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SAFE WORK INSTRUCTIONS FOR: MIL-140C-10 synthesis and the post-synthesis Commented [GK1]: Use same title for RMW & SWI

1. Authorization: Dalal Alqarni Commented [GK2]: Microwave assisted synthesis of ..

, Use of Microwave reactor Commented [GK3]: Via CEM Discover SP Focused
Microwave TM Synthesis System
2. Hazards & risks associated with equipment/machinery/technique/process
Commented [GK4]: and post synthesis vacuum
Chemical filtration, washing and solvent exchange
2,2-Bipyridine-5,5-dicarboxylic acid AND Biphenyl-4,4-dicarboxylic acid. Causes skin Commented [GK5]: Myself or Alan reflecting staff lab
irritation, causes serious eye irritation and may cause respiratory irritation (H315, H319 & H335 area responsibility.
respectively). Commented [GK6]: Link to model (use of the Discover
N,N-Dimethylformamide. Flammable liquid and vapour, harmful incontact with skin, causes serious eye SP Microwave reactor only in accord with manufactures
irritation, harmful if inhaled and may damage fertility or the unborn child (H226, H312, H319, H332 & user manual. Also useful here to give a short elaboration
H360 respectively). of the purpose and scope of the work.
N,N-dimethylacetamide. Combustible liquid , harmful in contact with skin, harmful if inhaled, causes Commented [GK7]: Perhaps these can be grouped with
individual names, DG class and risk phrases but group
serious eye irritation and may damage fertility or the unborn child (H227, H312, H332, H319 & H360 hazard comments to reduce volume? Individual
respectively). chemicals should be sub-points under Chemicals dot
Acetic acid glacial. Flammable liquid and vapour, may be corrosive to metals, harmful in contact with point?
skin and causes severe skin burns and eye damage (H226, H290, H312 & H314 respectively).
Acetone. Highly flammable liquid and vapour, causes serious eye irritation and may cause drowsiness or
dizziness (H225, H319 & H336).
Methanol. Highly flammable liquid and vapour. Toxic if swallowed, in contact with skin or if inhaled
Causes damage to organs (H225, H301 + H311 + H331 & H370 respectively).
Zirconium(IV) chloride. May be corrosive to metals and causes severe skin burns and eye damage
(H290 & H314).
Indium(II) chloride. Causes skin irritation, causes serious eye irritation and may cause respiratory
irritation (H315, H319 & H335 respectively).
Palladium(II) chloride. Toxic if swallowed, may cause an allergic skin reaction and causes serious eye
irritation (H301, H317 & H319 respectively).
Tricarbonyldichlororuthenium(II) dimer. Harmful if swallowed, harmful in contact with skin, causes
skin irritation, causes serious eye irritation, harmful if inhaled and may cause respiratory irritation.
(H302, H312, H315, H319, H332 & H335 respectively).
Rhodium(III) chloride hydrate. Harmful if swallowed and causes serious eye damage. (H302 & H318 respectively).

Sharp: broken glassware from sample tubes. Commented [GK8]: What sample tubes present such a
Environmental stressor: large noise from sonnicator. hazard? Caution might exists for glass Tristar tubes
Electrical: mass balance, sonnicator. where leverage due poor use may lead to breakage. You
might note use of glass manifold system (schlenk line) if
Equipment/Machinery/Vehicles to be used and soxhlet apparatus.
Thermal hazard: Microwave, oven, hotplate.
Commented [GK9]: No use described?
Commented [GK10]: From the step by step instructions
it appears you should provide specification of the
3. Before you start work: Ensure all safety controls are in place and available as required in accord with Microwave reactor and a vacuum system.
the risk assessment, ensure all equipment and supplies are setup ready at hand, ensure a clean tidy Commented [GK11]: Use of these items is not specified
workspace, ensure other users of the workspace are aware of the hazards and risks associated with in the step by step instructions.
your work.
Commented [GK12]: These must therefore be specified
in the RMW.
4. The environment where the task is to be undertaken: Work is restricted to be conducted in
laboratory room 228.

5. Personal protective equipment to be used: Laboratory coat, safety glasses and closed footwear
must be worn at all times, and cryogen thermal gloves and full face mask are to be worn at times in
accord with the risk assessment.

6. Emergency procedures: Take appropriate action to attend and/or safeguard the immediate personal
welfare requirement of relevant persons as is safe to do so and then notify someone else of the
emergency so that appropriate emergency response assistance is available as soon as possible as the
Commented [GK13]: Step by step instructions would
highest priority. Then, as appropriate, contain / isolate any relevant hazards such as by pulling down
do well to incorporate steps specified in user manual;
the fume-cupboard sash, turning off power to any relevant equipment, as appropriate. Use a fire where hazards exist these should be noted in the RMW
blanket or fire extinguisher to extinguish any fires. with controls and risk assessment noted accordingly.

First setup instrument vent line and air supply and

7. After hours access procedures: After hours access must be registered in the departments after hours
power check vent tube connected and vented to fume
experiments log book (maintained at the general office) ahead of time, by 4 pm on any given day in cupboard, [orientation of air/N2 gas pressure regulator
accord with the departments afterhours policy hours, whereby a description of the experiment, the risks, (more installation concern than exp setup)], check air/N2
the location, and the names of both the researcher and their buddy must be specified. Afterhours supply regulated to min 25 PSI (20L/min flow); max 60
access for undergraduate students is restricted to low risk activities being conducted under the direct PSI; then turn on power (Activent auto returns to home
supervision of a senior staff member. position) and login.

8. Step by step procedures for task Prepare sample vessel Select vial (specify which size),
insert appropriate stir bar, detail step by setup addition
MIL-140C-10 synthesis of your reactants (see below), place cap on vial, install
appropriate attenuator then rotate it clockwise until it
locks into position, then place the sample vessel into the
attenuator. Note DiscoverSP is usable only with single
1. MIL-140C-10 will be synthesized by using a microwave-assisted solvothermal method in CEM use CEM supplied 10 and 35 ml reaction vessels and caps
Discover Microwave. A 30-mL glass microwave vial will be charged with 1 mmol ZrCl4 (>99.5%, for sealed reactions. Here you can detail step by step
addition of reactants (including volume/mass amounts)
Sigma-Aldrich) add 0.9 mmol of the ligand (Biphenyl-4,4-dicarboxylic acid) and 0.1 mmol of the
re-iterating hazards and safety controls accordingly as
ligand (2,2-Bipyridine-5,5-dicarboxylic acid). noted in RMW (e.g. gloves, working in fume cupboard.,
2. acetic acid (99.9%, Ajax) and N,N'- dimethylformamide (DMF, >99.5%, Ajax) will be introduced.
3. mixture will be heated with magnetic stirring to 220 C within 1 min, and held at this temperature Perform Method Load/create method, then press start.
Specify here step-by-step exactly how you intend to use
for 30 min
the instrument as in accord with the user manual. Note
4. cooling to 55 C within 2 min. here that the instrument can be run in any of various
5. The precipitates will be isolated by vacuum filtration. modes (Standard, Dynamic, Fixed Power, Power Cycling
6. The precipitates will be washed with N,N'-dimethylacetamide (DMA, >99.5%, Merck, 3 20 mL), and and SPS), which necessitate particular process
acetone (3 20 mL) parameters and safety controls (refer user manual ...
7. Solvent will be exchanged with methanol by using a Soxhlet washing procedure for 16 h. The
Commented [GK14]: Note instrument operation mode
resulting powder will be dried in vacuum. and process parameters.
Commented [GK15]: Seems part of overall
The post-synthesis programmed instrument process control.
Commented [GK16]: This would seem to follow Vessel
1. In a 100-mL round flask, the target metal (0.44 mmol) will be dissolved in 40 mL of acetonitrile. Removal. Add a few more details. Vacuum source.
2. Thereafter, 400 mg of MIL-140C-25 (1.16 mmol) will be introduced and the mixture will be heated at Filter and assembly and collector types. How filtrate will
90 C for 16 h. be labelled and disposed.
3. The resulting bright yellow precipitates will be filtered and washed with acetonitrile (3 x 40 mL) and Commented [GK17]: This could be merged with above
methanol (3 x 40 mL) before vacuum-dried to yield the MIL-140C-M. (M= Ru, Rh, Pd and In) step, then control measures and risk assessment noted in
RMW. It is important that RA for handling individual
9. Clean-up procedures: All work areas are to be kept as clean as possible to ensure a safe work area, chemicals be documented as you have done, nevertheless
as such wastes and rubbish should be disposed of appropriately as soon as possible. Clean-up it is also appropriate to document assessment of
involving chemical contaminations and/or chemical spills should be conducted in accord with the risk processes you conduct in the RMW. Where MSDS do not...
assessment, using the chemical spill kit provided in either the local laboratory or the departments Commented [GK18]: What procedure. Procedure titles
corridors as appropriate, as required, and decontaminating contaminated equipment / apparatus are helpful and useful to link within RMW. Again add
appropriately. Hazardous wastes and/or hazardous contaminated equipment / apparatus must be some more detail: size of apparatus, add reference to
appropriately labelled to alert personnel of the relevant hazards present (including the name of the particular setup design, location, etc.. Use of what type
waste and its related primary and subsidiary dangerous goods classes and stickers, and a listing of the of finger? Product dried in finger within vacuum? Dried
different chemicals contained within the waste and their dangerous goods classes), and then tended to in vacuum or vacuum oven? How are volatiles vented. ...
asap. Commented [GK19]: Can you specify what this is at this
10. Waste disposal procedures: Hazardous wastes and/or hazardous contaminated equipment /
apparatus should be disposed of in accord with the departments procedure for hazardous waste Addition of sequence of chemical structures would be
disposal asap. helpful for the overall process. Remember that this
document is all about clear communication to ensure ...
Commented [GK20]: Perhaps you could introduce a
more result oriented title as would help interpretation of
the following steps. These steps may be introduced as
sub-steps of this overall post-synthesis processing.
Commented [GK21]: Metal chloride? Describe what is
to be done (process to be risk assessed), then clarify why.
Commented [GK22]: Not previously described. Not in
chemicals list. Not in RMW.
Commented [GK23]: You might note as specified above
in step-by-step instructions or as noted below if detailed
Commented [GK24]: Note both yourself and myself
PREPARED BY: Dalal Alqarni. here.
SIGNED: Dalal Alqarni. .. DATE: 19/06/17

Guidelines for the development of safe Responsible Officer: Director, OHS Page 1 of 1
work instructions, v3
Date of first issue: June 2001 Date of last review: November 2009 Date of next review: 2012
Printed copies of this document are uncontrolled copies. For current version check