Standard Operating Procedure
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Read the EH&S Standard Operating Procedures Fact Sheet before filling out this form.
Print out the completed form and keep a readily accessible hard copy in the lab (also
keeping an electronic copy is highly recommended).
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Date:
November 9, 2010
SOP Title:
Phoshorous halides/oxyhalides
Principal Investigator:
Richmond Sarpong
Room and Building:
841A Latimer Hall
Lab Phone Number:
(510) 643-2485
Section 1 – Process
Section 2 – Hazardous Chemicals
Phosphorous halides/ oxyhalides (such as phosphorus trichloride, phosphorus tribromide, phosphorus
trichloride oxide, and phosphorus tribromide oxide) are corrosive and very toxic by inhalation or
ingestion. They can cause skin burns, eye damage, and may cause damage to other organs through
prolonged or repeated exposure.
Section 3 – Potential Hazards
Phosphorous halides/oxyhalides react violently with water. Also, they can be fatal if swallowed
or inhaled. They can cause skin burns, eye damage, and may cause damage to other organs through
prolonged or repeated exposure.
Materials to avoid:
Water, strong bases, sodium/sodium oxides, strong oxidizing agents, potassium, ammonia, alcohols,
dimethyl sulfoxide. (DMSO), metals
Section 4 – Approvals Required
Use of phosphorous halides/oxyhalides reagents requires training and the approval of the appropriate
lab member.
Section 5 – Designated Area
Phosphorous halides/oxyhalides should always be used in a fume hood.
Section 6 – Special Handling Procedures and Storage Requirements
Clear all areas where the reagent will be opened prior to use. Do not use any phosphorous
halide/oxyhalide reagents while working alone.
Proper syringe/needle transfer is as follows: All glassware and solvents should be dried prior to the
treatment with any phosphorous halide/oxyhalide reagent. Flame-dried glassware which has been
cooled under an inert atmosphere just before use is ideal. Upon charging a dry flask with dry
reagents/solvents and reaching the desired temperature, the appropriate phosphorous halide/oxyhalide
can be added. Make sure the reagent has warmed to room temperature prior to use.
Phosphorous halide/oxyhailde reagents are typically contained in a Sure-Seal bottle, the septum of
which can be pierced by a clean, dry needle fitted to a Schlenk line which is supplying an inert gas.
This line is used to keep the reagent under a blanket of inert gas during the entire process. The inert
gas flow is adjusted by monitoring of the oil bubbler on the Schlenk line. A clean, dry reagent needle
(<16 gauge) with the appropriate size syringe is used to pierce the septum and inert gas is drawn in to
the syringe, then the needle is removed and the gas inside is expelled to the atmosphere. This process
is repeated several times, piercing the same hole in the septum, to remove most air from the needle and
syringe. Upon purging the needle appropriately, the tip is submerged below the level of reagent and
the required amount is drawn up into the syringe. Be careful to hold the end of the plunger as well as
the joint where the needle and syringe meet.
Once the desired amount of phosphorous halide/oxyhalide reagent has been drawn into the syringe,
the tip of the needle is pulled above the level of reagent, and the plunger is pulled out slightly to draw a
blanket of inert gas into the needle. The needle is then removed from the reagent bottle and quickly
pierced into the septum of the reaction flask. Be careful to hold the needle and syringe together,
as applying force to dispense the reagent can cause them to separate and expose the reagent to moisture.
Once the addition of reagent is complete, the needle can be removed from the reaction flask. The
excess reactive reagent can be expelled into a beaker that contains sodium carbonate. After the
excess reagent has been expelled, the needle can be rinsed with hexanes multiple times, then water.
Clean the needle immediately after use to prevent clogging. To close the reagent bottle, simultaneously
place a piece of tape over the hole formed by the needle while removing it from the bottle. This should seal
the bottle and keep air and/or moisture from entering. Replace the cap and wrap the outside with
parafilm to further ensure safe storage..
Section 7 – Personal Protective Equipment
Wear a laboratory coat made of flame-retardant material or cotton, chemically resistant gloves, and
safety glasses.
Section 8 – Engineering/Ventilation Controls
Work inside the hood. Keep the hood sash as low as possible to prevent spills/splashes outside the
hood.
Section 9 – Spill and Accident Procedures
In case of a fire, use Metal-X, soda ash, or sand for small fires. For large fires, use an ABC fire
extinguisher. Do not use water on the fire. In case of contact with your person, get to the nearest
safety shower immediately. Remove all contaminated clothing and get underneath the running water
quickly.
Spills*
Cover the spill with a 1:1:1: mixture by weight of sodium or calcium carbonate, clay cat litter, and
sand. After the material has been absorbed, slowly add the mixture to cold water. After the mixture
has been allowed to stand for 24 hours, neutralize the solution and decant it down the drain.
*
Procedure adopted from Armour, M. A.; Hazardous Laboratory Chemicals Disposal Guide, 3rd ed.;
CRC Press: Boca Raton, 2003.
Section 10 – Waste Disposal*
Fully quench all of the reagent before disposal. To quench the reagent, slowly add excess sodium
carbonate to the phosphorous halide/oxyhalide in a large evaporating dish. After the material has been
absorbed, slowly add the mixture to cold water. After the mixture has been allowed to stand for
24 hours, neutralize the solution and wash the solution down the drain.
*
Procedure adopted from Armour, M. A.; Hazardous Laboratory Chemicals Disposal Guide, 3rd ed.;
CRC Press: Boca Raton, 2003.
Section 11 - Decontamination
Remove all contaminated clothing, wash all contaminated skin with copious amounts of water.
Section 12 – Process Steps
Process Steps
Safety Measures
Training Documentation
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