A.

Develop a safety checklist for use before operation of this

experiment

The checklist is used by the operator to ensure that the apparatus is safe

to begin the procedure. Normally, the checklist would not include basic

safety equipment in the laboratory, such as a fire extinguisher, safety

shower, MSDS sheet unless the item is unusual.

The pre-start-up checklist might include the following item:

i. Apparatus is in pre-start-up mode: valve V1 to V5 closed, pump P1

off, heater and temperature controller off, stirring motor in reactor

off, water and acetic anhydride stock tanks empty.

ii. Rotameters must be recently calibrated.
iii. Adequate feed stock must be available for the entire procedure.
iv. Feed stocks must be certified as proper chemical and proper

concentration.
v. Hood containing apparatus must be functioning with a positive

indication of adequate air flow.

vi. Spill kits must be available.
vii. Operator has had proper PPE, including compatible gloves, apron,

goggles.
viii. Water level in the recirculating bath must be adequate.
ix. Check integrity of all lines.
x. Open and close all valves fully to insure proper operation.
B. What safety equipment must be available

i. Operating hood for apparatus.

ii. Spill containment for all storage tanks, reactor and sample point.
iii. Spill kit.
iv. Proper PPE for operator, including compatible gloves, goggles,

aprons.
v. Safety shower, eyewash station in laboratory.
vi. Fire extinguisher in laboratory.
vii. MSDS sheets for all chemicals used.
C. Perform an informal safety review of the experiment. Suggest
modification to improve
the safety.
i. Operation of the apparatus in a hood.
ii. Spill containment for all storage vessels, reactors and sample

points.
iii. Lids for all storage vessels and reactors to reduce vapor

emissions
iv. Aniline is the most hazardous material used in the procedure. It

has and IDLH of 100ppm. The titration must be done with in a

functioning hood using appropriate PPE.

v. The acetic anhydride is combustible, with flash point of 120oF and

an IDLH of 200ppm. It has a strong vinegar like odor.

vi. All electrical connection must be to a properly wired ground fault

interrupter system.
vii. A visual flow meter in the water recirculation loop is suggested.

This would provide a visual indication on the event that the

recirculating pump failed.

viii. A separate temperature measurement in the reactor is suggested
Recommendation to improve the safety of the experiment

1. Operator must ensure that feed lines are open and unplugged prior

to operation.
2. Operator must check to ensure that the feed stock materials are the

proper chemicals at the proper concentration.

3. Rotameters must be recently calibrated.
4. Update operating procedure to ensure that flow is adjusted aster

stock has been added to stock tanks.

5. Operator must check status of valves prior to operation to ensure

that they are functioning properly.

6. Valves must be of proper type and material of construction to be

compatible with chemicals.

7. Check and update maintenance procedure for valves, lines, and

rotameters.
8. Check pre-startup procedure to ensure that spill kits and proper PPE

are available to handle spills. Operator must be trained for spills.

9. Check that lines are proper material of construction for chemical

used.