Standard Operating Procedure

Acid and Base Bath Use
Investigator: UG & PG students, RAs, technical & academic staff Location: All William Perkin Laboratories

Page 1 of 10 Revision: 00

1.0

PURPOSE

This document describes the safety requirements that laboratory workers and supervisors must follow when using acid baths and base baths. Its purpose is to minimize risks to the health and safety of laboratory workers.

2.0

SCOPE

This SOP offers instruction on the preparation, use and safe disposal of acid baths and base baths in the laboratories within the Perkin building. There is also a separate section dealing with the cleaning of NMR tubes. These chemical baths are used to clean glassware after use. This document is meant to inform laboratory workers about the health and physical hazards of cleaning baths. The procedures detailed herein apply to all Heriot-Watt University personnel and students working within the William Perkin Building Teaching and Research Laboratories. A laboratory worker with a chemical background should be able to read and understand this SOP in about 1 hour. This SOP may be used for training of laboratory workers in the use of cleaning baths. This SOP is meant to compliment, but not to replace, other classes of SOPs which are required in laboratories (such as those related to analytical procedures) and which also contain relevant safety information and/or references.

3.0

SAFETY RISKS

Hazards arising from cleaning bath use arise from the base bath (organic solvents and corrosive base), acid bath (irritant acid solution) and chemicals associated with any glassware being cleaned: Failure to follow the procedures in this SOP may result in: skin and eye irritation; skin defatting or dermatitis from prolonged or repeated skin exposure; central nervous system depression; reproductive and fetal effects; chronic toxic effects, such as liver or kidney effects, from inhalation of solvent vapours; acutely toxic effects, including blindness and death; flash fires.

4.0 4.1

DEFINITIONS Acid Corrosive material that produces H+ (aq) ions in aqueous solution. Strong acids ionise completely or almost completely in dilute aqueous solution. Weak acids ionise only slightly. Corrosive material that produces OH– (aq) ions in aqueous solution. Strong bases are soluble in water and are completely dissociated. Weak bases ionise only slightly.
Active Date: 7 December 2012 Retired Date:

4.2

Base

DOC #

HWU_Perkin_ClBaths_SOP_09

but should be removed into a fumehood when a solvent is spilled on the gloves. [Spill kits are distributed around the Perkin building see HWU-Perkin_SpillKits_SOP_03]. SPILL MATERIALS. A primary irritant causes irritation by direct contact with the skin. eyes. or respiratory system.7 Acid Bath Base Bath Laboratory workers Primary Irritant Skin Defatting Agent Location: All William Perkin Laboratories Page 2 of 10 Revision: 00 A bath formed from dilute aqueous acid (usually hydrochloric acid) A cleaning bath formed from an alcoholic hydroxide solution (usually potassium hydroxide and isopropanol) Refers to all permanent and temporary laboratory workers. Lightweight PVC gloves are sufficient to prevent incidental contact. A skin defatting agent causes deterioration of the fatty layer of the skin with prolonged or repeated contact. Spill kits should be available to deal with laboratory spillages. before working with these chemicals. knowledge of potential hazards.5 4. 6. use of spill kits. and appropriate emergency procedures. All laboratory workers are required to use due diligence in working with cleaning baths.3 4. Heavier nitrile gloves are required for cleaning up spills and are required whenever hands or fingers are immersed in the bath. technical & academic staff 4. RAs. GLASSES. all cleaning baths should be housed in a fumecupboard GLOVES. Laboratory supervisors are required to ensure that workers have the necessary personal protective equipment. 5. Laboratory workers who do not wear glasses or who wear contact lenses must be provided with splash-proof chemical goggles or face shields when handling flammable solvents. and chemical resistant gloves should also be available. University staff and visitors who make use of laboratory space. Ideally.6 4.0 MATERIALS and/or EQUIPMENT FUMEHOODS. DOC # HWU_Perkin_ClBaths_SOP_09 Active Date: 7 December 2012 Retired Date: .Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. All laboratory workers who work with cleaning baths must be satisfied that they have received sufficient education in safety techniques including: use of personal protective equipment. A lab coat is required when working with cleaning baths. Laboratory supervisors are responsible for ensuring that adequately ventilated areas are available for operations utilising organic solvents. Before performing any procedure involving cleaning baths a laboratory worker must read and be satisfied that they understand the SOP associated with that procedure. Face shields may be necessary when there is a potential for splashes.0 RESPONSIBILITIES Laboratory supervisors are responsible to ensure that all laboratory workers who work with cleaning baths have been educated in relevant safety issues. PROTECTIVE CLOTHING. Gloves shall be worn whenever cleaning baths are handled. Safety glasses are necessary when using cleaning baths.4 4. FACE SHIELDS. Paper towels or adsorbent materials such as spill control pillows. Laboratory supervisors are responsible for checking that only appropriately trained individuals are allowed to work with cleaning baths in the areas under their supervision. students.

2 8.6 8. Into a large plastic container (20-25L) carefully pour approximately 7-8 L of isopropanol. Establish the presence of working fire extinguishers and a fire blanket (see 6. electric sparks. Do not position the bath close to the edge of a shelf or in a place where it can be easily disturbed. Until this occurs the base bath will be relatively ineffective for cleaning. Personal protective clothing. laboratory coat and safety spectacles) should be worn when preparing a base bath.3 8.4 8.6 8. Personal protective clothing.1 9. This is most likely to be in the form of pellets. Ensure that an eyewash station is located nearby. the base bath is corrosive. The pellets are likely to take several days to dissolve completely in the alcohol. lab coats and eye protection are worn where required.4 7. When fully active.1 GENERAL PROCEDURES Read the relevant Material Safety Data Sheet (MSDS) sheets for the materials used in cleaning baths. Do not position the bath close to the edge of a shelf or in a place where it can be easily disturbed. welding activities. The fumecupboard should not be used for any purpose other than cleaning and should be free of clutter. RAs. Add approximately 500g of solid potassium hydroxide. laboratory coat and safety spectacles) should be worn when preparing a base bath.9 8. A general risk assessment should be carried out prior to preparing. technical & academic staff Location: All William Perkin Laboratories Page 3 of 10 Revision: 00 FIRE EXTIGUISHERS AND FIRE BLANKETS.2 7. If possible use a physically different container than for the base bath. PREPARATION OF THE BASE BATH The base bath should be located.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. Take great care when using it. 7. such as a Bunsen burner. MSDS sheets can be found online from commercial chemical suppliers. ideally within a fumecupboard in a quiet part of the laboratory. using and disposing of cleaning baths.3 7. away from direct sunlight.5 7. Ensure that gloves. This will minimize confusion.0 8. may be performed in the vicinity of a base bath.0 above). The bath should be kept in a cool location.0 7.3 9. especially if they are stationed in close proximity to each other. The base bath should be labeled with its contents and with the appropriate hazard warning signs indicating that it is flammable and corrosive (available at O:\Support & Safety\Safety\eps safety related equipment and hazards\Hazard Signs for Labs). (gloves.8 8. Active Date: 7 December 2012 Retired Date: 8. Take care to avoid splashes. (gloves.5 8. This equates to the contents of three Winchester bottles. Place a loose fitting lid on the base bath container. Bunsen burners. No activities involving an ignition source.10 9. The bath should be kept in a cool location.1 7.0 9. The fumecupboard should not be used for any purpose other than cleaning and should be free of clutter.2 9. away from direct sunlight. Ensure that adequate spill kits and absorbent material are available before initiating work.4 DOC # HWU_Perkin_ClBaths_SOP_09 . The area should be free of ignition sources such as live electrical circuits. and hot surfaces (including heat guns). PREPARATION OF THE ACID BATH The acid bath should be located.7 8. Ensure the presence in the laboratory of a carbon dioxide (Type B-C) or dry chemical (Type A-B-C) fire extinguisher and a fire blanket. ideally within a fumecupboard in a quiet part of the laboratory.

4 10. The acid bath should be labeled with its contents and with the appropriate hazard warning sign indicating that it is corrosive and toxic (available at O:\Support & Safety\Safety\eps safety related equipment and hazards\Hazard Signs for Labs). while the acid bath is essentially to remove any residual base that may be coating the glass.7 Location: All William Perkin Laboratories Page 4 of 10 Revision: 00 The acid bath MUST be prepared in a fumecupboard. Glassware contaminated with metal residues will not be cleaned by the base bath. technical & academic staff 9. If more concentrated baths are formulated these will be increasingly hazardous and are not recommended.2M acid solution. Active Date: 7 December 2012 Retired Date: 10.0 10.3 10. Carefully add approximately 200mL of concentrated hydrochloric acid to the water. NMR tubes should never be placed in the base bath (see 12. (See photograph below). At this concentration. Volumetric glassware should only be held in the base bath for brief periods. For such items. safety glasses and a laboratory coat) when using cleaning baths.6 9.8 9. Many organometallic reagents will react vigorously with bases. The volumes of acid/water suggested will equate to approximately 0. The base bath acts as the principal cleaning bath and is used first.1 10.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. Glassware to be placed in the base bath should first be rinsed with water and a little acetone to remove any excessive grime. The acid bath will not normally act as a cleaning bath.10 9. due to the evolution of corrosive acidic fumes. e. An exothermic reaction occurs when acids and water mix.6 DOC # HWU_Perkin_ClBaths_SOP_09 .5 10. RAs. soaking in 6M HCl solution may be required until the solid has dissolved.11 9. The bath will be rapidly deactivated by very dirty glassware. adding a small amount of water to a large volume of acid can lead to splash injuries from concentrated acid. Leave the acid bath in the fumecupboard until any fumes from the acid are dispersed.2 USE OF THE CLEANING BATHS Always wear personal protective equipment (gloves. To a large plastic container (20-25L) add approximately 10L of cold water.12 10.5 9. the acid bath may be mildly corrosive. Ensure that glassware which has been in contact with materials incompatible with base is pretreated before cleaning. 9. Never add water to acid.9 9. Cover the bath with a loose fitting lid.g. Ideally the bath should be sited permanently in the fumecupboard. It is recommended that a faceshield be worn for this part of the operation in case of splashing of acid.0 below).

17 10. it is likely that the bath has become saturated with vacuum grease from quickfit glass joints. The pH of the acid bath will increase due to contamination with base during transfer of glassware. Ensure that all glassware is submerged below the surface of the liquid. Be aware that evaporation will also cause the bath to become more concentrated and therefore more corrosive. excess grease will deactivate the base bath.21 11. All glass joints should be separated before placing in the base bath.11 10. carefully place the glassware to be cleaned in the base bath. the glass items should be recovered from the bath. the base bath solution should be in physical contact with all parts of the item. REGENERATION AND DISPOSAL OF THE CLEANING BATHS.20 10. See 8.2 11.12 10. While wearing heavy duty gloves.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students.g. excess liquid shaken off. After soaking. The base bath will lose its effectiveness over time due to the build up of grease and other materials. Again. Check all items before placing in the bath. Do not drop the glassware in the bath as this may cause splashing of caustic base material.0 11. Check the baths for any cracks or holes before reuse.19 10. Keep the lid on the container when not in use to reduce evaporation of the solvent.4 DOC # HWU_Perkin_ClBaths_SOP_09 .16 10. See Perkin Chemical SOP08 SpecWaste for details. Items should not be left for longer than this as the glass may degrade and thin. The base bath contents should be carefully transferred via a funnel to an appropriate container(s) e. then thoroughly rinsed with water. glass Winchester bottles and processed as special waste.7 Location: All William Perkin Laboratories Page 5 of 10 Revision: 00 Do not place broken glassware in the base bath. excess grease should first be removed with a paper towel. The cleaning baths should be periodically regenerated. Inevitably there will be some loss of solvent due to evaporation.0 below). Failure to do this may result in the joints becoming welded together permanently. Evaporation of water may require the periodic replenishing of the acid bath.9 10. Both bath containers should be cleaned to remove any solid deposit before being refilled. Prolonged soaking in the bath will lead to degradation and a consequent thinning of the glass.14 10.13 10.0 above for guidance on the preparation of the baths. consequently the base bath will need to be periodically replenished with isopropanol.1 11. In this instance it should be processed as special waste (see Perkin Chemical SOP08 SpecWaste).8 10. beakers e. It is not necessary to hold glassware in the acid bath for prolonged periods. further measures may be needed.18 10.10 10. Again. The base bath will need to be regenerated (see 11. If the glassware is not clean at this stage. For effective cleaning. It is normally permissible to dispose of acid bath contents down the drain followed by copious flushing with water. the glassware should be carefully placed in the acid bath. These should not be placed in the bath. however it is sometimes convenient to leave overnight. In the case of greased quickfit glassware. Items which are cracked or obviously damaged may break completely producing dangerous glass shards. will need to be physically pushed below the surface. technical & academic staff 10.0 and 9. Do not leave items in the base bath for more than one overnight period. ensure all areas are exposed to the liquid. Hollow items such as round bottomed flasks.15 10.t. After removal from the acid bath.c.3 11. This should not be carried out if it has become contaminated with toxic or noxious material. After rinsing. RAs. Ensure that appropriate gloves are worn for this procedure. glassware should be thoroughly rinsed with water before placing carefully in a hot oven to dry. If a greasy deposit is found to be coating the glass. Active Date: 7 December 2012 Retired Date: 10.

A long form (c. CLEANING NMR TUBES Location: All William Perkin Laboratories Page 6 of 10 Revision: 00 NMR tubes should never be cleaned in a base bath.1. Placing the NMR tube on the pipette Inverted NMR tube resting on Pasteur pipette Condenser tubing Vacuum pump inlet 12. This may be extremely difficult to remove. The suction from the pump will dry the tube within a few minutes.a. NMR tubes should be cleaned immediately after use.5. If not.0 12.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. The tube should then be carefully supported in a clamp attached to a retort stand. 12.7.2. RAs. A modest suction should be applied through the pipette. Brief use of a hot air gun will accelerate the process. technical & academic staff 12.6.4. Active Date: 7 December 2012 Retired Date: DOC # HWU_Perkin_ClBaths_SOP_09 .3. 12. 12. The NMR tube should be inverted and placed on the pipette (see photographs below). The tube should be emptied of solution and rinsed with acetone three times. 12. 12. The glass is easily degraded and the tubes are highly likely to be physically damaged. 230mm) Pasteur pipette should be carefully attached to the rubber tube of a water or analogous pump (wear gloves). the volatile NMR solvent will evaporate and leave solid material coating the glass tube.

The fumehood must be free of any sources of ignition e. If unsure how to proceed seek help and retrieve the necessary MSDS sheets. MANAGEABLE CHEMICAL SPILLS (Rule of thumb 100 mL – 500 mL): 1 2 3 4 5 6 Eliminate sources of ignition. After absorbing any excess liquid. 7 MAJOR CHEMICAL SPILLS (e. SMALL SPILLS (generally less than 100 mL): Small spills generally consisting of only a few mL may be wiped up using paper towels or other absorbent pads. Prolonged exposure to heat will damage the tube and inhibit spinning in the spectrometer.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. hot hotplates. RAs.g. Keep people out of the immediate area.8.0 13. TRAINING. Eliminate sources of ignition. The fumehood must be free of any sources of ignition e. Supervisors must verify that laboratory workers understand the hazards involved in the use of cleaning baths. package all contaminated material in a suitable container.4. DOC # HWU_Perkin_ClBaths_SOP_09 Active Date: 7 December 2012 Retired Date: .2. Transfer the material containing the spill to a plastic container and carry to a fumehood for later disposal. If the residual waste is hazardous.1.g. This should be done as quickly as possible. Alert others working in laboratory. 13. A full 2.5L bottle of flammable organic solvent dropped & smashed on the floor) 1 2 Alert others working in laboratory and adjacent areas to evacuate the building. attach a label and submit for waste disposal. technical & academic staff 12. while minimising any exposure to vapours. clean-up materials should be placed in the fumehood and allowed to evaporate. SPILL PROCEDURES. Each laboratory will nominate a research worker deemed to be responsible for maintenance of the cleaning baths. All laboratory workers must be made aware of and have easy access to the Health and Safety Policy. 13. 14.g. hot hotplates. Location: All William Perkin Laboratories Page 7 of 10 Revision: 00 Never put NMR tubes in a drying oven. The Department will provide a safety briefing to all laboratory users before they are authorised to use cleaning baths. The person cleaning up the spill should wear a respirator and gloves. A chemical binder is available in WP115 for small spills. 13. Establish barriers if the spill has occurred in public passageways. Allow fumes to evaporate in the fumehood overnight or over a weekend. 13.3.0 Refer to product Material Safety Data Sheet and the instructions on spill kits to be prepared for carrying out proper spill clear-up-procedures.

You will find a red phone in the middle of corridor on each floor. Remove victim to fresh air. 4 5 6 7 15. 15. DO NOT give anything by mouth if victim is unconscious.5. Meet security to inform them of the details. A chemist. Security Officers and/or the fire department. DOC # HWU_Perkin_ClBaths_SOP_09 Active Date: 7 December 2012 Retired Date: . the affected individual must be examined at a medical facility. If an individual ingests an organic solvent have them rinse their mouth out with water.6.31/3. Formulate a clean-up plan in consultation with the Safety Officer. Phone security by picking up a red corridor phone. Advise them of your name and give a quick summary of the details.1. On picking up the phone you will be automatically connected to the University Central Control Room. FIRST AID PROCEDURES Any splash or exposure of the skin should be immediately. On picking up the phone you will be automatically connected to the University Central Control Room. 15. 15.3. In the event of eye contact.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. call for emergency assistance using a red corridor phone and contact a departmental first aider through the Perkin Building stores. DEPARTMENTAL FIRST AIDERS ARE: Name Koen Collart Georgina Rosair Sarah Walker Jack Corps Tel Ext 4235 8036 4233 4239 Room No WP 2. flush for 15 minutes with water.15 minutes. technical & academic staff 3 Location: All William Perkin Laboratories Page 8 of 10 Revision: 00 Pull the fire alarm. DO NOT give anything by mouth unless instructed to do so by qualified medical staff. 15. Advise them of your name and status and give a quick summary of the details of the spill.27 WP G. thoroughly flushed for 5 . with knowledge of the chemical that was spilled and who is also educated in the use of (SCBA) will do the clean up. You will find a red phone in the middle of corridor on each floor.03 WP 1. Retrieve the necessary MSDS sheet(s) if safe to do so. RAs.2.15 WP2. The plan may involve two people wearing self-contained breathing apparatus (SCBA). while a Safety or a Security officer observes from a safe distance. Do not allow contaminated clothing to remain in contact with the skin.4. Immediately contact a departmental first aider through the Perkin Building stores and call for emergency help by using a red corridor phone.21 15. If skin irritation or dermatitis develops.0 15.

J. RAs. 6. HALE. Boca Raton 2000 SOP Prepared by: Dr D. No. R. Location: All William Perkin Laboratories Page 9 of 10 Revision: 00 1. FURR. 5th Edition. technical & academic staff 14. CRC Press. Inherent Safety and Pollution Prevention Strategies for the Analytical Laboratory. CRC HANDBOOK OF LABORATORY SAFETY. KEITH A. 4.13 REFERENCES.Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. Managing the Modern Laboratory Vol.. 2004 2. Ellis SOP Reviewed by: DOC # HWU_Perkin_ClBaths_SOP_09 Active Date: 7 December 2012 Retired Date: .

Standard Operating Procedure Acid and Base Bath Use Investigator: UG & PG students. technical & academic staff Location: All William Perkin Laboratories Page 10 of 10 Revision: 00 Signatories: Name Signature Name Signature DOC # HWU_Perkin_ClBaths_SOP_09 Active Date: 7 December 2012 Retired Date: . RAs.

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