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 4, 2010
SOP Title:
Titanium Tetrachloride (TiCl4)
Principal Investigator:
Richmond Sarpong
Room and Building:
841A Latimer
Lab Phone Number:
(510) 643-2485
Section 1 – Process
Section 2 – Hazardous Chemicals
Titanium tetrachloride is extremely moisture sensitive and reacts violently with air and/or water. Upon
reaction with water TiCl4 will also liberate highly toxic gases (HCl gas).
Section 3 – Potential Hazards
TiCl4 is reacts violently upon exposure to water, and as such can be purchased as solutions in an
organic solvent. They must be handled under an inert atmosphere to minimize exposure to both air and
moisture. Inhalation of gases released upon contact with moisture will cause destruction of the tissue
of the mucous membranes and may be fatal. Contact with the skin will cause severe burns and contact
with the eyes will cause damage. TiCl4 may also be harmful if absorbed through the skin.
Section 4 – Approvals Required
Use of titanium tetrachloride reagents requires training and the approval of the appropriate lab member.
Section 5 – Designated Area
Titanium tetrachloride should only be used in the fume hood. Additionally, it should be stored under
inert atmosphere.
Section 6 – Special Handling Procedures and Storage Requirements
Clear all areas where the reagent will be opened prior to use. Do not use any titanium tetrachloride while
working alone.
There are two options for the handling of titanium tetrachloride. The first option is the use of a syringe
and needle; the second is to transfer using a cannula. For smaller amounts of reagent, the preferred
technique is to use a syringe and needle, while a cannula transfer is safer and more practical for amounts
>15 mL. See http://www.sigmaaldrich .com/ etc/medialib/docs/Aldrich/Bulletin/
altechbullal134.Par.0001.File.tmp/al_techbull_al134.pdf for a detailed procedure on proper Schlenk
technique.
Proper syringe/needle transfer is as follows: All glassware and solvents should be dried prior to the
treatment with any titanium tetrachloride. 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 titanium tetrachloride can be added. Titanium tetrachloride is often stored
under refrigeration and must be warmed to room temperature prior to use.
Titanium tetrachloride is contained in a Sure-Seal bottle, the septum of which can be pierced by 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. If either of these comes apart the reagent will come out and will most likely lead to injury and
damage.
Once the desired amount of titanium tetrachloride 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. At this point, the titanium tetrachloride is dispensed, usually slowly to control heat
evolution. 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 of sand. 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
A laboratory coat, gloves and safety glasses should be worn at all times when handling titanium
tetrachloride.
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 contact with your person wipe of excess liquid (to reduce extreme burning upon exposure to
water) and get to the nearest safety shower immediately. Remove all contaminated clothing and get
underneath the running water quickly. The large amount of water should remove hydrochloric acid and
reduce burning.
In case of contact with the eyes, rinse eyes at the eye-wash station for at least 15 minutes and continue
to rinse during transport to the hospital.
In the case of a spill, soak up with inert absorbent materials and dispose of as hazardous waste. Keep in
suitable closed containers for disposal. Do not let the product enter drains and avoid the inhalation of
vapors.
Section 10 – Waste Disposal
Fully quench all reagent before disposal. For the quench of excess titanium tetrachloride, slowly add to
a pre-cooled flask of isopropanol at 0 °C in an ice bath in a dry flask. Control the exotherm by the slow
addition of reactive.
Section 11 - Decontamination
Remove all contaminated clothing, wipe all excess liquid then wash all contaminated skin with copious
amounts of water.
Section 12 – Process Steps
Process Steps
Safety Measures
Training Documentation
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