Micro-Distillation of Process Samples by ISL PMD-110
Area
3
Job Hazards
Unit
Lab
Yes
Operating Procedure #
OPS-LB-PS-017
Job Hazards
Access and Egress
Moving Parts
Activities of Others
Noise
Adverse Weather
Rail Movement
Chemical Exposure
Sharp Edges
Electricity
Slips, Trips, and Falls
Fatigue
Static Electricity
Fire and Explosion
Trip Injuries
Ground Contamination
Trapped Pressure
Manual Handling
Working at Height
Certified by
Yes
Revision #
Scope / Objective
PMD-110 Automatic Micro-Distillation
Analyzer
Y
Standard (SSP-0011)
Full Face Shield / Goggles
Hood
Gloves—Chemical
Personal Fall Protection
References / Documents
Respirator / Filter Mask
Supplied Air
 ASTM D7345
 ISL PMD-100/110 SOP
Materials and Reagents
Citizen IDP-3551 Printer

Use
Clothing—Chemical Protection
Equipment

Page
1 of 2
PPE
This procedure covers the determination of the distillation characteristics of
process samples with boiling range between 20 – 400° C (68 – 752° F) at
atmospheric pressure using an automatic micro distillation apparatus.
Other:
Date
09.20.2011



Granular Pumice Stones
Toluene
10 ml Disposable Syringes with Nozzle
Tube
Special Instructions


ISL 10 ml Mini Distillation Flasks
Acetone
Environmental
Micro-Distillation of Process Samples by ISL PMD-110
1
Place volatile samples in ice bath to chill prior to analysis.
2
Power on the PMD-110 from main switch on rear panel just above power cord.
3
Press any key to bring display to the START menu.
NOTE: If analyzer already on, access the START menu by pressing
panel.
4
(back key) located to left of
key on front
Check and empty the condenser waste beaker if level is too full.
NOTE: Testing cannot be started without the waste beaker in position due to a safety micro-switch.
5
Press the PRODUCT button.
6
Select the sample type from list by navigating the highlighted bar with the arrow pad on keyboard.
7
Press OK button.
8
Press the SMPL ID button and input the alphanumeric sample ID; press OK button.
9
(Optional Step) Press OPER button and select user running test with arrow pad; press OK.
10
Into a clean, dry distillation flask add about 4 – 8 chips of small grain pumice stone.
11
Fill plastic 10 ml syringe with sample; invert syringe and push plunger to 10 ml mark ensuring any air bubbles are removed
Completed Date:
Note:
Prepared By:
Approved By:
This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet.
Micro-Distillation of Process Samples by ISL PMD-110 Continued
Area
3
Unit
Lab
Operating Procedure #
OPS-LB-PS-017
Certified by
Revision #
Date
09.20.2011
Page
2 of 2
Micro-Distillation of Process Samples by ISL PMD-110 (continued)
12
Insert the syringe nozzle into distillation flask (while orienting the side arm of the flask upward) and slowly dispense sample into flask.
NOTE: If sample is dispensed too quickly, spillage will occur which will alter result of the test.
13
Life plastic protection shield up and away from the heating compartment.
14
Attach distillation flask to measuring head assembly ensuring flask is fully seated inside the black rubber lip seal (a click is heard
when properly seated).
15
Ensure spring loaded push rod for heating element is in the lower position.
NOTE: Inspect o-ring on measuring head attachment for any cuts or wear – replace if needed.
16
Insert glass side arm tube of flask to condenser tube gasket opening, then gently press in the spring, clip as you attach measuring
head (missing verbiage that wasn’t able to view on scanned documents).
17
Press the spring loaded push rod for the heating elements to raise it to the upper position against flask bottom.
18
Lower plastic protection shield over the heating compartment.
19
Press START NOW button to begin test.
NOTE: Once distillation is complete, result is automatically calculated and displayed on screen. A print-out of the results will be
automatically initiated.
20
An audible alarm will sound at end of test – press button with picture of bell (
21
Press button for ACQUIT to silence alarm.
) to display alarm condition; i.e. “end of test”.
NOTE: At end of test, the heater compartment cooling fan will run for five minutes.
22
Lift plastic protection shield and press spring loaded push rod to lower flask heating element.
23
Once distillation flask has cooled, press spring clip of the measuring head and gently pull it from the connection.
24
Remove distillation flask from measuring head and place in flask holding device.
25
Immediately wipe liquid condensate from measuring head with a lint free tissue – wipe both temperature probes and the upper hole
around the black sealing ring.
26
Return the measuring head to the holder.
27
Clean distillation flask first with toluene and then with acetone.
28
Return distillation flask to holder in the inverted position to allow it to drain.
29
If any flasks are heavily coated with carbon residue, place them in muffle furnace to clean.
Completed Date:
Note:
Prepared By:
Approved By:
This procedure is only valid at the time of printing. The control version can be found on the Meraux Refinery intranet.