National Lab Standards for Undergraduate Chemistry (Draft Report)
National Lab Standards for Undergraduate Chemistry (Draft Report)
March 2018
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Table of Contents
SECTION ONE: ...... 10
COMMON IMPORTANT POINTS TO ALL CHEMISTRY LABORATORIES ...... 10
1 EXECUTIVE SUMMARY ...... 10
Terms of Reference for Preparation of Laboratory and Workshop Standards of Undergraduate
Science and Engineering Education program ...... 10
2 INTRODUCTION ...... 11
2.1 BACKGROUND ...... 14
3 LABORATORY STANDARDS FOR TERTIARY CHEMISTRY EDUCATION
(UNDERGRADUATE) ...... 16
3.1 Lab Planning Module ...... 16
3.1.1 Types of Spaces ...... 16
3.1.1.1 Dry Laboratory ...... 16
3.1.1.2 Wet laboratory ...... 17
3.2 Workshops ...... 18
3.2.1 Glassblowing Service ...... 19
3.2.2 Mechanical and Electrical/Electronics Workshop ...... 19
3.3 Storage of Chemicals ...... 19
3.3.1 Principles of Safe Storage ...... 19
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3.3.2 Storage Facilities ...... 20
3.3.3 Storage of Different Materials...... 22
SECTION TWO: ...... 25
Minimum Standards for Undergraduate Inorganic Chemistry Laboratory ...... 25
1. HUMAN RESOURCES (Inorganic Chemistry) ...... 25
1.1 Teaching and support staff ...... 25
1.1.1. English language qualifications ...... 27
1.2. Manpower for Laboratory Cleaning ...... 27
2. INFRASTRUCTURE ...... 28
2.1. Teaching Laboratories ...... 28
3. LABORATORY FACILITIES ...... 30
3.1 Major Instruments and Equipment...... 30
3.2 Other Facilities/Accessories...... 33
3.3 Glassware and Accessories ...... 34
3.4 Chemicals and Reagents ...... 36
4 LABORATORY SAFETY ...... 40
4.1 Storage of Chemicals ...... 40
Introduction ...... 40
4.2 Physical Location ...... 41
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4.3 Chemical Incompatibility...... 42
5 SAFETY MANUAL ...... 44
5.1 Elementary Safety Rules ...... 44
5.2 General Safety Policies ...... 45
5.3 Responsibility for Safety...... 46
5.3.1 Responsibility of the Chemistry Department and Instructors ...... 46
5.3.2 Individual Responsibilities ...... 46
5.3.3 University and Occupational and Environmental Safety Office (OESO) Responsibilities
46
5.4 Personal Protection ...... 47
5.4.1 Maintenance ...... 47
5.4.2 Hygiene ...... 48
5.4.3 Eye Protection ...... 48
5.4.4 Foot Protection ...... 49
5.4.5 Skin Protection ...... 49
5.4.6 Hand Protection ...... 50
5.4.7 Respiratory Protection ...... 50
5.5 General Safety Equipment ...... 50
5.6 Fire Hazards ...... 51
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5.6.1 Electrical Equipment ...... 51
5.6.2 Flammable Liquids ...... 51
5.6.3 Combustible Liquids ...... 52
5.6.4 Safe Handling and Storage of Flammable and Combustible Liquids ...... 52
5.7 Types of Fires ...... 52
5.8 Types of Fire Extinguishers ...... 53
5.9 Chemical Hazards ...... 54
5.9.1 Labeling ...... 54
5.9.2 Laboratory Cleanliness ...... 55
5.9.3 Transport of Chemicals ...... 55
5.10 Rules for Chemical Storage ...... 56
SECTION THREE: ...... 58
Minimum Standards for Undergraduate Organic Chemistry ...... 58
1. Human Resource ...... 58
1.1. Instructors ...... 59
1.1.1. Role and responsibilities: ...... 59
1.2. Laboratory Manager...... 59
1.2.1. Role and responsibilities: ...... 59
1.3. Laboratory Technician (Technical assistant) ...... 60
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1.3.1. Role and responsibilities: ...... 60
2. Infrastructure ...... 61
2.1.1. Building Design Issues ...... 61
2.1.2. Important consideration in designing chemical laboratories...... 61
3. Laboratory Facilities ...... 64
3.1. Fixed chemical cabinets: ...... 64
3.2. Metal cabinets for solvents ...... 64
3.3. Furniture Design, Location, and Exit Paths ...... 65
3.4. Cleanability ...... 66
3.5. Breakrooms ...... 66
3.6. Entries, Exits, and Passageway Width ...... 66
3.7. Inside Laboratory Facilities ...... 67
4. Equipment, apparatus and chemicals ...... 68
4.1. Emergency equipment ...... 68
4.2. Other important equipment ...... 69
4.3. Instruments:...... 69
4.4. Apparatus ...... 69
4.5. Chemicals/reagents ...... 71
5. Chemical Storage ...... 74
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5.1. Flammable liquid storage ...... 74
5.2. Chemical storage groups ...... 74
6. Laboratory Safety...... 76
6.1. Safety Culture and Your Role in It ...... 77
6.2. Personal Protective Equipment (PPE) ...... 77
6.2.1. Hair and clothing (Dressing for the Laboratory) ...... 77
6.2.2. Eye Protection ...... 78
6.2.3. Gloves...... 79
6.2.3.1. Gloves Comparison Chart ...... 79
6.3. Laboratory Protocols ...... 80
6.3.1. Laboratory Environment ...... 80
6.3.2. Housekeeping ...... 81
6.3.3. Labeling Chemicals ...... 81
6.3.4. Inhaling Harmful Chemicals ...... 81
6.3.5. Hazardous waste containers ...... 82
6.3.5.1. Sealing hazardous waste containers ...... 82
6.3.5.2. Labeling hazardous waste containers ...... 82
6.3.5.3. Hazardous waste container storage ...... 82
6.3.6. Disposal of Chemicals ...... 83
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6.4. Important points to be noted ...... 83
7. Guide to Chemical Hazards ...... 86
7.1. Important symbols to be noted ...... 86
7.4 References ...... 87
SECTION FOUR: ...... 88
1...... 88
1.1. Wet lab ...... 88
1.2. Dry lab ...... 89
2. Human resources ...... 90
3. Practical Analytical Chemistry ...... 91
3.1. Minimum standards for instrumental analysis ...... 91
3.2. Chemical reagents required to carry on practical analytical chemistry ...... 93
3.3. Chemical reagents required to carry on real sample analysis ...... 93
4. Laboratory safety ...... 94
4.1. Good safety practices: Do ...... 94
4.2. Bad safety practices: Don’t ...... 95
4.3. Proper labeling and safe storage of chemicals ...... 95
4.3.1. Labeling ...... 95
4.3.2. Storage ...... 96
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4.3.2.1. Pattern of organic chemicals in storage cabinets ...... 96
4.3.2.2. Pattern of inorganic chemicals in storage cabinets ...... 97
4.3.2.3. Some important tips for storage ...... 98
4.4. Safe use of chemical fume hood ...... 98
4.5 References ...... 99
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SECTION ONE:
COMMON IMPORTANT POINTS TO ALL CHEMISTRY LABORATORIES
1 EXECUTIVE SUMMARY
Terms of Reference for Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education Program
1.Review best practices of laboratory standards already in use in Ethiopia and elsewhere in undergraduate programs of science and technology fields, particularly analytical, inorganic, organic and physical chemistry and submit documentation on the same;
2. Define the minimum standards and norms of laboratories in Analytical, Inorganic, Organic and Physical Chemistry to be adopted by the Ministry to be implemented by the existing public universities and the ones to be established;
3. Prepare and present draft reports and standards to group of experts and stakeholders for feedback and comments;
4. Finalize the draft documents based on the comments and feedback from the Academy, Experts and stakeholder workshops before submitting the final report to the Ministry.
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2 INTRODUCTION
Chemistry is fundamental to understanding our environment, new developments in technology, and our society. In other words, it is central to our lives. That’s why chemistry is often called the “Central Science”. Although the traditional division of chemistry into analytical, biological, inorganic, physical and organic chemistry is still applied, these distinctions between chemistry sub-disciplines are fading, and chemistry increasingly overlaps with other sciences. Regardless of the fact that chemistry is usually taught either as a separate discipline or as a complementary component of science as a whole, the molecular perspective, i.e. the properties and behavior of matter lies at the heart of chemistry. Thus the goal of quality chemistry teaching should be to communicate this molecular view to students
and to teach the skills necessary for the students to apply this perspective.
Chemistry programs in higher education should offer their students a wide-ranging and thorough chemistry education that provides them with the intellectual, experimental, and communication skills necessary to become successful scientific professionals. Offering such a program requires an energetic, committed and accomplished faculty/staff, a modern and well- maintained infrastructure, and a rational chemistry curriculum that develops content knowledge and broader skills through the utilization of efficient academic approaches.
Since the establishment of the University College of Addis Ababa (1950), renamed Haile Selassie I University (1962), since 1975 Addis Ababa University (AAU), the number of public universities under the Ministry of Education (MoE) in Ethiopia has dramatically risen to well over 40. While the diversity of institutions and the growth of the student population will significantly contribute to strength in higher education, it is of paramount importance to ensure that the programs offered in all public higher education institutions in the country are appropriate to the educational missions of their institutions. Graduates, who attain a bachelor’s degree in chemistry from the various institutions, must complete all the requirements of an integrated, thorough program including introductory and foundational course work in chemistry and in-depth course work in chemistry or chemistry-related fields
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with a strong emphasis on laboratory experience and the development of professional skills needed to be a competent chemist.
In today’s global world, excellent chemistry education opportunities provided by an institution to its students not only produces competent and qualified chemists, but it also helps new graduates in the transition from undergraduate studies to graduate/professional studies or excellent career opportunities. In this regard, it’s worth to note that in many countries, including Ethiopia, the large majority of undergraduates that complete a bachelor in chemistry do not go to graduate school but enter the chemical, pharmaceutical, food, textile, leather and other allied industries. From the industry perspective, “a chemist who understands how to think, has the technical background, is inquisitive, but who is not necessarily so focused on a particular discipline is what any chemical industry expects from a bachelor’s degree holder in chemistry” (Shannon Bullard, DuPont Chemical Company).
Learning the fundamentals of chemistry is still the key factor, but equally important is the so- called soft skills-collaboration and communications that students can learn in class but more often learn through research experiences and internships. Last but not least, one area that does not receive much attention in academia is safety. The lack of safety training for undergraduate chemistry students in chemical handling and storage; chemical fume hoods; chemical safety plans can cause adverse effects to students during their undergraduate studies and later in their careers, because employers will have to invest considerably in developing safety training courses for their new bachelor’s degree employees.
In summary, in order to support a viable, high quality and sustainable undergraduate chemistry program, the institutional environment must be put in place with a continuing and stable financial support. In this regard there is a clear need that a number of factors need to be given due attention with regard to
Human Resources (Faculty/staff) Infrastructure ( Physical Plant, Instrumentation, Laboratory Safety Resources) Safety and Curriculum
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Within the scope of the “Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education Program” this project aims at developing the minimum standards for undergraduate chemistry studies, sub-discipline Inorganic Chemistry in the areas of
a) Human Resources b) Infrastructure and c) Safety
to be implemented in all public universities in Ethiopia.
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2.1 BACKGROUND
Ethiopia’s higher education infrastructure has grown rapidly in the last 20 years. From just two universities some 20 years ago, the country has built 51 (47 public and 4 private) universities excluding Public Technical and Vocational Education and Training Institutions (TVET Institutions) and about 108 private colleges and university colleges over the past two decades. Access to education in Ethiopia at all levels, has improved significantly, with greater numbers of students completing secondary education and continuing on to tertiary education. Since 2010, MoE has adopted the policy of 70:30 university intake ratios in favour of science and technology. While the pace of growth of higher education expansion in Ethiopia has been very impressive, the rapid growth of Ethiopia’s higher education system has come at a cost with daunting challenges (quality, costs, infrastructure and human resources). The quality of these new universities varies widely; from successful research schools, to substandard institutions whose eligibility for a university title is questionable, because they lack the corresponding infrastructure, staff and resources. The major cause for this is that the construction of classrooms, laboratories, office space for teaching staff, libraries and expansion of library collections, basic laboratory facilities, computer labs, and the development of electronic networks lag way behind enrolment expansion. The consolidation of new facilities and infrastructure will certainly take some time. However, at this critical stage, where much has already been accomplished, the primary focus should be on quality assurance and a commitment to appropriate and sustained infrastructure. Cognizant of this key and burning issue, MoE is planning to establish and maintain minimum standards for laboratories and workshops of undergraduate science and engineering education programs of public universities. To this end, MoE has requested the Ethiopian Academy of Sciences (EAS), the sole Government advisor in the area of Science and Technology to undertake the aforementioned task in collaboration with the respected departments of Addis Ababa University. Hence, as part of this undertaking as per the TOR, the minimum standards for laboratories and workshops of undergraduate programs in Chemistry, sub-disciplines, Analytical,
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Inorganic, Organic and Physical Chemistry have been prepared for the following specific areas: a) Human Resources b) Infrastructure c) Laboratory Facilities d) Safety Manuals
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3 LABORATORY STANDARDS FOR TERTIARY CHEMISTRY EDUCATION (UNDERGRADUATE)
Introduction
Academic laboratory buildings include both teaching and research and labs. While teaching labs are unique to the academic sector, academic research labs can be very similar to those of the private (at its infancy in Ethiopia) and government sectors.
Science functions best when it is supported by architecture that facilitates both structured and informal interaction, flexible use of space, and sharing of resources.
3.1 Lab Planning Module
The laboratory module is the key unit in any lab facility. When designed correctly, a lab module will fully coordinate all the architectural and engineering systems. A well-designed modular plan will provide flexibility and expansion.
3.1.1 Types of Spaces
3.1.1.1 Dry Laboratory
The Dry Laboratory Space Type is a laboratory space that is specific to work with dry stored materials, electronics, and/or large instruments with few piped services. The laboratories defined by this space type are analytical laboratories that may require accurate temperature and humidity control, dust control, and clean power. Dry laboratory space types are designed to accommodate scientific equipment and project-specific work patterns. Typical features of dry laboratory space types include the list of applicable design objectives elements as outlined below:
Constant and Reliable Temperature and Humidity: As some equipment and experiments are temperature- and humidity-sensitive, constant conditions are required in Dry Laboratory Spaces to ensure that equipment can perform properly and that experiments produce accurate results. Laboratories are usually supplied with variable volume terminal reheat system with pre-filters
16 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry and after-filters for 90% efficiency. In general, laboratory spaces have positive pressure relative to other spaces with no return air from the laboratory to the other spaces.
Dust Control: Just as experiments and equipment may be sensitive to changes in temperature and humidity, so might they be to dust and other foreign particulates.
Durable/Flexible/Mobile Casework: As working conditions will often change due to new equipment, projects, experiments, dry laboratories are usually fitted with mobile casework to allow for flexibility in the floor plan. This casework is generally a pre-manufactured laboratory metal casework system. Counters are typically a plastic laminate with integral splash.
Reliable, Easy to Access, Wiring System: Due to the flexible nature of the Dry Laboratory, the distribution of critical wiring (Power, Voice data, and Heating, Ventilation, Air Conditioning (HVAC) should be clearly laid out, and easy to access and redirect. Thus, a raised floor system is the recommended system of distribution of critical services for this space type.
Fire and Life Safety: All Laboratory Spaces typically will contain a hand-held chemical emergency fire extinguisher in an emergency equipment cabinet.
3.1.1.2 Wet laboratory
Wet Laboratory space types are laboratories where chemicals, solvents, or other materials are used and analyzed requiring water, direct ventilation, and specialized piped utilities. Wet Laboratory Space Types are unique in that they must accommodate simultaneous and separate ventilation and utility connections at individual lab modules to ensure both the reliability and accuracy of results as well as occupant safety throughout the space. Typical features of wet laboratory space types include the list of applicable design objectives elements as outlined below:
Surfaces: Resilient surfaces are an integral part of the Wet Laboratory space type design. Use epoxy paint for lab walls and monolithic, seamless, chemical-resistant vinyl flooring with integral coved based and heat-resistant plastic films/ sheets finish.
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Separate Laboratory Modules: A Wet Lab space is typically divided into separate laboratory modules that contain individually controlled connections to HVAC, utilities and safety devices. Modules are defined spatially by floor-to-ceiling structural slab with underfloor plenum divider.
While research labs must have air conditioning for temperature control in the space, undergraduate and teaching labs do not need to be cooled, and mechanical systems can be limited to providing heat and ventilation only.
Dust Control: Just as experiments and equipment may be sensitive to changes in temperature and humidity, so might they be to dust and other foreign particulates.
Gas/Utility Services: Utility connections in Wet Laboratory Space Types can include vacuum, pneumatic supply, natural gas, and distilled water. The fittings and connections for each module are connected to the building distribution system for six nominal piping systems. High-pressure gas cylinders (N2, Ar, He) are also used in wet labs.
Fume Hoods: To ensure safe containment of chemicals in use, fume hoods are required to maintain high fume hood face velocity and high air volume. However, in teaching labs (undergrad labs) that are typically not continuously in use by students, using constant air volume fume hoods in these labs will allow the sash to be shut off completely to maximize energy savings. Users should always turn off constant air volume fume hoods and close the sash when they are not in use.
It is also typical of this Space Type to include an acid and corrosives vented storage cabinet located under the fume hood, as well storage for emergency equipment.
Fire and Life Safety: All Laboratory Spaces typically will contain a hand-held chemical emergency fire extinguisher in an emergency equipment cabinet, safety showers, eyewashes, and first aid kits. Moreover, personal protective equipment (PPEs) should be made available at suitable places, where visitors are required to wear them before they enter or pass through wet laboratories.
3.2 Workshops
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3.2.1 Glassblowing Service
A workshop furnished with a comprehensive range of equipment to repair and manufacture basic scientific glassware (vacuum lines, Schlenk tubes, traps, and other common laboratory glassware together with the technical expertise of the staff. 3.2.2 Mechanical and Electrical/Electronics Workshop
1. A mechanical workshop providing maintenance and repairs to laboratory equipment and facilities. Electrical/electronic workshop for testing and repair work of portable electrical and electronic equipment including instrumentation and instrument controllers.
3.3 Storage of Chemicals
Chemical storage is an important part of chemical safety. There is a range of storage facilities suitable for chemicals in the laboratory environment. Several of these are specially designed for the safe storage of different types of hazardous substances. It is important to understand what substances can be safely stored in which storage container.
3.3.1 Principles of Safe Storage
Labeling: All chemical containers must be appropriately and clearly labeled with the following information: Name of substance Hazard category (e.g. corrosive, flammable, oxidizing, and toxic). Compatibility: It is essential to segregate incompatible substances. The improper storage or mixing of chemicals can result in serious incidents and injuries. (See Appendix 1), Incompatibility table for common laboratory chemicals. Minimize quantities: Store the minimum stock levels of hazardous materials that is reasonable for the level of usage in the lab. Large quantities of hazardous materials should be stored in purpose built external chemical stores.
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Remember: LESS IS BETTER- IT IS SAFER!
Maintain good housekeeping. As in all work areas, clutter should be kept to a minimum on general shelving as well as in storage cabinets/cupboards. Maintain good stock control and be aware of time-sensitive compounds such as ethers which once opened and exposed to the air can produce peroxides which are highly explosive. This means a regular review of what is being stored and disposal of surplus or unwanted chemicals. Pay particular attention to expiry dates and the date when a bottle is first opened should be clearly shown on the label. Do not store chemicals under sinks as they may leak and some chemicals react when wet. Store large breakable containers, particularly of liquids, below shoulder height. Storage of other materials e.g. plastic containers, above this height is acceptable provided that there is a safe means of access to the storage location.
Sensible shelf storage – ensure shelves are not so high that workers need to access them via the benches or lab chairs. Keep light and/or infrequently used containers on the higher shelves. Lips on shelves are helpful as is ensuring that chemicals stored on shelves over the centre of the bench, cannot be pushed back and fall off the far side.
Items in cabinets should be stored on trays, whether the trays be integral to the storage cabinet or are additional.
3.3.2 Storage Facilities
Shelving: Provided for storing hazardous substances should be fit for purpose and fitted to an appropriate standard by a competent person. The following principles should be followed in relation to storage on shelves o Do not overload shelves – if they are bowed they are overloaded.
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o Store breakable containers, particularly of liquid and hazardous chemicals below shoulder height. o Store large heavy containers at low level o Where items are stored above this level ensure they are light weight/infrequently used and that there is a safe means of access [e.g. step stool or ladders]. o Central shelving on benches should have raised edges/lips to prevent items being pushed off the other side.
Acid cabinets: Modern versions are made of acid resistant materials [such as polypropylene, HDPE or wood] and contain a tray to catch any leakage or spillage. Wooden cabinets should not be used for storage of oxidizing acids such as nitric or perchloric. Some acid storage cabinets currently in use may be made of metal and after prolonged use will show signs of corrosion. Where acid storage cabinets are acquired for the first time, or old ones replaced these should be acid resistant Acid cabinets should have the proper sign on the exterior;
Flammable solvent cabinets: These are made of either metal or wood with a minimum fire resistance of a half hour (some are to one-and-a-half-hour standard, e.g. BS 476). They should contain a spillage tray made of suitable material that is compatible with solvents. They should have the proper signs on the exterior;
Ventilated cabinets: These are cabinets which are fitted with forced ventilation. They may be free-standing with their own extract system, or may be situated beneath a fume cupboard and attached to its duct. They are designed to safely store chemicals that give off noxious fumes and smells. These fumes are sucked away by the forced ventilation.
Fridges & freezers may be used for storage of certain hazardous substances. However, where the substances are flammable the unit must not contain any internal light source or
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thermostat that could provide a source of ignition for any flammable vapor. Proprietary laboratory fridges and freezers that meet these requirements are available from major lab supply companies, domestic appliances should be avoided. Fume cupboards are not designed or intended to be used as storage areas and they should be kept clear of materials and containers when these are not needed for the ongoing operational work. Materials stored in fume cupboards may disrupt the air-flow making the fume cupboard less efficient and compromising the safety of the user.
3.3.3 Storage of Different Materials
Acids - Concentrated acids must be safely stored inside a suitable cabinet as detailed above. Small quantities of dilute acids, such as used with pH meters, may be stored on the bench providing they are appropriately labeled. Fuming acids, acids chlorides should be stored in ventilated enclosures.
Incompatibles: Alkalis & Flammable liquids are incompatible with acids and must be stored separately. Alkalis - Even although these materials are marked with a corrosive label, as are acids, they must be stored separately from acids since any accidental mixing of the concentrated materials will generate large quantities of heat and fumes. Flammable solvents - (e.g. alcohols, toluene, hexane etc.) should only be stored in specialized flammable solvent cabinets as detailed above. Such cabinets must be clearly labeled and positioned away from doors or other means of escape from the laboratory. Fridges used for flammable substances should be spark-proof. This is to avoid the possibility of an internal light or thermostat control unit providing a source of ignition should a container containing flammable substances leak or break. Maximum quantity of flammable solvent, including waste flammable solvent, stored in a lab area should not exceed 50 litres in total. For working volumes, i.e. those kept on the bench, 500 ml in a suitable closed container should be adequate for most purposes,
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though these should be kept to a minimum and be appropriately labeled as to content and hazard.
Peroxide formation: A significant number of laboratory solvents can undergo auto- oxidation under normal storage conditions to form unstable and potentially dangerous peroxide by-products. This process is catalyzed by light and heat and occurs when susceptible materials are exposed to atmospheric oxygen. The following commonly used laboratory solvents can produce organic peroxides that are significantly less volatile than the solvent in which they are formed, as a result, evaporative concentration or distillation can produce dangerous levels of peroxides.
o diethyl ether, o tetrahydrofuran, o cyclohexene, o glycol ethers, o decalin and o 2-propanol These solvents are sufficiently volatile that multiple openings of a single container can result in significant and dangerous peroxide concentration. The following precautions should be taken in relation to these materials: o All peroxide-forming solvents should be checked for the presence of any peroxides prior to distillation or evaporation. o Solvents containing low levels of free radical scavengers such as the antioxidant Butylated hydroxytoluene [BHT] should be used whenever the presence of the stabilizing species does not interfere with intended application. o Uninhibited materials should be stored with care and frequently checked for peroxide formation. o Peroxide-forming solvents should be purchased in limited quantities and older material in inventory should be preferentially selected for use. o Materials should be stored away from light and heat with tightly secured caps and labeled with dates of receipt and opening.
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o Periodic testing to detect peroxides should be performed and recorded on previously opened material.
Compatibility - Do not store flammable liquids with any of the following: o Concentrated acids, e.g. nitric acid, sulphuric acid, hydrochloric acid o Chlorinated solvents o oxidizing agents, e.g. halogenated substances, peroxides, perchlorates, nitrates) o reducing agents, e.g. sodium borohydride, lithium aluminium hydride must never be stored with flammable solvents since fires and explosions can result after any spillage, even without a naked flame or heat. The cabinet or bin must be kept securely closed at all times to prevent spread of fire. Chlorinated solvents - (e.g. chloroform, dichloromethane (DCM), trichlorethylene) are best stored in ventilated cabinets separately from flammable solvents, because there are violent reactions when certain flammable solvents and chlorinated solvents are allowed to mix. Also, when chlorinated solvents are involved in a fire they can generate toxic gases such as phosgene. They should not be stored with alkali metals such as lithium, potassium or sodium, since any mixing may cause an explosion. They can be stored in metal bins if ventilated storage is not available. Solvent waste - It is very important to keep chlorinated/halogenated solvents in separate containers from other solvents. Solvent waste containers must be clearly labeled as to their contents and must be of appropriate material. The quantity of flammable waste solvent stored in fume cupboards or ventilated cabinets should be the minimum necessary, being limited to the container in use, and the container should be removed when full. This minimizes the fire load arising. Noxious chemicals - Ventilated cabinets are designed to safely hold chemicals which give off noxious fumes and smells. These fumes are sucked away by forced ventilation. Often these are located under fume cupboards and use the same
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extract system as the fume cupboard. However, free-standing units are also available with their own ventilation system. These should be used to store materials such as mercaptans and amines which have a strong smell. They can also be used to store lachrymators. If ventilated cabinets are not available, containers of these noxious materials can be stored in sealed secondary containers which should only be opened in a fume cupboard. Oxidizers - (e.g. peroxides, perchlorates and nitrates) are best stored separately from other materials. Ideally, they should be stored in a bin or cabinet made from metal or other non-organic material. Oxidizing agents must never be stored with flammable solvents or reducing agents since fires and explosion can result after any spillage, even without a naked flame or heat. They should not be stored where they can come in contact with wooden shelves or paper. Perchloric acid is especially hazardous and is best stored standing in a tray filled with sand within a cabinet or bin, away from organic materials or dehydrating agents such as sulphuric acid.
SECTION TWO:
Minimum Standards for Undergraduate Inorganic Chemistry Laboratory
1. HUMAN RESOURCES (Inorganic Chemistry)
1.1 Teaching and support staff
Faculty members are responsible for defining and executing the overall goals of the undergraduate program. The faculty facilitates student learning of content knowledge and development of professional skills that constitute an undergraduate chemistry education. An energetic and accomplished faculty is essential to an excellent undergraduate program. An approved program therefore has mechanisms in place to maintain the professional competence of
25 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry its faculty, provide faculty development and mentoring opportunities, and provide regular feedback regarding faculty performance. The faculty of an approved program should have a range of educational backgrounds and the expertise to provide a sustainable and engaging environment in which to educate students. In addition: • There must be at least two full-time permanent faculty members with a PhD degree, fully committed to the Undergraduate Inorganic Chemistry lectures, laboratory courses supervision and undergraduate research. Two full-time analytical technicians with a bachelor’s degree At least one full-time permanent faculty member with an MSc degree, fully committed and responsible for all undergraduate laboratory courses in Inorganic Chemistry. Two technical assistants with a bachelor’s degree in charge of undergraduate laboratory experiments and laboratory course preparations in chemistry or allied field;
One full-time chromatography technician with a bachelor’s degree in chemistry or allied field; ( common for all four streams) One full-time Occupational and Environmental Safety Officer with a bachelor’s degree in occupational health, safety, or a related scientific field ( biology, physics, chemistry or engineering) A team of technicians for the glassblowing unit
o Chief glass blower/head of glass blowing unit from any field or degree discipline. He/she will have to be trained in glass blowing and design o One assistant glass blower to be trained by the head A team of technicians for the mechanical and electrical/electronics workshop One mechanical and electrical/electronics workshop manager with professional technical qualifications and 5 years work experience responsible for planning, leading, organizing, and supervising the day to day activities of the Workshop Section. o Two technicians, TVET graduates (one for mechanical workshop and one for electrical workshop)
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Student Teaching Assistants. The participation chemistry graduate students (wherever possible) in the instructional program as teaching assistants both helps them reinforce their knowledge of chemistry and provides a greater level of educational support for students they supervise. If graduate students serve as teaching assistants, they must be properly trained and supervised. One storekeeper for glassware store (common facility) One storekeeper for chemicals store (common facility)
The employer should provide opportunities for technical assistants and technicians for upgrading their skills through regular training courses within the country and abroad;
1.1.1. English language qualifications
All technical assistants and student teaching assistants must have reached a minimum required standard of English language and are required to provide evidence of this. If they meet the academic requirements of the course but do not have the required level of English language, the employer should arrange for an intensive English language training course.
1.2. Manpower for Laboratory Cleaning
Laboratory chemical hoods and adjacent work areas must be kept clean and free of debris at all times by the undergraduate students. Particular attention should be given to the following: Keep solid objects and materials (such as paper) from entering the exhaust ducts, because they can lodge in the ducts or fans and adversely affect their operation. Keep the chemical hood with a minimal number of bottles, beakers, and laboratory apparatus; therefore, students should always keep unnecessary equipment and glassware outside the chemical hood at all times and store all chemicals in approved storage cans, containers, or cabinets. Furthermore, students are responsible to keep the workspace neat and clean in all laboratory operations, particularly those involving the use of chemical hoods, so that any
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procedure or experiment can be undertaken without the possibility of disturbing, or even destroying, what is being done. Cleaning personnel are only needed to regularly clean the floors of both the wet and dry laboratories.
2. INFRASTRUCTURE
2.1. Teaching Laboratories
The number of students supervised by a faculty member or by a teaching assistant in a teaching lab should not exceed 30. Teaching laboratories require space for: teaching equipment, such as a reading desk and whiteboards; storage space for student book bags and laboratory coats; Teaching labs must support a wide range of dynamic activity from standard lectures to active team-based inquiry with all the tools and technology necessary to enable any teaching and learning task easily. Many teaching labs have mobile casework (equipped with locks) installed in a way that allows for different teaching environments and for multiple classes to be taught in the same space. Some teaching labs even use casework that a student can easily change in height to accommodate sit-down (76.2 cm.) or stand-up (91.44 cm.) work. The flexibility of the furniture encourages a variety of teaching and learning possibilities. The additional cost of flexible furniture is offset by the amount of space saved by eliminating the requirement for separate sit- down and stand-up workstations. The figures below depict both types of teaching labs.
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Flexible Teaching Lab with 24 stations
Teaching Lab (Casework)
Source: Whole Building Design, National Institute of Building Sciences, 2018
Shared bench space can range from 4.5 to 9 meters per teaching laboratory. It is usually configured as perimeter wall bench or center island bench; and is used for bench top instruments, exhibiting displays, or distributing glass materials. 10 to 20 meters of wall space per lab should be left available for storage cabinets, as well as for built-in and movable equipment such as refrigerators. A typical student workstation is 1 to 1.20 meter wide with a file cabinet and data and electrical hookups for computers. Fume hoods shared by two students should be at least 1.80 meters wide. The distance between student workbenches and fume hoods should be minimized to lessen the possibility of chemical spills.
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For undergraduate courses, write-up areas are usually provided inside the lab. A teaching lab must accommodate more people (i.e., students) and stools than does a typical research lab. Prep rooms, which allow teaching staff/technicians to set up supplies before classes, may be located between two teaching labs. The number of students typically enrolled in a course usually determines the size of the teaching lab used for that course. A typical lab module of 3.2 meters x 9 meters (30 net square meters may support four to six students. An inorganic chemistry lab for 24 students would be approximately 140 square meters. Usually there is very little, if any, overhead shelving in the center of a lab. Overhead storage is at the perimeter walls, and the center of the lab has only base cabinets so as to maintain better sight lines for teaching and learning.
NOTE: The use of unusually hazardous materials may require a dedicated area for such work to most efficiently manage security, safety, and environmental risk. However, it must be noted at this juncture, that such facilities are very unlikely to be required for an undergraduate chemistry course.
3. LABORATORY FACILITIES
3.1 Major Instruments and Equipment
Characterization and analysis of chemical systems require high quality and properly maintained instrumentation and specialized laboratory equipment that are utilized in undergraduate chemistry laboratory teaching.
Nuclear Magnetic Resonance Spectroscopy
An NMR equipment is sensitive and demanding in terms of its location, environment and servicing and also extremely expensive. Ideally, chemistry undergraduate programs should have a functioning NMR spectrometer that undergraduates can use or have access to service of an NMR instrument. Here we have two options:
Room-sized and bench top NMRs each having their own advantages: 30 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry
Large NMR
Cost can exceed USD 1 million for the highest-resolution instruments More sensitive, with higher-resolution spectra Requires helium to cool superconducting magnet Operated from a large console by an experienced specialist
Bench top NMR
Cost is generally below USD100,000 Less sensitive, with lower-resolution spectra Does not require helium, and uses a permanent magnet at room temperature Can be operated by a technician using automating software
SOURCE: NMR instruments manufacturers
As mentioned above, it is very unrealistic to acquire an NMR machine for each public university, due to the high cost and maintenance requirements. Moreover, an NMR machine has a high capacity and one NMR machine can easily cover the requirements of several public universities. Therefore, stable arrangements must be made with proximal sites (to be decided at a later stage) to provide ready access to appropriate NMR instrumentation.
The following instruments must be on site and used by undergraduates:
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Molecular Spectroscopy
Two FT-IR spectrometers (common facility) Three UV-visible spectrometers (common facility)
Chemical Synthesis
At least six high vacuum lines for handling reactive, volatile compounds Two high temperature resistance furnaces Two preparative HPLC systems Four Solvent purification systems Two high pressure autoclaves One freeze dryer
Magnetic and Electrical Properties
Two bench top magnetic balances Six electrical conductivity apparatus
Chemical Analysis
One Flame Atomic Absorption Spectroscopy (common facility) One CHNS analyzer (common facility) One thermogravimetric balance with gas flow facility and differential scanning calorimeter (common facility) One analytical HPLC system Electrochemical instrumentation for cyclic voltammetry and other techniques
Surface Studies
One surface area and chemisorption equipment (common facility)
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NOTE: It is advisable to recruit two full-time analytical technicians and one full-time chromatography technician in charge of the aforementioned instruments (see Section1 : Human Resources)
3.2 Other Facilities/Accessories
One optical polarimeter Two water distillation systems Two vacuum ovens At least six vacuum pumps Six diaphragm/membrane pumps Two Lab Shakers Four centrifuges Bunsen Burners and accessories Clamps and Supports Crucibles Flow meters At least four drying ovens Two refrigerators At least six rotary evaporators Twenty hotplates with stirrers Ten portable pH meters Four Bench top pH meter Six top loading balances Four analytical balances Two Immersion coolers Two Open heating bath circulators Three melting point apparatus One Ice Cube maker (common facility) One freeze dryer (common facility)
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Four Stereo microscopes
3.3 Glassware and Accessories
Air-Sensitive glassware Ampule Beakers Boiling Media Bottles and Caps Burettes Condensers Chromatography TLC Desiccators and Desiccants Diazomethane Generators
Evaporators and Accessories
Extractors Filtration equipment and filter papers Flasks Forceps and tweezers Gas Tubes and Traps Glass Bubblers Glass Chromatography Columns
Glass Condensers
Glass Crucibles
Glass Desiccators
Glass Dewars Glass Dishes
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Glass Distillation Apparatus Glass Distillation Columns Glass Distillation Heads Glass Distillation Traps Dryers and Racks Glass Funnels Glass Stirring Equipment Glass Stopcocks Glass Sublimation Supplies Glass Tubes Watch glasses Glass Vacuum Gauges and Manometers
Glass Vacuum Manifolds
Glassware Adapters
Glassware Kits
Glassware Valves Ground glass joint clips Labels and markers Mortar and pestle Microcentrifuge tubes Parafilm Photochemical Supplies Pipettes Pressure Vessels Racks Schlenk tubes and flasks Septa Spatulas and scoops Stoppers
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Syringes Taper joint clips Thermometers Timers Tongs Tubing Tubing connectors Vials Volumetric flasks Wash bottles
3.4 Chemicals and Reagents
Acetic acid Ammonium hydroxide
Ammonium dichromate Ammonium sulphide
Ammonium molybdate Barium carbonate
Ammonium iron(II) sulfate Barium chlorate
(Mohr’s salt) Benzene
Borax
Ammonium vanadate Butanone (methyl ethyl ketone)
Acetic anhydride Calcium nitrate tetrahydrate
Acetone Carbon disulfide
Aluminum sulphate Ceric ammonium nitrate
Ammonia Charcoal
Ammonium carbonate Chloroform
Ammonium chloride Chlorosulfonic acid
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Chromium potassium sulphate Ferrous chloride
Chromic acid Ferric chloride
Chromic chloride hexahydrate Ferrous oxalate Formaldehyde Chromium trioxide Formic acid Chromium sulfate High vacuum grease Chromium trioxide Hydrazine Collins reagent Hydrazoic acid Cobalt chloride Hydrochloric acid Cobalt(II) nitrate hexahydrate Hydrofluoric acid Copper(I) iodide Hydrogen peroxide Copper (II) oxide Imidazole Copper sulfate pentahydrate Iodine Dichloromethane Iron powder Diethyl ether Iron(III) hexacyanoferrate(II) Diethylenetriamine Isopropyl alcohol Dimethylformamide Lead dioxide Dimethylsulfide Lime Dimethyl sulfoxide Limestone Dioxane Lithium aluminium hydride Ethanol Lithium diisopropylamide Ethyl acetate Magnesium sulfate Ethylenediamine Magnesium chloride Fehling's reagent Magnesium carbonate Fenton's reagent
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Manganese(IV) oxide Potassium chromate
Manganese(II) chloride tetrahydrate Potassium dichromate
Manganese nitrate hexahydrate Potassium bromide
Manganese sulphate Potassium bromide (spectroscopic grade)
Methyl tert-butyl ether potassium ferrocyanide
Millon's reagent Potassium hydroxide
Nickel chloride dihydrate Potassium iodide
Nickel chloride hexahydrate Potassium nitrate
Nickel iodide Potassium oxalate
Nickel nitrate hexahydrate Potassium permanganate
Nitric acid Potassium thiocyanate
Osmium tetroxide Potassium nitrate
Oxalic acid Potassium peroxodisulphate
Oxalyl chloride Pyridin
Palladium(II) acetate Pyridinium chlorochromate
Perchloric acid Raney nickel
Phosphoric acid Silver oxide
Phosphorus pentachloride Silver nitrate
Phosphorus tribromide Sodium
Phosphorus trichloride Sodium amide
Phosphoryl chloride Sodium azide
Nickel sulfate hexahydrate Sodium bis(trimethylsilyl)amide
Paraffin liquid for oil baths Sodium borohydride
Potassium bicarbonate Sodium carbonate
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Sodium chlorite Tin(IV) iodide
Sodium hydride Titanium tetrachloride
Sodium hydroxide Titanium(III) sulfate solution
Sodium hypochlorite Titanium (IV) sulfate
Sodium metavanadate Triethylamine Sodium nitrite Tollens' reagent Sodium silicate Triphenylphosphine Sodium sulfide Urea Sodium sulphite Vanadium pentoxide Sodium tungstate hydrate Yittrium (III) oxide Sulfuric acid Zinc dust Tetrahydrofuran Zinc sulphate Tetramethylammonium hydroxide
Tetramethylsilane
Thiourea
Thionyl chloride
Thiophenol
Tin
Tin foil
Tin(IV) chloride
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4 LABORATORY SAFETY
4.1 Storage of Chemicals
Introduction
Chemical storage is an important part of chemical safety. It is the means by which
chemicals are
kept viable for a future date,
prevented from reacting with other chemicals or the physical environment,
prevented from producing unsafe conditions,
minimizes risks during an emergency.
Incorrect storage may lead to the deterioration of the material to an impure, unsafe or
explosive condition. The integrity of the container may also be compromised.
Chemical containers are often stored in chemical storerooms, laboratory shelves, laboratory
cupboards and safety cabinets. The risk of accidents, unintended chemical reactions and
generation of unsafe conditions may be influenced by the:
Location of the containers
Compatibility of chemicals in the same storage location
Quantity of chemicals stored in containers and in each location
Environmental storage conditions, including:
o temperature
o moisture
o light
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o atmospheric content (both inside and outside of the container)
Age of the chemicals and their containers.
The conditions of storage for unwanted and waste chemicals are also important, as many incidents have occurred where chemicals awaiting collection for disposal have become unstable or reacted with each other.
4.2 Physical Location
Large chemical stores are usually located away from valuable assets, buildings, residences, public places etc. This is done so that damage can be minimized in the unfortunate event of a fire, adverse chemical reaction, leak, spill or explosion or any other unforeseen events. A reasonable distance of separation should be allowed between small stores, laboratory cupboards and valuable assets.
It is important to be aware of factors in the local environment that could increase the risk from chemical storage, and to ensure that storages and such environmental factors are appropriately segregated. Local environmental factors include:
Ignition sources
These include flames, hot sources, sparks and sparking electrical equipment (switches), or sources of static electrical discharges. Flammable material should be separated from ignition sources by physical means or distant Ventilation
o Volatile chemicals should be stored in adequately ventilated areas, to prevent the generation of an explosive atmosphere, harmful atmosphere or unpleasant odors. For example, diethyl ether only requires a concentration of 2 % in air to reach its lower explosive limit. This is equivalent to 2.5 mL in 30 L (a small cupboard space). Flammable liquids should not be stored in cupboards beneath laboratory fume cupboards that have electrical switching equipment such as power points, because of the risk of igniting an explosive atmosphere.
Regardless of the size or location of a chemical storage area, appropriate safety hazard management procedures should be in place and available, including:
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An emergency response plan
Spill containment equipment
Firefighting equipment
4.3 Chemical Incompatibility
Regardless of the type of storage location (chemical store, storage cabinet, cupboard etc.) problems can arise when incompatible materials are stored in close proximity). When storing chemicals consider what would happen if a container leaked or broke - Could it or would it react with those chemicals surrounding it? As a minimum, chemical compatibility / incompatibility of the chemicals located below and to either side of each material need to be considered. For each volatile material, consider - Will the vapors react with other vapors or chemicals within the cupboard?
Such incompatibilities can easily occur if chemicals are stored in alphabetical order. For example, methylated hydrocarbons near nitric acid. Materials should be first separated into compatible classes, then if desired, placed in alphabetical order. In this regard it’s worth to note that A Dangerous Goods Storage Compatibility Chart and Incompatibility of Common Laboratory Chemicals document are available to assist in this process.
Once chemicals have been sorted by Dangerous Goods Class (these are materials or items with hazardous properties which, if not properly controlled, present a potential hazard to human health and safety, infrastructure and/ or their means of transport consideration should be given to any need for:
Storage cabinets
o These are an additional means of safety for chemicals in storage. They have a double-skinned metal construction, with a trough for containing spills at the bottom of the cabinet. They are available for flammable liquids and corrosive substances and must be constructed in accordance with relevant Australian
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Standards requirements. Even if a storage cabinet is used, only the minimum amount of chemicals that are required should be stored in the laboratory.
Containment trays
o These are usually plastic trays with high sidewalls that are used as an initial form of containment if a container leaks. Each tray should hold at least the volume of the largest container placed in the tray. Strong plastic bags may also be suitable, especially if the material is volatile.
Shelf liners
o These are an inexpensive option for protecting the shelving material from damage. Bench protector sheet is used where non-hazardous aqueous solutions are stored.
Container material
o Harsh or highly reactive materials should be stored in containers of appropriate composition. For example, oxidizing agents should be stored in PTFE (Teflon, Polytetrafluoroethylene) or PFA (Perfluoroalkoxy alkanes).
Quantity and Chemical Storage Limit for Laboratories and Other Spaces
The quantity of hazardous materials should be kept to a minimum for efficient operation (LESS IS BETTER- IT IS SAFER!).
This should be, at most, three months demand from a chemical store.
For a laboratory or workshop, a one-week supply should be adequate.
Don’t buy a 2.5 L Winchester bottles of solvent if you only need 100 mL. Even if it works out cheaper per mL, the cost of disposing of unwanted chemicals is often more than the cost of purchasing smaller containers.
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5 SAFETY MANUAL
Introduction
5.1 Elementary Safety Rules
1. Keep this manual within easy access in your laboratory and be familiar with its contents.
2. The safe way is the right way to do your job. Plan your work. Follow instructions. If you do not know how to do the job, ask your instructor or technical assistant.
3. Report to the Safety Coordinator all unsafe conditions, unsafe acts and "near misses" which might cause future accidents.
4. Be able to use all safety devices and protective equipment provided for your use. Know the location and contents of the nearest safety station.
5. Maintain good housekeeping by keeping your work area clean and orderly.
6. Wear proper clothing. Avoid bringing long hair, loose sleeves, cuffs, rings, bracelets, etc. in proximity to moving machinery. Proper shoes are required in the laboratory — no bare feet or sandals.
7. Playing in the lab in any form is dangerous and prohibited. Do not run in laboratory areas or halls.
8. Do not oil, grease, or work on unprotected machinery in motion.
9. All machinery and equipment under repair and adjustment shall be properly "locked out" and tagged.
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10. Know the evacuation procedure for your area, the location of fire exits, the location and use of fire extinguishers, and the proper method of reporting fires.
11. Compressed gas cylinders should be secured firmly. Never move a cylinder unless the protective cap is screwed over the valve.
12. Don't try completely new and untried experiments involving potentially dangerous chemicals without help.
13. Never leave a reaction or experiment running unattended unless you have told your lab partners enough about it to deal with potential hazards while you are away. Leave an overnight form on the door if the laboratory will be unattended.
14. Report every accident or fire, no matter how trivial, at once.
5.2 General Safety Policies
The safety and well being of its students, faculty, and staff come above all other considerations at any Higher Education Institution. No experiment that subjects personnel to unreasonable risk is acceptable, no matter how desirable the information which might be obtained. It is the first duty of instructors, supervisors and all persons in authority to provide for safety in the environment and operations under their control. It is the Chemistry Department's policy to comply not only with legal safety standards, but to act positively, where it can, to prevent injury, ill-health, damage and loss arising from work carried out within its building. The Department seeks to encourage all its members to participate in and contribute to the establishment and observance of safe working practices.
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5.3 Responsibility for Safety
5.3.1 Responsibility of the Chemistry Department and Instructors
The first responsibility for laboratory safety lies with the faculty members in charge of the laboratories. It is their duty to evaluate the safety hazards connected with any experiment and to avoid conducting any experiment which cannot be carried out without excessive risk to personnel or property. It is also the responsibility of the faculty members to be certain that every person working in their laboratories is aware of the safety hazards and safety regulations in the laboratory. It is highly recommended that the person in charge of a laboratory have safety rules posted prominently in convenient locations for everyone to read. All undergraduate teaching laboratory staff have the primary responsibility for enforcing regulations on solvent storage, waste solvent disposal, personal protective equipment, etc., and for reporting problems to the Chemistry Department Safety Coordinator.
5.3.2 Individual Responsibilities
Every undergraduate student of a Chemistry Department must participate either in on-site or online safety training and pass the appropriate online test. Undergraduate students engaged in the use of chemicals and apparatus inside the Department are responsible for protecting themselves and their neighbors. The individual student has to take the initiative in protecting herself/himself from hazards which have been explained to them, e.g. they should protect their own eyes by wearing safety glasses. Their next responsibility is to their neighbors.
5.3.3 University and Occupational and Environmental Safety Office (OESO) Responsibilities
Proper disposal of chemical waste Proper maintenance and distribution of fire extinguishers and fire alarm testing and maintenance of equipment
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Inspection of emergency showers and eye wash equipment Ready availability of personal protective equipment Provision of periodic online safety training is for all personnel working in a lab
planning and presentation of departmental safety meetings keeping alert to new hazards which develop in the use of chemicals and informing responsible bodies of these hazards planning emergency drills maintaining a regular inspection procedure so that at least once each year all research and teaching laboratories have been inspected with reports submitted to the relevant bodies
In addition, the Safety Coordinator is available to help members of the Department with individual safety problems. Potential safety problems should be discussed with the safety coordinator. All accidents or near-misses should be reported. This may help to prevent future accidents.
5.4 Personal Protection
5.4.1 Maintenance
The laboratory should be kept clean and free from litter, by regular maintenance. At the completion of each experiment, equipment should be cleaned and properly stored. Do not let unused equipment or chemicals accumulate in the lab. Do not use the aisles of the lab or the space in front of the emergency escape panels for storage. Dispose of all hazardous wastes in accord with the procedures indicated in this manual. Reagent bottles must be properly labeled — when pouring hold the bottle with its label to your palm to protect the label. Notify your safety officer of bottles whose contents are in doubt.
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5.4.2 Hygiene
Wash hands often — always before eating or leaving the laboratory. Washing should be an instinctive reaction to spillage of any chemical on the skin.
Never eat or drink in the lab — never use lab equipment as a food or drink container.
No food items should ever be stored or even cooled in a laboratory refrigerator. Food and beverages can become contaminated within a very short period of time to a life- threatening level by absorption of chemical vapors. Any food/beverage found in inappropriate areas will be removed without notice.
5.4.3 Eye Protection
Various types of eye protection listed in order of increasing effectiveness include:
Ordinary spectacles
Safety glasses with side shields
Protective goggles, which can be worn over spectacles, if necessary
Face shields
Head shields, which protect all of the head and throat
All persons wear, at least, safety glasses (equipped with side shields), or goggles for eye protection while in the laboratory. In situations in which there is potential of a corrosive chemical being splashed into the eyes, safety glasses or goggles AND a face shield are required. In situations where there is potential for an explosion to occur, head shields are required in addition to safety glasses or goggles. Normal eye protection is required when you are wearing contact lenses since contact lenses provide little to no protection from chemicals in the eye. (In fact, contact lenses can complicate flooding the eye with water should a chemical get in the eye.) Plain lens safety glasses, with side shields should be provided for chemistry employees at no charge. Students who wear prescription glasses, and who do not wish to wear safety goggles must cover the costs involved in being fitted with prescription safety glasses. All undergraduates
48 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry are expected to purchase and wear safety glasses at all times when they are working at their laboratory benches or in any area where hazardous activities could endanger their eyes. Teaching Assistants and faculty supervising them are expected to enforce this regulation at all times. Teaching Assistants are reminded that the safety performance of classes under their regulation is one of the criteria by which they will be evaluated by the faculty.
5.4.4 Foot Protection
All persons in labs must wear shoes (bare feet or sandals are not allowed) and adequate clothing to protect the skin from spilled chemicals.
5.4.5 Skin Protection
Always wear clothing that minimizes the amount of skin that can be exposed to potentially harmful chemicals. Never wear shorts in the lab. A lab coat or apron should be worn when working with hazardous materials. Chemical substances can act on unprotected skin in three ways:
Local Damage The action of many chemicals is limited to the skin itself. Corrosive burns, irritation, and chafing due to loss of skin oils are a few examples.
Sensitization Sensitizer chemicals may not have any initial effect, but will cause the skin to react, during subsequent exposures, to quantities much smaller than would otherwise have any affect.
Absorption The skin provides no barrier against some chemicals, which can penetrate freely and enter the blood stream affecting such target organs as the liver and nervous systems.
A chemical may cause damage by more than one of the above effects. Some examples include chlorinated solvents, such as ethylene dichloride, which will defat the skin causing irritation and tissue breakdown, also can permeate the skin possibly causing liver and kidney damage.
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5.4.6 Hand Protection
Our hands are the body parts most likely to be exposed to chemical contact under normal situations. Even though careful technique may help to avoid direct contact with a chemical; the potential for exposure still demands the use of protective gloves.
The use of protective gloves within the laboratory is essential in many instances. However, it is important to realize that if you are wearing gloves while handling chemicals, you must never come in contact with any item that a person not wearing gloves could. For instance, if you are entering or leaving the lab, DO NOT touch the door handle with your gloves on. While you are clearly unaffected by this action, any contaminants on your gloves will be transferred to the hand of the next person that opens the door with an ungloved hand. Likewise, remove your gloves if you are pressing elevator buttons, using a computer keyboard, using a pen that might also be used later by yourself or another person not wearing gloves, etc. Also, do not touch your face, hair, etc. while wearing protective gloves.
5.4.7 Respiratory Protection
Fume Hoods Fume hoods provide constant respiratory protection in all laboratories in the building. Such protection is adequate for most controlled experiments. In using the hoods in the building, the following facts should be kept in mind.
1. Lowering the sash will increase air velocity and offer greater protection from toxic fumes. Normally the sash opening should be less than 46 cm. It is important to keep the sash below the 46 cm mark. Airflow in the fume hoods should be periodically measured.
2. Placing equipment no less than 12 cm in the hood will also reduce the possibility of fumes escaping into the laboratory.
5.5 General Safety Equipment
In each lab there should be the following safety equipment:
safety shower
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eyewash station
one or two fire extinguishers
fume hood(s)
a first aid kit (which the laboratory teaching staff is responsible for restocking with items purchased at the stockroom)
5.6 Fire Hazards
5.6.1 Electrical Equipment
1. Be careful not to spill flammable liquids around electrical equipment in use.
2. Ground equipment to avoid electrical arc or spark formation from static.
3. Avoid temporary wiring.
4. Replace defective cords.
5. Keep equipment in good working condition.
5.6.2 Flammable Liquids
Any liquid having a flash point below 60 ºC and having a vapor pressure exceeding 2.7 atm. in. absolute at 37.8.
Class IA: flash point below 22.7ºC and B.P. below 37.8ºC Class IB: flash point below 22.7ºC and BP at or above 37.8ºC. Class IC: flash point at or above 22.7ºC and BP below 37.8ºC.
Flammable liquids should be stored in Safety Storage Cabinets.
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5.6.3 Combustible Liquids
Any liquid having a flash point at or above 60ºC.
Class II: flash point at or above 37.8ºC. Class IIIA: flash point at or above 60 ºC and below 93ºC. Class IIIB: flash point at or above 93 ºC.
5.6.4 Safe Handling and Storage of Flammable and Combustible Liquids
Limit the amount of combustibles in the laboratory. Keep combustibles a safe distance from heat sources and stored at least 46 cm below the
ceiling.
Limit the quantities of flammable liquids at any one location to those actually necessary, but not to exceed the limits specified. Use only approved containers, e.g., safety cans or metal drums for all transportation and
handling.
Label all containers used for liquids with the name of the material and the words: "DANGER - FLAMMABLE (or COMBUSTIBLE)" - Keep away from heat, sparks, and open flames - Keep closed when not in use.
5.7 Types of Fires
Many fires are small at origin and may be extinguished by the use of portable fire extinguishers. The proper type of extinguisher for each class of fire will give the best control of the situation and avoid compounding the problem. The classification of fires given here is based on the type of material being consumed.
Class A Fires
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Fires in ordinary combustible materials, such as wood, cloth, paper, rubber and many plastics. Almost any fire extinguisher is effective on a CLASS A fire, but water is the best extinguishing agent.
Class B Fires
Fires in flammable liquids, gases, oil, paint and greases. Foam, dry chemical or CO2 extinguishers are the most effective on CLASS B fires. Do not use water.
Class C Fires
Fires which involve energized electrical equipment where the electrical non-conductivity of the extinguishing agent is of importance. Use Carbon Dioxide or Dry Chemical extinguishers. Do not use water. Class D Fires Fires in combustible metals, such as magnesium, titanium, zirconium, sodium, lithium, zinc and potassium. Use metal fire extinguishing agent at safety stations or sand, or vermiculite.
5.8 Types of Fire Extinguishers
Ideally, there should three main types of fire extinguishing agents in a chemistry teaching laboratory, the carbon dioxide extinguisher, the dry chemical extinguisher, and the metal fire extinguishing agent. Every teaching laboratory should be equipped with two carbon dioxide extinguishers.
Carbon Dioxide (CO2) Extinguishers These extinguishers are intended primarily for use on CLASS B and CLASS C fires. They have a limited range; thus, initial application must start reasonably close to the fire. On all fires the discharge should be directed at the base of the flames using care not to
spread the fire by blasting burning materials around the area. CO2 discharge should be
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applied to the burned surface even after the flames are extinguished, to allow added time for cooling and to prevent possible re-flash. On flammable liquid fires, best results are obtained when the discharge from the fire extinguisher is employed to sweep the flame off the burning surface, applying the discharge first at the near edge of the fire and gradually progressing forward, moving the discharge horn from side to side.
Dry Chemical (ABC) Extinguishers Dry chemical extinguishers are intended for use on CLASS A, CLASS B, and CLASS C fires. The discharge should be directed at the base of the flames. Best results are obtained by attacking the near edge of the fire and progressing forward, moving the nozzle rapidly with a side-to-side sweeping motion with care not to blast flaming liquid around the area. Discharge should be continued after flames are extinguished to prevent possible re-flash. For CLASS A fires the discharge should be continued intermittently to coat flowing areas of CLASS A materials.
Dry Powder Extinguishing Agent (D) Dry powder extinguishing agent is intended primarily for use on metal fires. The application of the agent should be of sufficient depth to adequately cover the fire area and provide a smothering blanket. Additional applications may be necessary to cover any hot spots which develop. Care should be taken to avoid scattering the burning metal. Where the burning metal is on a combustible surface, the fire should be covered with powder, and then a 5 cm layer of powder spread out nearby and the burning metal moved onto this layer, with more powder added as needed.
5.9 Chemical Hazards
5.9.1 Labeling
There are few greater potential hazards around the laboratory than that of unmarked or improperly labeled chemicals. All chemicals must have complete identification securely fastened
54 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry to the container. Chemicals of unknown stability and those which deteriorate with age shall have a preparation date clearly indicated on the label. Disposal of unlabeled bottles is dangerous and therefore very expensive and tightly regulated by law. The purpose of proper labels is multifold: They are required. They indicate the source, supplier, or manufacturer of the chemicals. They indicate the age of the chemical. They warn about the possible hazards. There should be some type of actively updated inventory of the chemicals in the laboratories. Most chemistry laboratories use an excel spreadsheet to maintain an active chemical inventory. 5.9.2 Laboratory Cleanliness
1. The laboratory should be kept clean and free from litter by regular maintenance. Do not let unused equipment or chemicals accumulate in the lab.
2. Reagent bottles must be properly labeled - when pouring hold the bottle with its label to your palm to protect the label. Notify your instructor officer of bottles whose contents are in doubt.
3. Never eat or drink in the lab - never use lab equipment as a food or drink container.
5.9.3 Transport of Chemicals Never transport open containers of chemicals through the hallways, stairs or in the elevator. All chemicals, with the exception of those contained in sealed metal cans, are to be transported in rubber buckets or chemical transport carts (with special dividers to hold glass bottles). Stockroom personnel have to be instructed not to allow any chemicals, except those in sealed metal can, to be removed from the stockroom unless they are transported in a rubber bucket or a chemical transport cart. Persons who transport chemicals less frequently may borrow a rubber bucket to transport chemicals from the stockroom to their labs. Borrowed buckets must be returned to the stockroom or left in the corridor for someone else to use. Do not use a cart without side rails for transporting reagents in glass bottles even when the bottles are in rubber buckets since the buckets may fall from the cart and the bottles may break.
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Gas cylinders must be transported in approved carts with the cylinders secured by straps and capped.
5.10 Rules for Chemical Storage
1. Avoid overhead storage of hazardous liquids and dangerous solids. 2. Use flammable or corrosive cabinets for most storage. 3. Refrigerate flammables only in approved flammable storage refrigerators. 4. Maximum separation of reactive chemicals minimizes risk. Therefore, don't store chemicals in alphabetical order--store by category. Do not store mutually-reactive chemicals near each other - e.g. sodium near the sink or in a sprinkled storage area, acids near bases, organometallics near alcohols. 5. Date ethers and other peroxide-forming compounds upon arrival and follow directions for storage, testing and disposal given in this manual. 6. Respiratory assailants and "stench" compounds should be stored in a properly vented storage cabinet. 7. Store cleanup kits close to storage areas.
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Appendix 1
Incompatible Chemicals
Chemical Incompatible with
Acetic acid nitric acid, peroxides, permanganates
ethylene glycol, hydroxyl-group-containing Acetic anhydride compounds
Acetone hydrogen peroxide
acids, flammable liquids, powdered metals, finely Ammonium nitrate divided organic or combustible materials
Chlorate salts, such as sodium or potassium acids, ammonium salts, metal powders, finely chlorate divided organic or combustible materials
ammonia, butane, hydrogen, turpentine, finely Chlorine divided metals
Copper hydrogen peroxide
Hydrocarbons bromine, chlorine, peroxides
combustible materials, copper, iron, most metals Hydrogen peroxide and their salts, any flammable liquid
Iodine Ammonia
acetic acid, acetone, alcohol, flammable substances, such as organic chemicals Nitric acid, concentrated Note: There have been many explosions from inappropriate or inadvertent mixing of nitric acid with organic chemicals in waste containers.
Oxalic acid silver, mercury
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Oxygen flammable materials, hydrogen, oils
Phosphorus, white air, oxygen
Potassium permanganate ethylene glycol, glycerol, sulfuric acid
Sodium (alkali metals: lithium, sodium, and carbon dioxide, water, alcohols potassium)
Sodium nitrite ammonium salts
Sulfuric acid chlorates, perchlorates, permanganates
SECTION THREE: (Estifanos Ele)
Minimum Standards for Undergraduate Organic Chemistry
1. Human Resource
The following are minimum human resources that are required to handle practical organic chemistry laboratories
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1.1. Instructors
The department of chemistry must have at least two PhD and two MSc holders specialized in Organic Chemistry.
1.1.1. Role and responsibilities:
PhD holders:
handling the Organic Chemistry courses
supervise the overall situations related to the laboratory courses
MSc holders:
teach laboratory courses
support students during the experiment
correct laboratory reports and give feed backs
grade students as per their performances
1.2. Laboratory Manager
The department should assign one academic staff to coordinate the practical courses, or employ a fulltime PhD holder in Organic Chemistry that will work as a laboratory manager.
1.2.1. Role and responsibilities:
The Laboratory Manager will:
design new or review the existing experiments considering the availability of required
chemicals
mobilize instructors and teaching assistants
complete a Laboratory Hazard Control Plan
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ensure students, staff or other persons working in the laboratory are aware of and comply
with the lab safety rules and standards
implement the Monthly Laboratory Safety Checklist
ensure that all chemicals brought into the laboratory have been entered in the chemical
inventory
provide and document work - site specific safety training and orientation
ensure proper disposal of chemicals and laboratory waste
1.3. Laboratory Technician (Technical assistant)
At least one laboratory technician (BSc holder in chemistry) is required for each laboratory course
1.3.1. Role and responsibilities:
liaising with academic staff to discuss timetables, equipment requirements and work
plans
running trials of experiments prior to classes and then demonstrating techniques for
experiments
preparing equipment and chemicals before lessons - from test tubes to state-of-the-art
microscopes
maintaining and repairing equipment and laboratory apparatus
record keeping, e.g. for students' practical sessions, tracking methods, results, etc;
ensuring that equipment is properly cleaned and that chemicals and other materials are
appropriately stored
cataloguing recordings and making them available when requested
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supporting the work of teachers in classes and laboratory sessions and giving technical
advice to staff and students
working with individual students and supporting them on practical work
managing the stock control of chemicals and equipment
ensuring that all health and safety procedures are understood and followed correctly
coordinating work in the laboratory to ensure efficient use is made of expensive pieces of
equipment
2. Infrastructure
2.1.1. Building Design Issues
The important part of designing a chemical laboratory at a tertiary level should consider the building structure, location, external and internal facilities and human resources. Because the handling and storage of hazardous materials inherently carries a higher risk of exposure and injury, it is important to segregate laboratory and non-laboratory activities during designing. In an academic setting, the potential for students to need access to laboratory personnel, such as instructors and assistants, is great. A greater degree of safety will result when non laboratory work and interaction is conducted in a space separated from the laboratory.
2.1.2. Important consideration in designing chemical laboratories
The selection of the site shall be such to minimize the risk of natural hazards (earthquake,
flooding etc.)
The number of students supervised by a faculty member or by a teaching assistant in an
instructional lab should not exceed 30. Therefore the lab size should be planned to
accommodate that.
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The lab shape can be of different type. The U-shaped with fume-hoods around the wall is
preferable as it allows the instructor to manage the movement and activities of all
students without much trouble.
Figure 1. Sample laboratory design
The laboratory shall be completely separated from outside areas (i.e., must be bound by
four walls).
Non combustible construction materials should be used (block, concrete etc). Special
consideration should be given to the choice of fireproof construction for the buildings.
Offices and preparation rooms should be separated from laboratories, and separate office
spaces should be provided for laboratory employees.
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An automatically triggered main gas shutoff valve for the building should be provided to
cut off the natural gas service in an emergency event. In addition, interior manual shutoff
valves shall be provided for both research and teaching areas.
Separate corridor for public access to the laboratory personnel should be included in the
designing
Glasses in the building shall be shatter resistant.
*****The laboratory shall have means of securing specifically regulated materials such
as radioactive materials (i.e., lockable doors, lockable cabinets, etc.).
The building must have enough windows that open for ventilation in case where hoods
are non functional
It is better to have a separate building that will not be shared with teaching class rooms
The building must be equipped with water lines which can be controlled from inside as
well as outside the building
High roof laboratory rooms are advisable for better ventilations
Enough number of hoods shall be installed on the side walls (one hood for two to three
students)
Additional fume hood for the instructor to be used for reagent and chemical storage is
also required.
Floor surface must be solvent/chemical resistant, impervious, one piece, and well fitted to
the wall. This can be achieved by use of glue, epoxy coated concrete slab, etc.
Floors in storage areas for corrosive liquids shall be of liquid tight construction
Lab waste water lines shall be separate from domestic sewage
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Laboratory areas shall have adequate natural or artificial illumination to ensure sufficient
visibility
3. Laboratory Facilities
There must be adequate storage cabinets to store reagents and chemicals. Sufficient space or facilities (e.g., storage cabinets with partitions) shall be provided so that incompatible chemicals/gases (waste and non-waste) can be physically separated and stored.
3.1. Fixed chemical cabinets:
for
solid chemicals and reagents (under fume-hoods)
liquid chemicals reagents (under fume-hoods)
acids and bases (under fume-hoods)
waste chemicals (separate place on one corner or under a fume hood)
3.2. Metal cabinets for solvents
For organic solvents (that meets International Fire Protection Association standards)
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. At least one in each organic chemistry laboratory.
. All organic solvents should be kept inside the metal cabinet
. The total amount of solvents to be stored in the lab should not exceed 50
liters
3.3. Furniture Design, Location, and Exit Paths
Chemical storage shelves shall not be placed above laboratory sinks.
Bench should be made from strong wood which is resistant to the chemicals. The counter
top should incorporate a lip to help prevent run-off onto the floor.
The lab shall have a minimum passageway clearance of at least 60 cm. Main passageway
used for emergency door must have a clearance width of at least 90 cm.
A pathway clearance of 90 cm must be maintained at the face of the access/exit door.
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Designated storage space should be provided for lab carts. Location must not reduce width of corridors or passageways to less than 90 cm widths. Laboratory shelving should NOT be installed at heights and distances which require workers to reach 30 centimeters above shoulder height and extend arms greater than 30 centimeters while holding objects 16 kg or less when standing on the floor or on a 15 cm step stool. The space between adjacent workstations and laboratory benches should be 150 cm or greater to provide ease of access. In a teaching laboratory, the desired spacing is 180 cm. Lab desks should be located near exit ways and in the path of fresh make up air.
Note: All equipment requiring anchoring, whether installed by a contractor or the University, shall be anchored, supported, and braced to the building structure
3.4. Cleanability
The laboratory shall be designed so that it can easily be cleaned. Bench tops must be a seamless one-piece design to prevent contamination. Spaces between benches, cabinets, and equipment must be accessible for cleaning and allow for servicing of equipment.
3.5. Breakrooms
The design of the laboratory building must incorporate adequate additional facilities for food storage/consumption and personal hygiene tasks.
3.6. Entries, Exits, and passageway Width
Self-closing laboratory doors should be operable with a minimum of effort to allow access and egress for physically challenged individuals. A minimum of a 90 cm-wide door should be provided to facilitate equipment movement. Laboratory benches, laboratory equipment and other furniture or obstacles shall not be placed so that there is less than 150 cm of clear egress within the laboratory. Laboratory doors that separate laboratory areas from non-laboratory areas are to be automatically self-closing.
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Corridors should not be less than 180 cm wide to allow for movement of large equipment and allow for circulation of materials on carts, etc. Common corridors shall not be programmed for laboratory operations.
3.7. Inside Laboratory Facilities
Enough drawers per bench per group of students are required to store hard wares, glass wares and aprons Laboratory should be sufficiently large to provide places for [30] students, working as [15] pairs; each student to have 0.36 m2 work surface available. There also needs to be sufficient free bench space for setting out long-term investigations, laying out equipment to be selected by students (items not on student work spaces). One double gas tap and one double electrical socket should be provided for each pair of students and one sink for three groups of students. Sinks should generally be of cast epoxy or fire clay. Electricity sockets should be positioned to minimize risk of penetration by water. Each laboratory needs a teacher’s area equipped with gas, water and electricity services, a white board for writing, an interactive whiteboard or screen for a projector, and lockable cupboard / drawers. Water taps should be about 30 cm above bench level (to allow tall containers to be filled or cleaned) and should be of a non-rotatable, epoxy-coated, pillar design. Taps should be fitted sufficiently close to the sink for water to go easily into the sink. For ease of maintenance each tap or group of taps on a bench should have a service valve. Electrical supplies to each laboratory should be protected by an earth-leakage circuit breaker. The cut-off for each laboratory should be adjacent to the teacher’s area. Power to any fume cupboards needs to be on a separate circuit. Each laboratory should have clearly labelled fire-fighting equipment and one fire blanket, to be located adjacent to the teacher’s base. Each laboratory should have (wooden-seated / wood) stools for all students and the teacher. Heights of stools shall be such as to leave a gap of 25 cm between the stool top and the underside of the bench.
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Sample laboratory stools.
4. Equipment, apparatus and chemicals
4.1. Emergency equipment
All laboratories that use hazardous chemicals must have access to:
Emergency shower and eyewash inside each laboratory or on the corridor Fire blanket (one pack in each lab) Emergency/first aid kit (one in each lab) Sand bucket (one in each lab) Sodium bicarbonate/ sodium carbonate bucket-for acid spills (one in each lab) Citric acid/ sodium bisulfate bucket (for base spill) Fire extinguisher (one in each lab) Water hose (on the corridors) Clean-up tools such as dustpan, scoop and brush, etc. should be chemical resistant and no sparking (plastic)
Note: Everyone working in the lab must know where the emergency equipment is located and how to use it
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4.2. Other important equipment
Ice cube maker (at least one, common to all organic chemistry labs) Water distiller (two, common to all organic chemistry labs) Water deionizer (one, common to all labs) Oven (one in each lab) Desiccators with silica gel (two in each lab) Melting point apparatus (Thiel-tube for practical organic I (at least 30); Digital for practical organic II and III (three in each lab) that can run multiple measurements at a time. Digital Balances (two in each lab) Bunsen burner (one for each group for each lab) Heating plate with stirrer (20-30, for organic chemistry II and III) Water bath (digital six-opening laboratory water bath) (two in each lab)
4.3. Instruments:
Tin Layer Chromatography (TLC) visualizer (one in each lab) High Pressure Liquid Chromatography (HPLC) (one, common to all) Gas Chromatography (GC) (one, common to all) Infra Red (IR) spectroscopy (one, common to all) Refractometer (one, common to all) Centrifuge (one, common to all) Sonicator (one, common to all)
4.4. Apparatus
A. List of Laboratory Equipments for Practical Organic Chemistry I S. No. Equipment 4 Büchner flask (100, 250 mL) 1 Adaptor 19/26, 24/29 5 Büchner funnel (different size) 2 Balance 6 Boss head (six) 3 Beaker (50, 100, 250 mL) 7 Bunsen burner
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8 Clamp (four) 26 Separator funnel 9 Condenser (two) 27 Spatula 10 Distillation flask 28 Still head adapter(19/26, 24/29) 11 Dropper (three) 29 Test tubes (different sizes) 12 Erlenmeyer flask (50, 100, 250 mL) 30 Thermometer 13 Flat bottom flask (100, 250 mL) 31 Thiele tube 14 Filter funnel (long stemmed) 32 Versatile clamp (two) 15 Filter funnel (short stemmed funnel) 33 Watch glass (two) 16 Fractionating column 34 Water aspirator 17 Glass rod 35 Water bath 18 Glass tube 36 Wire gauze 19 Iron ring (two, large and small) 37 Test tube holder 20 Iron stand (three) 38 Capillary tubes 21 Measuring cylinder (5, 10, 25, 100 mL) 39 Rubber band 22 Quick fit flask (19/26, 24/29) (two) 40 Boiling chips 23 Ice maker (common to all) 41 Test tube brush 24 Round bottom flask (50, 100, 250 mL) 42 Detergent 25 Reagent bottles
B. List of apparatus for practical organic chemistry II and practical organic chemistry III S. Apparatus 8 Beaker (250 mL) No. 9 Adaptor (19/26) 1 Erlenmeyer flask (250 mL, 50 mL) 10 Round bottom flask (19/26) (250 mL) 2 Graduated cylinder (100 mL, 25 mL, 10 11 Round bottom flask (50 mL) mL, 5 mL) 12 Still head (19/26) 3 Suction filtering flask (250 mL) 13 Vacuum adaptor (19/26) 4 Buchner funnel 14 Adaptor for thermometers 5 Test tube with side arm 15 Thermometer (300 °C) 6 Hirsch funnel 16 Condenser (19/26) 7 Separatory funnel
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17 Test tube 30 Spatula 18 Dropper 31 Filter paper 19 Watch glass 32 Boiling chips 20 Long stemmed funnel 33 Red litmus paper 21 Water aspirator 34 Blue litmus paper 22 Bunsen burner 35 Clean cotton 23 Boss head 36 Bandage 24 Iron ring 37 Paper towels 25 Test tube holder 38 Glass rod 26 Wire gauze 39 Rubber tube 27 Clamp 40 Melting point (app) 28 Iron stand 41 Refractometer 29 Water bath
4.5. Chemicals/reagents
A. List of chemicals for practical organic chemistry I
S. No. Chemicals 12 Benzoic acid 1 Acetanilide 13 Beta-naphthol 2 Acetic acid glacial 14 Bromine 3 Acetic anhydride 15 n-butanol 4 Acetone 16 Calcium chloride 5 Acetophenone 17 Calcium carbide 6 Acetylsalicylic acid 18 Carbon tetrachloride 7 Alpha-naphthol 19 Copper sulphate 8 Ammonia 20 Cyclohexene 9 Aniline 21 2,4-DNPH 10 Beef tallow 22 Egg albumin 11 Benzene 23 Eosin
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24 Ethanol 48 Silica gel 60 – 120 mesh 25 Ether 49 Silica gel G6 TLC 26 Fluorescein 50 Sodium acetate 27 Glucose 51 Sodium carbonate 28 Glycine 52 Sodium bicarbonate 29 n-hexane 53 Sodium chloride 30 Hydrochloric acid 54 Sodium citrite 31 Iron(III) chloride 55 Sodium hydroxide 32 Kerosene 56 Sodium nitrite 33 Lactose 57 Potassium sodium tartrate 34 Lead acetate 58 Starch 35 Magnesium chloride 59 Sucrose 36 Malachite green 60 Sulfuric acid 37 Maleic acid 61 Toluene 38 Methyl orange 62 p-toluidine 39 Milk or casein powder 63 Ninhydrine 40 Nitric acid 64 Cong red 41 Paraffin oil 65 Chromatographic paper (16 + 16 cm) 42 Petroleum ether 66 Litmus paper blue 43 Phenol 67 Litmus paper red 44 Phenyl hydrazine 68 Ninhydrine paper 45 Phosphoric acid 69 Filter paper 46 Potassium permanganate 70 Module 47 Salicylic acid
B. List of chemicals for organic chemistry II S. No. Chemicals 3 Toluene
1 KMnO4 4 H2SO4
2 NaCO3 5 Oxalic acid
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6 Benzoic acid 35 Cyclohexanone 7 Methanol 36 Sodium bisulphite 8 Chloroform
9 NaHCO3
10 Na2SO4, MgSO4, CaCl2 drying agent 11 Resorcinol 12 Conc. HCl 13 Decolorizing carbon 14 Aniline 15 Acetic anhydride 16 Glacial acetic acid 17 Zinc dust 18 Ammonia 19 Ethanol
20 Conc. HNO3 21 Sodium nitrite 22 α-naphthol 23 Sodium hydroxide 24 Potassium hydroxide 25 Acetone 26 Benzaldehyde 27 Cyclohexanol 28 85 % phosphoric acid 29 Salt (NaCl) 30 Anthracene 31 Maleic anhydride 32 Phthalic anhydride 33 Sodium dichromate 34 Dichloromethane
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Note: The chemicals and apparatus list are based on practical organic chemistry manual of the Department of Chemistry, AAU.
5. Chemical Storage
5.1. Flammable liquid storage
Flammable liquids should be stored in flammable liquid storage cabinets or inside a designated flammable liquid storage area.
Flammable-liquids storage cabinets are not intended for the storage of highly toxic
materials, acids, bases, compressed gases or pyrolytic chemicals.
Purchase the smallest volume container needed for research/teaching purpose. This is
especially important with glass containers storing flammable liquids since these are
highly susceptible to breakage.
****Large bottles should be stored low to the ground in order to prevent large spills
from dropping.
5.2. Chemical storage groups
Chemicals are best segregated by hazard class to avoid incompatibilities. DO NOT STORE CHEMICALS ALPHABETICALLY, except within a hazard class. Plastic bins can be used to provide secondary containment and segregation on shelves. Recommended general hazard classes for storage are listed below.
A - Compatible Organic Bases
Examples: hydroxylamine, tetramethylethylamine diamine, triethylamine, phenylhydrazine
B - Compatible Pyrophoric & Water Reactive Materials
React with water to yield flammable or toxic gases. Examples include sodium, potassium, metal hydrides and hydrolysable halides (titanium tetrachloride, phosgene etc.) Keep away from water sources. Do not store above or below sinks.
Caution! Use dry chemical extinguisher for fire.
C - Compatible Inorganic Bases
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Materials with a pH > 9. Examples include ammonium hydroxide, calcium hydroxide, and sodium hydroxide. Separate from acids. Store solutions of inorganic hydroxides in polyethylene containers.
D - Compatible Organic Acids
Examples: propionic acid, trichloroacetic acid, acetic anhydride, acetyl bromide. Separate from inorganic acids.
E - Compatible Oxidizers including Peroxides
React with water, fire, flammables and combustibles. Examples include inorganic nitrates (nitric acid), permanganates, inorganic peroxides, persulfates, and perchlorates (perchloric acid). Keep separate from flammables and other organic materials. Keep separate from reducing agents (i.e., zinc, alkaline metals, and formic acid).
Caution! Do not store directly on wooden surfaces
F - Compatible Inorganic Acids not including Oxidizers or Combustibles
Materials with pH < 5. Examples include hydrochloric and hydrofluoric acid. Separate from active metals including sodium and potassium and from organic acids.
G - Not intrinsically Reactive or Flammable or Combustible
Example: NaCl, buffer solutions
J* - Poison Compressed Gases
Example: Hydrogen sulfide, chlorine
K* - Explosive or other highly unstable materials
Example: Picric Acid, nitrocellulose
L - Non-Reactive Flammables and Combustibles, including solvents
Flammable/Combustibles vapors ignite easily at room temperature. Examples include alcohols, esters, ketones, ethers and pyrophorics. Store flammable liquids in approved safety cans or cabinets. Keep away from heat, sun, flame, and spark sources. Separate from oxidizers.
X* - Incompatible with all other storage groups
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*Storage Groups J, K, and X are particularly hazardous and are incompatible with all other storage groups, or require special storage considerations.
Chemicals Storage Groups
This storage system should be used in conjunction with specific storage recommendations from the manufacturer’s label and MSDS Note: when possible, isolate all storage groups in separate cabinets. If space does not allow, use the suggested cabinet scheme to combine storage groups. Use secondary containment as shown to prevent spilled materials from contacting containers of incompatibles that are in the same cabinet
6. Laboratory Safety
Chemistry laboratories present more hazards than are typically found in other science laboratories. Interestingly, the very properties that we value in some chemicals are also what make them hazardous. For example, we like the fact that some organic solvents dissolve organic molecules very nicely, but this same feature also makes them dry out our skin. We use the reactivity that acids and bases provide in order to effect a chemical change, but that reactivity also makes them hazardous if they are in contact with skin or are ingested. Hence,
76 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry safety in chemistry laboratory should be taken as an important step to perform safe experiments.
Incident prevention is a collective responsibility, which requires the full cooperation of everyone in the laboratory. Incidents are often resulting due to:
an indifferent attitude toward safety; failure to recognize hazards or hazardous situations; failure to assess the risks involved in the work being done; failure to be alert to your surroundings; failure to follow instructions or measures to minimize risks; and failure to recognize the limitations of your knowledge and experience.
6.1. Safety Culture and Your Role in It
The safety knowledge and skills that you learn in your chemistry courses is greatly influenced by the safety culture of your institution. The components of a strong safety culture require you to do your part. There are four areas that should receive your attention: leadership, learning safety, building a positive safety attitude, and learning lessons from safety incidents.
6.2. Personal Protective Equipment (PPE)
PPE is used to eliminate or minimize exposure to some hazards encountered when working in the chemistry laboratory. PPE includes items designed to protect specific areas of the body, such as eyes and hands. It commonly includes gloves, eye protection, laboratory coats, and aprons.
6.2.1. Hair and clothing (Dressing for the Laboratory)
Clothing worn in the laboratory should offer your skin basic protection from splashes
and spills.
No shorts, short skirts, and shirts that expose skin to potential spills.
No bulky, loose sleeves and loose-fitting clothing that may knock laboratory items
over, be dragged through chemical spills, or present a fire hazard with open flames.
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No clothing made of artificial fibers. Cotton made clothing is preferable.
Wear laboratory coats or aprons. Nonflammable, nonporous aprons offer the most
satisfactory and the least expensive protection.
Laboratory jacket or coat should have snap fasteners rather than buttons, so that it can
be readily removed in case of contamination.
Wear shoes with uppers made of leather or polymeric leather substitutes that
completely cover your feet and toes (closed-toe shoes). This will offer your feet the
best protection from spills and dropped items.
Constrain long hair and loose clothing. Long hair can easily become entangled in
equipment, can be exposed to chemicals, or can catch on fire by direct exposure to lit
Bunsen burners.
Avoid wearing jewelry, such as rings, bracelets, necklaces, and wristwatches, in the
laboratory.
6.2.2. Eye Protection
Everyone in the laboratory, including visitors, must wear eye protection at all times,
even when not performing a chemical operation.
Use the more protective eyewear for variable environments. Goggles rated for
chemical splash protection are the preferred eye protection.
Do not rely on normal prescription eyeglasses for laboratory eye protection against
shrapnel from an explosion or splashes of hazardous chemicals. Serious injuries have
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resulted from the wearing of normal prescription eyewear without chemical splash
goggles or safety glasses.
6.2.3. Gloves
Wear gloves in order to protect contamination of hands by
different chemicals.
Select glove material based on the chemicals being used.
Gloves must be before free of cracks and small holes.
Remove gloves before leaving the work area and before handling such things as cell
phones, calculators, laptops, doorknobs, writing instruments, laboratory notebooks,
and textbooks.
Wash hands when leaving the laboratory, even if you have worn gloves.
6.2.3.1. Glove Comparison Chart
Summary: Consult this chart for an overview of commonly used glove types for laboratory use and their general advantages and disadvantages
Note: These photos are examples. Glove colors and appearances will vary. Many other models are commercially available in each glove category.
Advantages and Glove material Intended use Example Photos disadvantages
Good for biological and Latex (natural Incidental contact water-based rubber) materials.
Poor for organic
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solvents. Little chemical protection. Hard to detect puncture holes. Can cause or trigger latex allergies
Excellent general use glove. Good for solvents, oils, greases, and Incidental contact (disposable some acids and exam glove) bases. Nitrile Clear indication Extended contact (thicker
of tears and reusable glove) breaks.
Good alternative for those with latex allergies.
6.3. Laboratory Protocols
6.3.1. Laboratory Environment
The chemistry laboratory can provide a wealth of opportunity for learning, but while working in the laboratory, you should remain alert to your actions and the actions of those around you. Variations in procedure, including changes in the chemicals to be used or in the amounts that will be used, may be dangerous.
Alterations should be made only with the knowledge and approval of your instructor.
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Before working in the laboratory, take note of your surroundings. Locate the exits, eyewash fountains, safety showers, fire blankets, first aid kits, and fire extinguishers; practice walking to them.
6.3.2. Housekeeping
In the laboratory and elsewhere, keeping things clean and neat generally leads to a safer environment.
Keep aisles and access to safety equipment free of obstructions such as chairs, boxes, open drawers, backpacks, and waste receptacles. Avoid slipping hazards by keeping the floor clear of spilled liquids, ice, stoppers, glass beads or rods, and other such small items. Keep workspaces and storage areas clear of broken glassware, leftover chemicals, and dirty glassware. Broken glassware should always be disposed of in a broken glass disposal container and NEVER in an ordinary trash can. Inform your instructor immediately if glass is broken or chemicals are spilled. Wipe your bench area before leaving the laboratory, so that others will not inadvertently touch chemical residue. Never leave chemicals on balances, because this may unnecessarily expose the next user to the chemical; in addition, electronic balances are expensive and can easily be damaged by corrosive chemicals. Clean your dirty glassware at the laboratory sink using hot water, environmentally acceptable cleaning agents, and brushes of suitable stiffness and size. Do not force a brush into glassware.
6.3.3. Labeling Chemicals
Improper or insufficient labeling of chemical containers has resulted in numerous adverse incidents. It is unacceptable to use a marker to write over an existing manufacturer label.
In no instance should a container ever have two labels, one on each side of the bottle.
6.3.4. Inhaling Harmful Chemicals
If you are instructed to smell something in the laboratory, use your hand to waft vapors toward your face and sniff gently. You should never sniff a chemical by placing your nose
81 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry directly over a chemical container. The label on the container and the Safety Data Sheet (SDS) for the chemical may carry a warning about inhalation hazards.
Follow the instruction of your instructor
6.3.5. Hazardous waste containers
Hazardous waste must be stored in containers (including lids) made of materials that are compatible with the waste. Hazardous waste containers must be in good condition and free of leaks or any residue on the outside of the container. Unacceptable containers include household detergent and food service containers. The best container for your hazardous waste is the original chemical container.
6.3.5.1. Sealing hazardous waste containers
Hazardous waste containers must be sealed to prevent leakage or spillage. Containers should be sealed with a screw-type lid or other appropriate device. Plastic wrap, aluminum foil, and other make-shift lids are unacceptable. A container holding hazardous waste must ALWAYS be closed during storage, except when it is necessary to add or remove waste.
6.3.5.2. Labeling hazardous waste containers
Hazardous waste containers must be labeled with hazardous chemical waste tags. These tags require the laboratory to provide specific information including name, telephone number, building, room number, and exact contents of the container.
6.3.5.3. Hazardous waste container storage
You should designate an isolated portion of your laboratory as a hazardous waste storage area. Hazardous wastes must be stored with secondary containment so that spills cannot reach sink, hood, or floor drains. Incompatible hazardous wastes must be segregated to prevent reaction. Segregation methods include storing in separate cabinets, storing in separate hoods, or storing in separate secondary containment containers.
In this photo, hazardous waste is labeled with pink chemical waste tags, segregated by chemical compatibility, stored in secondary containment, and kept in an isolated area. Properly Stored Hazardous Waste
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Improperly Stored Hazardous Waste
In this photo, there are no labels, no secondary containment, no segregation, and containers are covered with waste residue
.
In this example, there is no secondary containment from hood drain and storage is in a high traffic area.
In this example, there are no labels, no secondary containment, and one container has not been properly sealed (open funnel).
6.3.6. Disposal of Chemicals
Proper handling of reaction by-products, surplus, waste chemicals, and contaminated materials is a major element of incident prevention, and there are very strict rules for disposing of chemicals. Improper disposal can result in serious damage to the environment and can also result in legal issues for your institution. Every student is responsible for ensuring that these wastes are handled in a manner that minimizes personal hazard and recognizes the potential for environmental contamination.
6.4. Important points to be noted
Whenever you are in the laboratory:
A. PROPER CONDUCT/BEHAVIOR
Do not work alone.
Never perform unauthorized experiments or change procedures without approval.
Maintain an awareness of your surroundings, and move purposefully around others.
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Never remove chemicals from the laboratory without proper authorization, and report to
your instructor any observed unauthorized removal of chemicals by others.
Never play tricks or engage in horseplay in a chemistry laboratory.
Notify your instructor if you observe violations of your laboratory’s safety rules; you
could save someone’s life.
B. PROPER LABORATORY ATTIRE
Prevent skin exposure by covering your skin.
Feet must be completely covered, and no skin should be showing between the top of the
shoe and the bottom of the skirt or pants.
Confine long hair, avoid wearing loose clothing, and remove scarves and jewelry.
C. SAFE HANDLING OF CHEMICALS
Read the procedure ahead of time, listen carefully to your instructor’s directions, and note
any safety requirements for the experiment in your pre-lab notes.
Never directly sniff a chemical. When instructed to smell something, use your hand to
waft vapors toward your face and sniff gently.
Never return reagents to the original container once they have been removed.
D. SAFE HANDLING OF EQUIPMENT
Never pipet by mouth. Always use a pipet aid or suction bulb.
Do not use hot plates with exposed or worn wiring.
Check Bunsen burner hoses for holes.
Always ensure balanced loading of test tubes in centrifuges.
E. ENGINEERING CONTROLS AND PERSONAL PROTECTIVE EQUIPMENT
Always wear the correct type of eye protection when working in the laboratory. Your
instructor will tell you the level of eye protection required
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Wear chemically resistant laboratory coats or aprons, if instructed to do so.
Work in laboratory hoods as instructed.
F. PROPER HOUSEKEEPING
Prevent spills by keeping chemicals and apparatus well away from the edges of your
laboratory bench or other workspace.
Dispose of chemical hazardous waste as instructed, and always ask for guidance if you
are unsure.
Always wash laboratory coats or other clothing on which chemicals have been spilled
separately from personal laundry.
Wipe down your work area for the next user.
Clean spills on the balances as instructed.
G. PROPER HYGIENE
Do not prepare or store (even temporarily) food or beverages in a chemistry laboratory.
Never consume any food or beverages when you are in a chemistry laboratory.
Never wear or take laboratory aprons or laboratory coats into areas where food is
consumed.
Do not chew gum, smoke, or apply cosmetics or lip balm in the laboratory. Be aware that
cosmetics, food, and tobacco products in opened packages can absorb chemical vapors.
Never take your hands or pen to your face or mouth while working in the laboratory.
Do not handle contact lenses in the laboratory, except to remove them when an
emergency requires the use of the eyewash fountain or safety shower.
Always wash your hands and arms with soap and water before leaving the laboratory,
even if you wore gloves.
H. EMERGENCY PREPAREDNESS
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Become thoroughly acquainted with the location and use of safety equipment and
facilities such as exits, evacuation routes, safety showers, eyewash fountains, fire
extinguishers, and spill kits.
7. Guide to Chemical Hazards
Interestingly, the very properties that make a chemical useful are often those that make it risky to use, so chemists must learn how to safely use chemicals that have significant inherent hazards, by using the principles of RAMP. The term RAMP is stands for
R Recognize the hazards A Assess the risks of the hazards M Minimize the risks of the hazards P Prepare for emergencies from uncontrolled hazards
Understanding the hazardous characteristics of all chemicals: toxicity, flammability, corrosivity, and reactivity. Know ways through which chemicals can enter the body: inhalation, ingestion, absorption, and injection
7.1. Important symbols to be noted
Globally Harmonized System of Classification and Labelling of Chemicals (GHS)
All users are advised to check the Safety Data Sheets (SDSs) before using any chemical. The SDS for a hazardous chemical is a document that describes the chemical’s hazards and the precautions that you must take to avoid harm.
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7.4 References
1.
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SECTION FOUR: Minimum Standards for Undergraduate Analytical Chemistry Laboratory (Solomon Mehretie)
1. Infrastructure of undergraduate laboratories
The laboratory-room will be built by considering non-combustible materials such as breaks and have high roofs with enough windows for proper ventilation.
1.1. Wet lab
The draft design of the wet lab is given below (Fig. 1) where it creates a reasonable close contact between lab instructor and students and easy access to laboratory facilities. This wet lab is space where a lot of chemicals, reagents, storage cabinets and other materials are properly placed. The laboratory space must have: . Impervious and chemically resistant work surfaces; . Safety shower; . Eye-wash station; . A fire extinguisher mounted to the wall or in an extinguisher cabinet; . A functioning chemical fume hood; . Appropriate gas and water supply lines controlled in both outside and inside the lab rooms; . Chairs and furniture that are constructed of non-cloth material; . Electrical outlets sufficient in number and location to minimize the use of extension cords; . Enough sinks and the waste water lines which are separated from any domestic sewage
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Fig.1. Suggest design of a wet lab set-up for undergraduate students
The minimum standard of the Analytical wet lab should
. accommodate not more than 30 students per lab room; . be designed to provide at least 2 m2 of net space per student, including lab tables and benches; . have a preparation room where it provides safe storage, handling and preparation area and permit easy distribution of chemicals.
1.2. Dry lab
Dry laboratory space types are designed to accommodate scientific equipment and project- specific work patterns with minimum space for sample accumulation and preparation as shown in Fig.2. This type of laboratory is especially important for instrumental analysis courses. The laboratory space must contain
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. A fire extinguisher mounted to the wall or in an extinguisher cabinet; . A small-size functioning chemical fume hood; . Appropriate gas and water supply lines controlled in both outside and inside the lab rooms; . Temperature and humidity control; . Dust control; . Durable and flexible casework
Fig.2. Suggest design of a dry lab set-up for undergraduate students
2. Human resources
Laboratory instructors should have M.Sc or Ph.D. in Chemistry and provide theoretical background to the undergraduate students on each experiment and instructions how to do the experiment. Each laboratory shall have full-time properly trained laboratory technician (has minimum B.Sc. degree in chemistry) to prepare regents and maintain laboratory facilities. Each laboratory shall assign at least one personnel as the laboratory safety officer (has
90 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry minimum B.Sc. degree in chemistry) available at all times to respond to emergencies such as fire, chemical accidents, first aid needs.
Instructors, technicians and safety officers are responsible for the safety of their students and should be in the laboratory during the entire lab period. They allow neither untrained students nor visitors to work with chemicals. These staff members of chemistry department have the following responsibilities: . set a good example by observing the rules and recommendation outlined by the Chemistry Department, wearing appropriate protective equipment, and practicing accident prevention, . review the procedures with the students for potential health, safety and environmental problems for each laboratory session, . be alert for unsafe conditions, . provide discipline and enforce rules, and . promptly take effective corrective action when necessary.
Staff offices should be reasonably close to laboratory facilities and positioned to facilitate student contact.
3. Practical Analytical Chemistry
3.1. Minimum standards for instrumental analysis
Instrumental analysis laboratory should have apparatus appropriate for providing hands-on laboratory experiences in order to carry out the analysis and determination of substances mentioned in their practical instrumental analysis manuals. The laboratory should have
. standard chemistry instrumentation items, such as pH meter, Ion meter, Conductometer, gas chromatographs, colorimeter, coulometer, refractometer, UV- Vis spectrophotometer and FTIR. . The following apparatus are also necessary to carry on Instrumental analysis
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1 Balance, analytical 14 Oven, drying 2 Bunsen burner 15 Oven, laboratory 3 Glass burette 16 Pipettes 4 Stirrer 17 Pipettors 5 Centrifuge 18 Pump, vacuum 6 Thin Layer Plates and developing Tank 19 Conical flask 7 Chromatograph, paper and developing tank 20 Magnetic stirrer 8 Electrodes: glass and calomel, 21 Thermometers, electronic 9 Ag/AgCl/sat. KCl reference electrode 22 Watch glass Volumetric flask (100, 250, 10 Electrodes: Chloride selective eletrode 23 500 mL and 1 L) 11 Constant current d.c. power supplier 24 galvanometer Volumetric flask (10, 25, 50 12 Electrodes: iodide selective eletrode 25 mL) 13 Electrodes: sodium ion selective eletrode 26 Device for Pressing KBr disk
. Chemicals and chemical reagents for instrumental analysis
1 1,10 -phenanthroline 15 Carbon tetrachloride 2 Hydroxylamine hydrochloride 16 methanol 3 Sodium acetate 17 Chloroform 4 Ammonium iron (II) sulfate 18 Cadmium nitrate 5 Sodium chloride 19 Calcium nitrate 6 Potassium bromide 20 Magnesium nitrate 7 Copper sulfate 21 Nickel nitrate 8 Cobalt chloride 22 Potassium nitrate 9 Zinc nitrate 23 Potassium iodide 10 Ethyl acetate 24 Potassium dichromate 11 ethanol 25 Sulfuric acid 12 benzene 26 Acetic acid 13 Sodium thiosulfate 27 Potessium chloride 14 Hydrochloric acid 28 Sodium hydroxide
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3.2. Chemical reagents required to carry on practical analytical chemistry
1 Hydrochloric acid 20 Potassium dichromate
2 Sodium carbonate 21 Potassium iodide 3 Sodium bicarbonate 22 Ammonium thiocyanate
4 Borax (Na2B4O7) 23 Acetic acid 5 Sodium chloride 24 Magnesium sulfate Ethylenediammine tetra acetic 6 Silver nitrate 25 acid (EDTA) 7 Ammonium chloride 26 Erichrome Black T (EBT) 8 Formaldehyde 27 Calcium Chloride 9 Potassium thiocyanate 28 Nickel chloride 10 Potassium chloride 29 Ethanol 11 Ferric chloride 30 Dimethyl glyoxamine (DMG) 12 Nitric acid 31 Ammonia
13 Potassium permanganet 32 NH3 /NH4Cl buffer
14 Oxalic acid 33 CH3COOH / CH3COONa buffer 15 Sodium oxalate 34 Methyl red 16 Sulferic acid 35 Methyl orange 17 Ammonium ferrous sulfate 36 Phenol red 18 Copper sulfate 37 Phenolphthalein 3 19 Sodium thiosulfate 8 Starch
3.3. Chemical reagents required to carry on real sample analysis
1 Hydrochloric acid 12 Starch 2 Sodium carbonate 13 Potassium iodide 3 Sodium hydroxide 14 Soda ash
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4 Potassium Iodate 15 Acetic acid 5 Chloroform 16 potassium permanganate 6 Ascorbic acid 17 Phosphoric acid 7 Phenolphthalein 18 Nitric acid 8 Methyl orange 19 Bleaching powder 9 Sodium thiosulfate 20 Hypochlorite 10 Sulfuric acid 21 Copper 11 Vinegar 22 Orange juice
4. Laboratory safety
4.1. Good safety practices: Do
. Know the potential hazards of the materials used in the laboratory. . Know the location of safety equipment such as emergency showers, eyewashes, fire extinguishers, fire alarms, and telephones. . Review emergency procedures to ensure that necessary supplies and equipment for spill response and other accidents are available. . Practice good housekeeping to minimize unsafe work conditions such as obstructed exits and safety equipment, hoods, and accumulated chemical waste. . Wear personal protective clothing while working with chemicals. This includes eye protection, lab coat, gloves, and appropriate foot protection (closed-toe shoes, no sandals). Gloves should be made of a material known to be resistant to permeation by the chemical in use. . Wash skin promptly if contacted by any chemical, regardless of corrosivity or toxicity. . Always wash your hands before leaving the lab. . Label all new chemical containers with the "date received' and "date opened."
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. Label and store chemicals properly. All chemical containers should be labeled to identify the container contents (no abbreviations or formulas) and hazard information. Chemicals should be stored by hazard groups and chemical compatibilities. . Use break-resistant bottle carriers when transporting chemicals in glass containers that are greater than 500 mL. . Use fume hoods when processes or experiments may result in the release of toxic or flammable vapors, fumes, or dusts.
4.2. Bad safety practices: Don’t
. Eat, drink, smoke, chew gum, or apply cosmetics in areas where chemicals are used and stored. . Store food in laboratory refrigerators, ice chests, cold rooms, or ovens. . Drink water from laboratory water sources. . Use ice from laboratory sources in beverages. . Use laboratory glassware to prepare or consume food. . Smell or taste chemicals. . Pipette by mouth. . Work alone in the laboratory without prior approval from the lab supervisor.
4.3. Proper labeling and safe storage of chemicals
Proper chemical labeling and storage is essential for a safe laboratory work environment. Inappropriate storage of incompatible or unknown chemicals can lead to spontaneous fire and explosions with the associated release of toxic gases. To minimize these hazards, chemicals in the laboratory must be segregated properly.
4.3.1. Labeling
. Manufacturer chemical labels should never be removed or defaced until the chemical is completely used. . All chemical and waste containers should be clearly labeled with the full chemical names (no abbreviations or formulas) and appropriate hazard warning information.
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Small containers that are difficult to label such as 1-10 ml vials and test tubes can be labeled as a group and stored together. . Unattended beakers, flasks, and other laboratory equipment containing chemicals used during an experiment should be labeled with the full chemical names. . All hazardous waste containers must be tagged with "hazardous waste." . All hazardous waste containers must be marked with an accumulation date. The accumulation date represents the date that hazardous waste is first placed in the container (waste containers should NOT be filled to more than 90% of their capacity). . All chemical storage areas such as cabinets, shelves and refrigerators should be labeled to identity the hazardous nature of the chemicals stored within the area (e.g., flammables, corrosives, oxidizers, water reactives, toxics, carcinogens, and reproductive toxins).
4.3.2. Storage
Stationary chemical cabinets for solid, liquid chemicals and reagents should be placed and the following tables show patterns of chemicals stored in a storage cabinets. Note that metal cabinets for organic solvents are mandatory.
4.3.2.1. Pattern of organic chemicals in storage cabinets
Organic 2 Organic 8 Store severe poisons in poisons cabinet Alcohols, glycols, amines, Phenols amides, imines POISON
Organic 3 Organic 6
Hydrocarbons, esters, Peroxides, azides aldehydes
Organic 4 Organic 1 Store flammables in a dedicated cabinet Ethers, ketones, hylogenated Acids, anhydrides, peracids hydrocarbons, ethylene oxide FLAMMABLES
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Organic 5
Epoxy compounds, Miscellaneous isocyanates
4.3.2.2. Pattern of inorganic chemicals in storage cabinets
Mineral acids except nitric acid Inorganic 10 Inorganic 7 (Dedicated as separate Sulfur, phosphorus, Arsenic, Arsenates, cyanides cabinets) phosphorus pentoxide (store away from any water) ACID
Store nitric acid away from
other acids
Inorganic 2 Inorganic 5
Halides, sulfates, sulfites, Sulfides, carbides, nitrides thiosulfates, phosphates, acetates
Inorganic 3 Inorganic 8
Nitrates, nitrites, azides Borates, chromates, permanganates (store ammonium nitrate away from all other substances-ISOLATE it)
Inorganic 1 Inorganic 6
Metals, hydrides Chlorates, perchlorates, chlorites, perchloric acid, (stor away from any water) peroxides, hypochlorites, hydrogen peroxide
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Inorganic 4
Hydrooxides, oxides, Miscellaneous silicates, carbonates, carbon
4.3.2.3. Some important tips for storage
. A definite storage place should be provided for each chemical and the chemical should be returned to that location after each use. . Chemical containers should be in good condition before they are stored. Containers should be managed to prevent leaks. . Chemicals (including waste) should be separated and stored according to their hazard group and specific chemical incompatibilities. . Special attention should be given to the storage of chemicals that can be classified into two or more hazard groups. For example acetic acid and acetic anhydride are both corrosive and flammable. In addition perchloric acid is both corrosive and a strong oxidizer. . Chemicals should be separated by distance. Physical barriers such as storage cabinets and secondary containers should be used to prohibit contact of incompatible chemicals in the event that they are accidentally released or spilled. . Liquid chemicals should not be stored above dry chemicals and be stored below eye level to avoid accidental spills. . Storage of chemicals within hoods and on bench tops should be avoided. . Stored chemicals should not be exposed to heat or direct sunlight. . Chemicals should not be stored in areas where they can be accidentally broken and spilled such as on the floor or on the edge of a bench top or exits.
4.4. Safe use of chemical fume hood
Chemical fume hoods are one of the most important items of safety equipment present within the laboratory. Chemical fume hoods serve to control the accumulation of toxic, flammable,
98 | P a g e Preparation of Laboratory and Workshop Standards of Undergraduate Science and Engineering Education program/ Chemistry and offensive vapors by preventing their escape into the laboratory atmosphere. In addition, fume hoods provide physical isolation and containment of chemicals and their reactions and thus serve as a protective barrier between laboratory personnel and the chemical or chemical process within the hood.
The fume hood is the best known local exhaust device used in laboratories. When used properly, it will protect the user from exposure to potentially harmful chemical contaminates. Proper hood performance depends on the velocity of air moving through the hood. A fume hood that isn't performing properly is often worse than no hood at all because the user is likely to have a false sense of security about its ability to provide protection.
4.5 References
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SECTION FIVE: (Mesfin Redi)
Minimum Standards for Undergraduate Physical Chemistry Laboratory
Physical chemistry provides the fundamental concepts and organizing principles that underlie all aspects of chemistry and related fields. Conventionally, it is divided into four major branches which are thermodynamics, chemical kinetics, quantum chemistry, and statistical mechanics. Therefore, physical chemistry teaching should include four lecture and two practical courses.
The physical chemistry lecture courses should address each of the major concepts listed below under the respective courses.
Chemical Thermodynamics lecture course: should cover topics: basic terms (system, thermodynamic state, state functions, work, heat, etc.); thermodynamic laws (0th, 1st, 2nd and 3rd laws); equation of state for ideal and real gases; state functions (enthalpy, entropy, Gibbs energy, etc.) and applications; microscopic interpretation of entropy; chemical potential applied to chemical and phase equilibria; non-ideal systems; standard states; activities; Gibbs phase rule; phase equilibria; single and multi-component phase diagrams Chemical kinetics: should cover topics: differential and integral rate laws of various orders (for only forward and reversible reactions); molecularity; derivation of rate laws from chemical mechanisms; steady-state approximation; chain reactions; collision theory; transition state theory; enzyme kinetics; reactions on surfaces; Langmuir isotherm Quantum chemistry: should cover topics: postulates and formulation of Schrodinger equations; operators and matrix elements; particle-in-a-box; simple harmonic oscillator; rigid rotor; angular momentum; Hydrogen atom; hydrogenic wave functions; spin; Pauli principle; approximate methods; Helium atom; Hydrogen molecule ion; hydrogen molecule; diatomic molecules; LCAO method; light-matter interaction; dipole selection rules; rotational spectra of linear molecules; vibrational spectra; term symbols; electronic spectra of atoms and molecules Statistical thermodynamics: should cover topics: Boltzmann distributions; molecular partition functions; partition function expressions for atoms, rigid rotors, and harmonic oscillators; standard thermodynamic functions expressed in partition functions
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The physical chemistry practical courses should provide students with sufficient experimental experience in connecting theoretical concepts with observed chemical phenomena using physical chemistry concepts. Accordingly, the physical chemistry practical courses, though may be selected according to the availability of resources, should include experiments to elaborate the major theoretical concepts.
The minimum set of experiments to be included and the resources required are listed below, which are based on the currently given physical chemistry courses at the Department of Chemistry, Addis Ababa University.
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Practical Physical Chemistry Course I
Exp. No Title Chemicals Apparatus/ Instrument
Othmer equilibrium apparatus; Heater (heating mantle), Boiling point diagram of a binary adjustable stand, graduated cylinders 50 mL(2), test tube, 1 Chlor Chloform; Ethanol system glass rod, thermometer, soft paper, boiling chips; Digital refractometer
Thermometer, electric water bath with stirrer, descant and 2 Partial miscibility of a binary system Phenol and water sample with closed test tube
Electric water bath with stirrer , thermometer, pipette, Dependence of saturation activity of Phenolphthalein solution, sodium hydroxide, 3 burette, Erlenmeyer flask 250 mL(2), measuring cylinder a solute up on temperature benzoic acid 150mL
Boiling apparatus, heater, Beckman thermometer, boiling 4 Boiling point elevation CaCl , NaCl, KCl 2 chips, condenser, pipette, weighing bottle
Sodium hydroxide 0.1 M, acetic acid 0.1M, sodium PH meter, combination glass electrode, magnetic stirrer, 5 Ionic Equilibrium acetate, phosphoric acid, buffer solution bar, beaker 500 mL (2), pipette 10 mL
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Thermodynamics of an Zinc sulphate solution 0.1 M, copper sulphate Daniel cell, thermometer, water bath, zinc and copper 6 Electrochemical cell solution 0.1 M, saturated potassium chloride electrode, digital multi-meter, beaker
Conductance of strong and weak Acetic acid, sodium chloride, sodium acetate, Conductivity meter, conductivity cell, beakers 150 mL, 7 electrolytes hydrochloric acid, potassium chloride pipette, volumetric flask 100 mL (5)
Digital balance (0.01 mg); Erlenmeyer flask (250 mL); 8 Isobaric expansion coefficient Ethanol thermostatic water bath; stand with clamps
Kinetics study of the Reaction of Crystal violet 1.5 * 104 M, NaOH 0.2 M, 0.1 M, Pipettes 10 mL (2) measuring cylinder, cuvette, beakers, 9 crystal violet with sodium hydroxide 0.05 M and 0.01M, distilled water volumetric flask
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Practical Physical Chemistry Course II
Exp. No Title Chemicals Apparatus/ Instrument
Vibrational-rotational spectra of HCl 1 HCl vapor phase Desktop computer, Gaussian software, Gas sampler in vapor phase
Volumetric flask 100mL (2), 50 mL (6), beakers, pipettes, 2 Surface tension of liquids Butanol, water pipette filler, Ostwald Stalagmometer
3 Viscosity measurement Polystyrene, toluene Viscometer, Volumetric flask 100 mL
Volumetric flasks (100 mL); beakers (20 mL); magnetic 4 Critical micelle concentration Sodium acetate; Acetic acid stirrer with fishers
Intermolecular interaction and virial 5 None Virial software program coefficient of some gases
+ 6 Potential energy of H2 None Poteng software program
Erlenmeyer flasks (200 mL 14); pipettes (50 mL, 25 mL, Organic acids (for example benzoic acid); NaOH; 7 Adsorption of charcoal 10 mL and 5 mL); Digital balance (0.01 mg); Filter paper; Activated charcoal; phenophtahaline funnel; burette
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Quartz cuvette, Teflon, beaker’; 8 Absorption spectroscopy Benzene, cyclohexane UV-Vis spectrophotometer
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The staff members and teaching support technical staffs are responsible in proper delivery of lecture and practical courses, respectively. To meet these demands required, there should at least two teaching with PhD degree and two support staffs with MSc degree, one each for Practical physical chemistry I and II each.
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