddy present for the entire cleaning procedure.
2. IMPORTANT: Put on fresh gloves, goggles, and a lab coat for all cleaning steps. Do
not wear both gloves while walking in the hallway.
3. Take the following items to the 3 hood in the Wet Lab (TASC2 6074): Grey tray, penetrometer
contained in case, mercury waste bottle, wrench, holder, penetrometer cleaning brush, Ziploc mercury waste bag, and Mercury QuikVac (all items in picture below).

4. Make sure the fan speed in the Wet Lab is set to High.
5. Place the grey tray inside the fume hood.

14

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

6. Carefully open penetrometer by holding the stem over the mercury waste bottle and rotating the
locking ring clockwise. Allow the mercury to drain from the stem into the waste bottle.

open

7. Drain any remaining mercury and sample material from the penetrometer head into the waste.
8. Use the QuikVac to clean up any spilled mercury.

9. Add some soapy water to the bottom of the grey tray.

10. Wipe down all tools and containers with the soapy water. Dispose of all paper towels in the mercury waste bag.

15

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

11. Clean the inside and outside of penetrometer with soap and isopropanol. Use scrubs and paper
towels as needed.

12. IMPORTANT: Do a visual inspection of every item after cleaning before removing
from the fume hood. Look for any shiny mercury droplets.
13. After every item is completely cleaned, use the QuikVac to remove any mercury from the grey tray.
14. Drain all water from the tray into the red waste container. IMPORTANT: Do not allow any of
the water to go down the drain.
15. Dispose of any remaining paper towels and gloves in the mercury waste bag.
16. Return all supplies to room 6140 beside the porosimeter. Inform a staff member about the Ziploc
mercury waste bag.

6. Data Collection
1. Select Save As on the automatically generated report.

16

4D LABS, Simon Fraser University 8888 University Drive, Burnaby, B.C. V5A 1S6
E nanofabrication@4dlabs.ca T 778.782.8084 F 778.782.3765 W www.4dlabs.ca

2. Choose whether to save it as a .rpt (only can be opened in Autopore IV), .txt, or .xls (recommended for excel).
3. An old report can be recalled by selecting Reports Start Report.
4. Select the sample file needed and choose Screen as the output. The report can then be saved as
described above.

7. Penetrometer calibration (staff only)

1. Weigh empty penetrometer.
2. Run low pressure analysis to fill penetrometer with mercury.
3. Weigh filled penetrometer.
4. Open Penetrometer properties.
5. Enter weights and calculate volume of mercury for the penetrometer.

References and Files

Autopore IV Manual and training notes.

Contact Information
Questions or comments in regard to this document should be directed towards Nathanael Sieb
(sieb@4dlabs.ca) in 4D LABS at Simon Fraser University, Burnaby, BC, Canada.

17