DEPARTMENT OF CHEMISTRY TEACHING LAB EXPERIMENT RISK ASSESSMENT FORM This form must be completed jointly by the Lab Officer in charge and the Lecturer in charge. A hardcopy of the completed form should be kept in a file together with the Project Risk Assessment. Name of Lecturer in Charge Name of Lab Officer in Charge Module / Expt No. A/P Jaenicke Stephan Activity being assessed: Tan Lay San CM2263/Expt. 2 Synthesis & Modification of a Zeolite A) Preparation of pure zeolite NaY 2A1 + 2NaOH + 6H2O 2Na[Al(OH)4 + 3H2, (1) or 2A1 + 2OH + 6H2O 2Al(OH)4 + 3H2 SiO2 + NaOH NaSiO2OH dissolved (2) Al(OH)4 + Na[SiO2OH] Na[(OH)3A1OSiOOH + OH or Al(OH)4 + [SiO2OH] (HO)3A1OSiOOH + OH (3) B) Synthesized zeolite is converted into high silica faujasite xSiCl, + Na56(A1O2)56(SiO2)136 Na56-x(A1O2)56-x(SiO2)136+x + xNaCl + xAlCl3 (4) Known or expected hazards associated with the activity: Hazards of reagents, solvents and known reaction products. State each substance and the approximate amounts to be used/produced. List of activities involved in this experiment which inevitably entail risks. The following are the activities being use: 1) Glass Apparatus. Refer to prepared risk assessment on Use of Glassware 2) Hotplate/Stirrer, Furnaces, Oven. Refer to prepared risk assessment on Use of Laboratory Heating Equipment 3) Electricity. Refer to prepared risk assessment on Use of Standard Electrical Equipment 4) Pump. Refer to prepared risk assessment on Use of Reduced Pressure or Vacuum 5) Fume Hood. Refer to prepared risk assessment on Use of Fume Hoods 6) Disposal of Syringe with metal needle, Pasteur pipettes. Refer to prepared risk assessment on Use and Disposal of "Sharps" 7) X-Ray Radiation. There isn’t any radiation detected outside the equipment. The radiation source is cut off once the main door of the equipment is open. Metallic Aluminium: 1.35 gm (prepare half the scale) Page 1 of 10 Printed on: 16 February 2016 No hazardous product as specified in Directive 67/548/EEC Silicone Tetrachloride: ~5 ml Material is extremely destructive to tissue of the mucous membranes and upper respiratory tract, eyes, and skin. Inhalation may be fatal as a result of spasm, inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema. Symptoms may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea, and vomiting. Sodium Hydroxide: 46 gm (prepare half the scale) Poison! Causes severe respiratory tract, eye & skin burns. May be fatal if swallowed. Harmful if inhaled. Causes damage to the following organs: lungs, respiratory tract, skin eye, lens or cornea. 0.01 M Hydrochloric Acid: for washing Products with a low hazard potential. Silicic Acid Hydrate, Powder: 45 gm (prepare half the scale) Irritating to eyes and respiratory system. Harmful by inhalation Aluminium Sulphate: 31.5 gm (prepare half the scale) Dust may harm or irritate the respiratory tract due to the formation of acidic sulphur compounds via hydrolysis. Ingestion may cause abdominal, nausea vomiting and gastrointestinal inflammation. Purified Nitrogen Nitrogen is colourless, odourless gas. The main health hazard associated with releases of this gas is asphyxiation, by displacement of oxygen. Symptoms of over-exposure by route of Exposure: The most significant route of over-exposure for Nitrogen is by inhalation. Liquid Nitogen The most significant hazard associated with this gas is inhalation of oxygen-deficient atmospheres. Symptoms of oxygen deficiency include respiratory difficulty, ringing in ears, headaches, shortness of breath, wheezing, headache, dizziness, indigestion, nausea, and, at high concentrations, unconsciousness or death may occur. The skin of a victim of overexposure may have a blue color. Contact with cryogenic liquid or rapidly expanding gases (which are released under high pressure) may cause frostbite. Symptoms of frostbite include Page 2 of 10 Printed on: 16 February 2016 change in skin color to white or grayish-yellow. The pain after contact with liquid can quickly subside. Refer Handling, Transportation and Storage of Liquid Nitrogen and other Cryogenic Material 10% Potassium Hydroxide: 500ml Corrosive. Causes burns. Harmful. Zeolite NaY Irritant. Irritating to eyes, respiratory system and skin. *amount stated are computed for the whole experiment. Incompatible materials (special precautions): Metallic Aluminium Substance to be avoided: reaction which by analogy cannot be excluded acids, alkalis, oxisdizing agent, halogens, nitrates, sulfates, sulfides, alcohols, ammonium compounds, alkali hydroxide, alkali salts, halogenated hydrocarbons, semimetallic oxides, nonmetals, nonmetallic oxides, halogen-halogen compounds, metallic oxides,metallic salts, air, oxygen, mercury compounds, semitallic halides, non-metallic halides, water Silicone Tetrachloride Water, alcohols, primary,secondary amines, ammonia, metals, dimethyl sulphoxide Conditions of reactivity: Normally stable Hazardous decomposition products: Hydrochloric acid, silicic acid. Sodium Hydroxide Reactive with organic materials, metals, acids, moisture. 0.01 M Hydrochloric Acid Conditions to Avoid: Heating. Materials To Avoid: Metals (generation of hydrogen). The generally known reaction partners of water. Further information: Unsuitable working materials – metals, metal alloys. Silicic Acid Hydrate, Powder Protect from moisture. Strong acid. Hydrogen fluoride. Purified Nitrogen Page 3 of 10 Printed on: 16 February 2016 Stability: Normally stable in gaseous state. Materials with which substance is incompatible: Titanium is the only element that will burn in Nitrogen. Lithium reacts slowly with Nitrogen at ambient temperatures. Conditions to avoid: Contact with incompatible materials. Cylinders exposed to high temperatures or direct flame can rupture or burst. Liquid Nitrogen Titanium is the only element that will burn in Nitrogen. Lithium reacts slowly with Nitrogen at ambient temperatures. Also, use of Liquid Nitrogen in cryogenic grinding of fatty materials can lead to an explosion. A mixture of magnesium powder and Liquid Nitrogen reacts very violently when lit with a fuse, forming magnesium nitride. Liquid Nitrogen is not corrosive to metals, but the extreme cold can make some metals brittle. 10% Potassium Hydroxide: Acids, organic materials, acrolein, nitro compounds, chlorinated solvents, acid anhydrides, phosphorus, potassium, metals. Absorbs CO2 from air. Zeolite NaY Materials to Avoid: Hydrogen fluoride, Strong acids, Strong bases. The risk of injury and its severity likely to arise from these hazards: Silicone Tetrachloride Skin Contact: Causes burns Skin Absorption: Harmful Eye contact: Causes burns Inhalation: Causes severe burns Ingestion: Toxic Sodium Hydroxide Eye: Extremely hazardous in case of eye contact (corrosive). Causes severe eye burns. Skin: Extremely hazardous in case of skin contact (corrosive). Skin contact produces severe burns. Hazardous in case of skin contact (permeates). Inhalation: Extremely hazardous in case of inhalation (lung corrosive). Hazardous in case of inhalation. Ingestion: Extremely hazardous in case of ingestion. May be fatal if swallowed. 0.01 M Hydrochloric Acid Skin Contact: Slight irritations Eye Contact: Slight irritations Page 4 of 10 Printed on: 16 February 2016 Further data: The product should be handled with the care usual when dealing with chemicals Silicic Acid Hydrate, Powder Skin: May cause skin irritation Eye: May cause eye irritation. Inhalation: Harmful if inhaled. Ingestion: May be harmful if swallowed Aluminium Sulphate Skin contact: May irritate Skin absorption: No information available Eye contact: May irritate Inhalation: No information available Ingestion: May be harmful Purified Nitrogen Inhalation: High concentrations of this gas can cause an oxygen-deficient environment. Individuals breathing such an atmosphere may experience symptoms which include headaches, ringing in ears, dizziness, drowsiness, unconsciousness, nausea, vomiting, and depression of all the senses. Under some circumstances of over-exposure, death may occur. The following effects associated with various levels of oxygen are as follows: Concentration symptom of exposure 12-16% Oxygen: Breathing and pulse rate increased, muscular coordination slightly disturbed. 10-14% Oxygen: Emotional upset, abnormal fatigue, disturbed respiration. 6-10% Oxygen: Nausea and vomiting, collapse or loss of consciousness. Below 6%: Convulsive movements, possible respiratory collapse, and death. Health effects or risks from exposure: ACUTE: The most significant hazards associated with this gas are inhalation of oxygen-deficient atmospheres. Symptoms of oxygen deficiency include respiratory difficulty, ringing in ears, headaches, shortness of breath, wheezing, headache, dizziness, indigestion, nausea, and, at high concentrations, unconsciousness or death may occur. The skin of a victim of over-exposure may have a blue color. CHRONIC: There is currently no known adverse health effects associated with chronic exposure to this gas. TARGET ORGANS: Respiratory system. Liquid Nitogen Skin Contact: Contact of the liquid with the skin can lead to severe cryogenic burns or dermatitis (red, cracked, irritated skin), depending upon concentration and duration of exposure. Page 5 of 10 Printed on: 16 February 2016 Eye Contact: Contact of the liquid with the eyes can cause pain, redness, severe cryogenic burns, and prolonged exposure could cause blindness. Contact with the undiluted liquid will cause frostbite, ulceration of the skin (which may be delayed in appearance for several hours), blistering, and pain. Contact with rapidly expanding gas poses a frostbite hazard. Other Potential Effect: Contact with cryogenic liquid or rapidly expanding gases (which are released under high pressure) may cause frostbite. Symptoms of frostbite include change in skin color to white or grayish-yellow. The pain after contact with liquid can quickly subside.Refer to : Handling, Transportation and Storage of Liquid Nitrogen and other Cryogenic Material 10% Potassium Hydroxide: Harmful if swallowed, inhaled or absorbed through skin. Potassium hydroxide solution is extremely destructive to tissue of the mucous membranes and upper respiratory tract, eyes and skin. Inhalation may result in spasm, inflammation and oedema of the larynx and bronchi, chemical pneumonitis and pulmonary oedema. Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. Zeolite NaY Inhalation: May be harmful if inhaled. Material is irritating to mucous membranes and upper respiratory tract. Ingestion: May be harmful if swallowed. Who is at risk? Persons handling the chemicals and as well as those present in the vicinity. Measure to be taken to reduce the level of risk: Proper laboratory attire and safety measures must always be used in order to reduce the level of risk. Wash hands thoroughly after handling. Do not take internally. Eye wash and safety equipment should be readily available. Eye protection: Chemical safety goggles. Hand protection: Gloves. Please refer to prepared PSSO SAFETY Information Center website: http://www.chemistry.nus.edu.sg/PSSO/index.htm#undergrad This experiment should be carried out in a fume hood. Training prerequisites: This assessment should be read by everyone who will be using the above mentioned chemicals. Refer to Completed Risk Assessment forms for common activities: Page 6 of 10 Printed on: 16 February 2016 http://www.chemistry.nus.edu.sg/PSSO/safety/risk/risk.htm#Common Level of risk remaining: The level of risk is low although constant vigilance is necessary to avoid injury. For X-Ray radiation, the level of risk is none (can not be detected by X-Ray radiation detector). Emergency action if : Spill: Silicone Tetrachloride Before dealing with spillages take necessary protective measures, inform others to keep a safe distance and, for flammable materials, shut off all possible sources of ignition. Spread soda ash liberally over the spillage. Transfer to container and arrange removal by disposal company. Sodium Hydroxide Small Spill & Leak: Use appropriate tools to put the spilled solid in a convenient waste disposal container. Large Spill & Leak: Stop leak if without risk. Do not get water inside container. Do not touch spilled material. Use water spray to reduce vapors. Prevent entry into sink. Call for assistance on disposal. Finish cleaning by spreading water on the contaminated surface and allow evacuating through the sanitary system. 0.01M Hydrochloric Acid Take up with liquid-absorbent material. Forward for disposal. Clean up affected area. Silicic Acid Hydrate, Powder & Zeolite NaY Sweep up, place in a bag & hold for waste disposal. Avoid raising dust. Aluminium Sulphate Before dealing with spillages take necessary protective measures, inform others to keep at a safe distance and, for flammable materials, shut off all possible sources of ignition. Transfer carefully into container and arrange removal by disposal company. Wash site of spillage thoroughly with water and detergent. 10% Potassium Hydroxide: Evacuate area. Wear rubber boots and gloves. Absorb on sand or vermiculite and place in closed containers for disposal. Ventilate area and wash spill site after material pickup is complete. Fire: Metallic Aluminium, 0.01M Hydrochloric Acid, Silicic Acid Hydrate (Powder), Aluminium Page 7 of 10 Printed on: 16 February 2016 Sulphate & Zeolite NaY Non-combustible. Silicon Tetrachloride Dry chemicals, carbon dioxide. DO NOT USE WATER Sodium Hydroxide Non-flammable. Purified Nitrogen Fire extinguishing materials: Non-flammable, inert gas. Use extinguishing media appropriate for surrounding fire. Unusual fire and explosion hazards: Nitrogen does not burn; however, containers, when involved in fire, may rupture or burst in the heat of the fire. 10% Potassium Hydroxide: Non combustible. Use extinguishing media appropriate to surrounding fire conditions. Do NOT use water. Is the experiment suitable for out-of-hours operation? Yes No References if any: Aluminium : http://www.sciencelab.com/msds.php?msdsId=9922844 Silicon Tetrachloride :http://www.sciencelab.com/msds.php?msdsId=9924929 Sodium Hydroxide : http://www.seas.upenn.edu/~nanofab/chemicals/MSDS_Base_NaOH.pdf Hydrochloric Acid : http://www.reagent.co.uk/msds/HYDROCHLORIC-ACID-0.01M-MSDS.pdf Silicic Acid: http://www.sciencelab.com/msds.php?msdsId=9927252 Aluminium Sulphate : http://www.sciencelab.com/msds.php?msdsId=9922863 Nitrogen : http://www.airgas.com/documents/pdf/001040.pdf Liquid Nitrogen: http://mems.uwaterloo.ca:8080/download/attachments/917527/Liquid_Nitrogen.pdf?version=1 Potassium Hydroxide, 10% :http://www.westernu.edu/bin/safety/msds/pcc/KOH%2010%25.pdf Page 8 of 10 Printed on: 16 February 2016 Signature of Lab Officer in Charge:……………………………………………………………….. Date:………………………… Signature of Lecture in Charge:………… …………………………………….. Date:… …………………….. Prepared Risks Assessments for standard equipment and operation are with the kind permission of Dr. Ken MacNeil, School of Chemistry, University of Bristol. Page 9 of 10 Printed on: 16 February 2016 Activity being assessed: Note any activity to be used which entail risk (e.g. use of glass vacuum apparatus, high pressures, high voltage, radiation, high temperatures). Give reference to any special protocols to be followed, and if appropriate attach copies to the risk assessment form. State any additional precautions taken to minimise risk. Known or expected hazards associated with the activity: FOR EACH CHEMICAL, read the MSDS and note:a) Particular hazards (e.g. highly toxic, carcinogenic, corrosive, flammable, pyrophoric, explosive, volatile, dust hazard). Note any dangerous combinations of properties (e.g. volatile and toxic). b) Requirements for safe handling (e.g. fume cupboard, inert atmosphere, low temperature). c) How to dispose of residuals Dispose to drain, with water dilution Neutralise, then to drain with suitable dilution To flammable liquid waste receptacle To non-flammable liquid waste receptacle Keep for recovery/recycling Keep for special disposal later (e.g. heavy metals) Double bag and dispose to dry waste Special procedure (specify) Incompatible materials (special precautions) Note any dangerously incompatible materials and hazards arising from contact of any reagents and substances used with common materials such as paper, benches, hoses, etc. Measures to be taken to reduce the level of risk Include hazards of previously unknown products. Location of work – laboratory, open bench, fume cupboard Level of risk remaining: Likelihood and consequences of any accident or unforeseen events whilst carrying out the activity. When this has been done, choose the appropriate procedure:a) Close supervision and/or attendance of trained first-aider needed. b) Specific approval of supervisor needed. c) Training is needed prior-to or during the operations specified. d) Training is complete and only general laboratory competence required. e) No risk perceived. Emergency action: a) Any special requirements to deal with accidental spillage or leakage. b) What to do in the event of accidental exposure (skin contact, inhalation, etc.). Page 10 of 10 Printed on: 16 February 2016