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STANDARD OPERATION PROCEDURE FOR Pyroprobe (C-110)

Date of the last revision: 02/15/2018

Last reviewed
by:__________________________________________Date:__________________________

SOP discussed
with:________________________________________Date:__________________________

Personal Protective Equipment (PPE) Required: Safety glasses, lab coat, and gloves.

(PPE may differ based on the samples and the hazards it possess).

Chemicals used (IUPAC Name, CAS Number, MSDS, Associated Risks


Nitrogen – Nitrogen, CAS Number: 8013-59-0, Contact with rapidly expanding gas may cause burns or
frostbite. Can act as a asphyxiant
Oxygen- Oxygen, CAS Number: 7782-44-7, Oxidiser, May cause or intensify fire. Keep away from
combustible materials. Keep valves and fittings free of oils and grease. Contains Gas is under pressure,
may explode if heated. Continuous inhalation of concentrations higher than 75% may cause nausea,
dizziness, respiratory difficulty, and convulsion.
Helium-Helium, CAS Number: 7440-59-7, Contact with rapidly expanding gas may cause burns or
frostbite. Can act as a asphyxiant
Hydrogen – Hydrogen, CAS Number: 4368-28-9, Flammable. Contact with rapidly expanding gas may
cause burns or frostbite. Can act as a asphyxiant. Acute or chronic respiratory conditions may be
aggravated by overexposure to this gas.

DO NOT OPERATE PYROPROBE UNTIL YOU HAVE BEEN


PROPERLY TRAINED BY THE LAB SAFETY COORDINATOR
1.- Reactor Ensure bypass valve is set to
Setup direct, not to bypass

Pack catalyst inbetween two


layers of quartz wool in a ¼’’
quartz tube

Ensure graphite ferrules spin


freely, replace ferrules that
bind
Attack quartz tube to exit
line first, then inlet line.

Change bypass valve to If pressure drops tighten


reactor and monitor ferrules further
pressure.

Gently place insulation at


furnace openings, do not
pack inside

Set reactor temperature and If reduction is needed place


flowing gas pulsing valve in the down
position with hydrogen flowing
for 30 minutes at 30% open
Check all heat tapes to
ensure lines are properly
heated

2.-pyroprobe Pack 1 mg of sample into


setup pyroprobe tubes, and place
in sample holder

Enable autosampler under


accessory window

3.-Software Open lab solutions, turn on


Setup transfer line to 300°

Go to batch processes, enter


names and labels for each
sample. Include a blank run
before and after samples

Open and check method file


for changes, load method file
into batch processing

If using autosampler copy file


names into autosampler
software

Under details on the right


side ingite the flame

Hit run If doing pulse reactions more


effort will be required with each
sample
Watch pyroprobe for
completion of each sample.
Next sample will need to be
manually started

When all runs are complete


turn off flame under details
window to stop gas flow

Hit stop and confirm stop


batch processing

Remove reactor bed and


dispose of all samples

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