Document LJJbQQN6OaN9NqzwnY9738emg

PUB. NO. CP--PI --1973 PUB. NO. TR--P6-1973 JANUARY 25, 1973 OFFICIAL STANDARDS PROPOSAL PROPOSED AMERICAN NATIONAL STANDARD GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORMER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS, C107.1- ( ) DSW 010204 NATIONAL ELECTRICAL MANUFACTURERS ASSOCIATION 155 EAST 44TH STREET, NEW YORK, N. Y. 10017 STLCOPCB4001657 TABLE OF CONTENTS PREFACE General........................................................ Benefits...................................................... Risks..................... ........................... .. Alternatives................................................ Interdepartmental Task Force on PCB's Section Page 1 1-3 11 11 11 12 12 CAPACITOR GUIDELINES Introduction............... ................... ................ Capacitor*grade Askarel............................. Plant Housekeeping and Employee Safety Control of Water Effluents ................. Scrap Disposal Procedures........................... Labeling.......................................................... 2 1-9 21 21 21 26 26 28 TRANSFORMER GUIDELINES General Guidelines Specific Guidelines 3 1-7 31 35 DISPOSAL SERVICES 4 1-2 APPENDIX--ANALYTICAL PROCEDURES AND LABORATORY SERVICE ORGANIZATIONS. A Tentative Procedure for die Determination of Airborne-polychlorinated Biphenyls Analysis of Water and Sediment for Polychlorinated Biphenyls...................................... 5 1-23 S 1-8 5 9-16 1973 by National Electrical Manufacturers Association DSW 010205 STLCOPCB4001658 o -9 <o3 $ to 3 2 3 s30 o tHQw- 8 co a 8 9 H S5 'e- <cw3H-> ol U s EP --a t- 5au 73 a S7 <0 IQ-H* c<u " 1 U ao c-- <o uo V n C4 (FOR NEMA USE ONLY) KEEP INFORMED Your attention is called to the fact that NEMA Official Standards Proposals have a maximum life of five years from the date of approval shown on the fronr cover. Prior to the end of the five-year period, they may be approved by an outside organization, or adopted as a NEMA Standard, or rescinded. This NEMA Official Standards Proposal CP-P1-1973 (TR-P6-1973) will soon be submitted for review and approval to the C107 Committee on Use and Disposal of Askarel and Askarel Soaked Materials of the American National Standards Institute. If you will fill out and return the postal card shown above, we will be glad to inform you of the final disposition of this NEMA Official Standards Proposal. There is no extra charge for this service. It would be appreciated if you will return one card from each copy of this publication which is in your possession. Each card should be filled out in full with your complete mailing address. DSW 010206 STLCOPCB4001659 i*cS III6 OSM 010207 STLCOPCB4001660 National Electrical Manufacturer! Association PROPOSED AMERICAN NATIONAL STANDARD GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORMER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS, C107.1- ( ) (NEMA Official Standards Proposal 1-25-1973.) This proposal was prepared by NEMA, in cooperation with the Capacitor and Transformer Working Groups of the American National Standards Institute Committee, C107, on Use and Disposal of Askarel and Askarel Soaked Materials. These proposed standards will be periodically reviewed for any revisions necessary to keep them up to date with advancing technology. Proposed or recommended revisions should be submitted to: Technical Director Manager, Engineering and Safety Regulations Department National Electrical Manufacturers Association 155 East 44th Street New York, New York 10017 l DSW 010208 STLCOPCB4001661 GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORMER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS SECTION 1 PREFACE DSW 010209 \ STLCOPCB4001662 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS FROFOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA. OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA SECTION 1 PREFACE I, GENERAL Askarels consisting of or containing polychlori nated bipheynls (PCB't) have been used in many applications fot over forty years, but only recently was evidence discovered that PCB's are widely dispersed in die environment. Systematic investi gations of the biological effects of PCB's have been undertaken within the past few yean to es tablish the effects of specific formulations upon specific species. Some studies have shown that PCB's may be an environmental contaminant. Simultaneously, significant steps have been taken by U. S. Industry to limit further releases of PCB's to the environment. PCB's have been used in three broad types of applications for the past forty years, as follows: (a) "open ended" applications, for example, in paints, specialty inks, paper coatings, plastics, etc., (b) "nominally closed" applications, for example, as the working fluid in hydraulic or heat transfer systems; and (c) "closed electrical system" applications, specifically as the insulating fluid in certain types of transformers and capaci tors. The Monsanto Company is the sole U. S. producer of PCB's. It has discontinued supplying the material for all type (a) and (b) applications. Evaluations of the alternatives and risk/benefits involved in the continued use of PCB's in closed electrical systems are summarized in the following. Askarel-Riled power and industrial capacitors are significantly smaller, more reliable, more durable, and safer than oil-Riled capacitors. As a result, askarels have supplanted mineral oils in more than 90 percent of the power and industrial capacitors made today. Over the past few decades most of the equipment that incorporates such capacitors has been designed to take particular advantage of the size, safety and reliability benefits of askarel ca pacitors (e.g., many types are today less than 14 percent of the size of equivalent oil capacitors and have a life expectancy of ten to more than twenty years). Various federal, state and local codes, therefore, require their continued use in or adjacent to public, commercial and industrial buildings which locations present the greatest potential danger to life and property. Ill, RISKS In the United States, medical records over a nearly forty-year period show that the only ad verse health effects experienced by U. S. workers exposed to askarels, either during the manufacture of these liquids or of electrical equipment con taining these liquids, have been limited to oc casional cases of non-chronic chloracne or other temporary skin lesions or irritations, II, BENEFITS Askarel- filled transformers do not bum or sustain fire under conditions of internal electrical arcing. Askarel-Riled transformers and capacitors are delivered to customers as sealed units from which there is no escape of askarel under normal oper ation. While certain types of equipment failures can permit loss of some askarel to the environ- Section 1 Page 1 DSW 010210 STLCOPCB4001663 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS. FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA meni, Transformer failures are limited approx imately 0.02 percent of the units in service per year. With respect to capacitors, such losses are limited to approximately 0.02 percent of the askarel put into service per year. In addition, limited amounts of PCB's can get into the en vironment during the manufacture, delivery, improper use, maintenance, repair and disposal of transformers and capacitors. Specific control measures have been instituted by individual manufacturers and are supplemented and strengthened by national standards and procedures such as this Guide which provides information to prevent the inadvertent loss of PCB's to the environ ment at all stages from initial askarel manufacture through ultimate disposal. iV. ALTERNATIVES For technical and local and national code rea sons, it would be impossible to replace most askarelfllled transformers now in service with oil-filled units of equivalent ratings, without major construction changes that would be required to compensate for the fire resistance of the askarel-filled units. For certain applications and locations, dry-type trans formers may replace askarel-filled transformers. For new installations, while many of the lim itations noted above would still apply, building and installation design provisions could be made to accommodate the use of oil-filled, open drytype, or sealed dry-type transformers provided necessary technical, code, physical size, and cost considerations are properly evaluated. Section 1 Page 2 The principal alternative to askarels for capac itors is mineral oil, but such replacement would return capacitor technology to its pre-1932 level and would necessitate the redesign and replace ment of such widely used equipment as fluores cent light fixtures and racks for power and in duction heating capacitors, which could not now accommodate the increased si2e of oil capacitors while maintaining their present ratings. The cost of askarel liquids is about five to ten times more than mineral olL Thus, long before there were any environmental concerns about PCB's, there was a strong economic in centive ro find other less expensive Insulating liquids with the desirable characteristics of askarels. Since the 1930's at least ten major chemical or electrical companies have invested large amounts of time and money in this search, all with no success. While potential substitutes that are most costly than askarels have also re ceived some consideration (e.g., fluorinated liquids), little is known about either their elec trical performance or possible ill effects upon the environment, There are today no fluids that can be used as a direct replacement for askarels. V. INTERDEPARTMENTAL TASK FORCE ON PCB'S An in-depth study of PCB's has recently been completed by five Executive Branch Departments of the federal government. This Interdepartmental Task Force on PCB's issued their report entitled, "Polychlorinated Biphenyls and the Environment," in May, 1972. * See Section 1 Page 3 for the conclusion quoted from page 4 of this report. * Distributed by the National Technical Infor mation Service, U. S. Department of Commerce, Springfield, Virginia 22151. Price $6.00. DSW 010211 STLCOPCB4001664 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA "The use of PCB'S should not-be banned entirely. Their continued use for transformers and capacitors in the near future is considered necessary because of the significantly increased risk of fire and explosion and the disruption of electrical service which would result from a ban on PCB use. Also, continued use of PCB's in transformers and capacitors presents a minimal risk of environmental contamination. The Monsanto Company, the sole domestic producer, has reported voluntarily eliminating its distribution of PCB's to all except manu facturers of electrical transformers and capacitors. " Reference should be made to the Interdepartmental Task Force Report for additional information and conclusions. DSW 010212 Section 1 Page 3 STLCOPCB4001665 GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORM ER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS SECTION 2 CAPACITOR GUIDELINES DSW 010213 V i STLCOPCB4001666 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA ' SECTION 2 CAPACITOR GUIDELINES I. INTRODUCTION The environmental effects of askarels are under In- depth study by governmental and other agencies. Askarels have been considered relatively harmless to humans based on about forty years of safe industrial usage. There has been no known instance of human Injury when they were used under the normally ac cepted precautions and conditions of handling in both manufacturing and user applications. Traces of askarels are being found in the en vironment and in fish and birdlife. The long-term genetic and ecological effects are not yet com pletely understood For these reasons, care should be taken to contain askarels and minimize their entry into the environment. There are two general classes of askarels used by the electrical industry. The higher chlorinated grades are the more persistent in nature. Because of their high degree of nonilammability, they are used in transformers where personnel safety is of paramount importance. Capacitor-grade askarel has a lower degree of chlorination (composed primarily of the 3-chlorine isomers of biphenyl) and a higher degree of bio degradability. Generally, it has not been found in animal life. It is used in capacitors where the extreme degree of nonflammability required in transformers is of less importance. Although capacitor- and transformer-grade askarels both contain members of the PCB family, they do differ in composition, degree of biodegrad ability, persistence in nature, electrical stability, chemical stability, and degree of nonflammability (both are recognized as nonflammable). It is for these reasons that this section of the Guidelines is intended to apply to capacitor-grade askareL II. CAPACITOR-GRADE ASKAREL In September of 1971, a new grade of capac itor impregnant, Aroclor 1016, was made avail able to the industry. This new grade contains a typical concentration of 0.4 percent by weight of the higher boiling homologs of the chlorinated biphenyls. * Aroclor 1016 replaces Aroclor 1242 which previously was the major capacitor impreg nant and contained around 7 percent of the higher boiling homologs (the mote persistent in nature). This 0.4 percent level of the higher boiling ho mologs should be the maximum concentration acceptable in any capacitor impregnant. Aroclor 1242 and 1254, previously used as impregnams, do not meet this requirement and should no longer be used in capacitors designed and manufactured for alternating-current applications. Aroclor 1016 has the same UL nonflammability rating as Aroclor 1242. Its typical properties ate given in Table 1. (See Section 2 Page 2.) III. PLANT HOUSEKEEPING AND EMPLOYEE SAFETY The following procedures and limits are in tended to be minimum requirements to be met by manufacturers and users of capacitors contain ing askareL Handling, control and disposal pro cedures are given, together with exposure limits and indicated antidotes and cleanup procedures. A. Material Askarel for use in capacitors should consist of homologs and isomers of chlorinated biphenyl with the concentation of the higher boiling homologs at about 0.4 percent. * Aroclor 1016 is considered to be the standard impregnant meeting these require ments. * Monsanto Method T-02302. Section 2 Page 1 DSW 010214 STLCOPCB4001667 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA. OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Table 1 Typical Properties of Aroclor 1016 property and Method Color (APHA).................................................................................... Condition............................................................................................. Specific Gravity at 25/15.5*C (ASTM D 1810)....................... Acidity (mg. KOH/g.) (ASTM D 974, D 664)....................... Moisture............................................................................................... Refractive Index at 25*C (ASTM D 1817)................... .............. Inorganic (Free) Chlorides (ASTM D 1821)............................... Pour Point (ASTM D 97)................................................................ Dielectric Constant (ASTM D 924) (1000 Hz at 100*C) .... Resistivity (ASTM D 1169) (500 VDC at 100'C, 0.1-inch Gap.)........................................................................................... Hydrolysis Stability Test (ASTM D 1820) (As Chlorides) ... Thermal Stability Test (ASTM D 1936) (As Chlorides)......... Distillation Range (ASTM D 20 Corrected) 10 percent Distilled by Weight.............................................. 90 percent Distilled by Weight............................. .. Higher Boiling Homologs (Monsanto Method T-02302)........... Sulfates (ASTM D 117).................................................................... Dielectric Strength at 25*C (ASTM D 877)............................... Flash Point, Cleveland Open Cup (ASTM D 92)..................... Fire Point............................................................................................ Corrosion Test (6 hours at 210'C with bright aluminum foil) Change in Weight of Aluminum...................... .................. Viscosity at 100*F (SUS) (ASTM D 88)..................................... Specific Heat at 25*C .................................................................... Coefficient of Expansion (ASTM D 1903)..................... .............. Fixed Chlorine (Carius)................................................ ................ Power Factor at 100*C 60 Hz (Monsanto Method T-2273) Bulk.......................................................................................... Drums.......................................................................................... Typical Values 40, max. Clear 1.362-1.372 0.010 max. 35 ppm, max. 1.6215-1. 6235 0.05 ppm, max. -14*C or lower 4.70-4.90 500 x 109 ohm-cm, min. 0.5 ppm. max. 0.4 ppm, max. 323*C, min. 356*C, max. 0.4 percent, max. None , 35 kv, min. 338*F, min. None to Boiling Point 0.0 percent 71-81 0. 30 0.00068 cc/cc/*C 41. 3 0. 5 percent 1 percent, max. 4 percent, max. Section 2 Page 2 DSW 010215 STLCOPCB4001668 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA. OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS. FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Commonly used solvents include benzene, kero sene, acetone, trichloroethane, trichloroethylene and perchloroethylene. Typical vapor pressure data for Aroclor 1016 are.- o*c = 0.001 mm 25*C = 0.006 mm 150*C = 4.3 mm 200'C = 29.0 mm At 25*C and 760 mm Hg pressure, saturated alt contains approximately 0.09 mg/liter. [l mg/liter = 90.0 ppm (v/vj l ppm (v/v) = 0.011 mg/liter] B. Bulk Fluid Shipment, Receiving, and Transfer__________________ __ Shipment of askarel from point of manufacture to point of receiving should be done in closed containers such as rail tank cars, truck tanks, marine or barge tanks, or sealed drums. Con tainers should be labeled as to contents and carry a label cautioning against loss of fluid to the open environment. Containers used to transport askarel should not be used for storage or to transport other material without being com pletely cleaned of all traces of askareL (Clean ing procedures must take cognizance of pre cautions against excessive exposure and of the need for proper disposal of contaminated cleans ing solvents and materials as set forth in Part V of this Section,) Transfer from shipping containers to processing systems should be through closed piping or tubing with appropriate valves, pumps, etc, provision should be made for trapping and disposing of fluid lost by leakage or spills from the transfer system and from the storage con tainers. Drums to be retired from use should be cleaned before crushing, delivery to scrap dealers, or other disposaL Contaminated cleaning fluids and ma terials should be disposed of as indicated in Part V. C. General Safety Precautions Although it is generally accepted that exposure to capacitor*grade askarel is not hazardous pro vided simple precautions are taken, exposure should still be avoided. 1. Vapors--Hie odor of askarel is noticeable well below the maximum air concentra tions considered safe. Up to 1.0 milligram per cubic meter of air has been determined to be the maximum safe level of exposure during an 8-hour work day (Par. G, referance 8). The procedures for performing the necessary analyses are contained in Section 5, "A Tentative Procedure for the Determination of Airborne-Polychlorinated Biphenyls. " Breathing vapor or fumes from heated askarel should be avoided. Provisions should be made for adequate ventilation and regulation of manufacturing operations to avoid open exposure to askarel (especially at 55*C or higher). The gases produced when askarel is decomposed by very high temperatures (such as that of an electric arc) in the pres ence of air or organic insulating materials contain a high percentage of hydrogen chlo ride, and small percentages of carbon di oxide, carbon monoxide and oxygen. Minute concentrations of this combination of gases are very unpleasant and irritating, thus giving ample warning of their presence. If exposure to high concentrations of askarel is necessary under emergency conditions, an approved gas mask or self-contained breathing appa ratus should be worn. Such exposure should be under the surveillance of other personnel capable of rescue in case of an accident. If the odor of askarel is detected by the person wearing protective equipment, he should im mediately go into fresh air. All gas masks, respirators and replacement parts should have Bureau of Mines approval and be maintained on a regular schedule in accordance with the manufacturer's recommendation. Section 2 Pane 3 DSW 010216 STLCOPCB4001669 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION 8Y ORGANIZATIONS OUTSIDE OF NEMA 2. Liquid--Unlike insulating oil, tfiere is vir tually no lire hazard in handling askareL A limited solvent action (similar to that for paint thinner) on the fats and oils of the skin with prolonged contact may lead to drying and chapping of the skin. As with insulating oil, some people are al lergic to askarel and continued exposure may result in skin irritation. Both the liquid and vapor are moderately irritating to eye tissue. Operating procedures should be such as to minimize or eliminate contact with askarels. Use of eye protection is recommended. The use of porous gloves which can absorb and retain askarels is to be avoided. Bar rier creams# ot resistant glovest should be used if contact is unavoidable. Use of en closed transfer and handling equipment, processing equipment, and mechanical washers reduces direct contact. Medicinal washes or mild detergents fol lowed by the application of cold cream will reduce the irritation resulting from the contact of an open cut or abrasion with askareL Safety glasses with side shields or a face shield should be worn when handling askarels. If liquid askarel contacts the eyes, the eyes should be irrigated immediately with large quantities of running water for 15 minutes and then examined by a physician. (A drop of castor oil has been found to reduce ir ritation. ) Persons developing a skin irritation or res piratory tract irritation while working with askarels should be placed under the super vision of a physician. Ingestion or swallowing of askarels is not generally regarded as a problem of the in dustry. Should accidental ingestion occur, a physician should be consulted. Hands should be washed with warm water and soap before eating, drinking, smoking or using toilet facilities. D, Manufacturing Housekeeping Manufacturing equipment and operating pro cedures should safeguard against loss of askarels to the environment through proper containment and disposal procedures. Enclosed systems of sealed piping, properly gasketed joints, valves, containers, and pro cessing chambers should be used for any portion of the operation where askarel temperatures may exceed 55*C. Enclosure should preferably extend to all other portions of the system insofar as practicable. Containment provisions should be established around all askarel processing areas to ensure against inadvertent loss to sewer systems by spillage, leakage, or other uncontrolled con ditions or events. Spills of askarel should be removed promptly by means of absorptive material, such as sawdust, or trapped and removed by pumping or other suitable means. * For example, PLY No. 9 Gel (Mllburn Co., Detroit, Michigan), or Kerodex #71 (Ayers Laboratories, P. O. Box 8236, Church Street Station, New York, N. Y. 10049), or the equivalent. t Edmont, Solvit 5-352 (Mersick of Bridgeport, 22 Cross Street, Bridgeport, Conn. 06601), or the equivalent. Section 2 Page 4 DSW 010217 STLCOPCB4001670 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Waste fluids containing askarel not suitable for reconditioning or reuse should be collected (by means of traps, drip pans, trays, etc.) from the various parts of the manufacturing and processing area (including washers or other cleaning devices). Disposal should be made in accordance with Part V of this section. Wiper rags, clothing and other extraneous ma terials saturated with askarels should be collected within the containment area for properly controlled laundering or disposal (see Part V of this section). E. Disposal of Askarel Wastes Methods for disposal of liquids and saturated solids generated by the manufacturing operation should be in accordance with those outlined in Part V of this section and should include (but not be limited to) the following wastes: 1. Contaminated liquid askarel which is unsuit able for reclaiming as a dielectric fluid, 2. Liquid askarel from solvent operations or water/detergent type washers. 3. Saturated earth or other absorbent media from filtering operations. 4. Saturated sawdust or other absorptive ma terials from spills. 5. Saturated filters from vapor control devices and other filters. 6. Saturated wastes (paper, rags, etc.). 7. Saturated, spent gasket materials. 8. Askarel-contaminated vacuum pump oils. 9. Askarel-contaminated stream jet vacuum system condensates. F. Miscellaneous Procedures 1. Spills by leakage from finished capacitors should be cleaned up promptly by means of absorbent media which should then be moved to containers provided for that pur pose within the containment area and later disposed of properly. 2. Askarel wastes should never be disposed of down effluent drains or sewers. The utmost care must be exercised to prevent accidental loss by these avenues to the environment. 3. Capacitors failing tests or otherwise desig nated for disposal must be controlled and handled in accordance with the intent of the procedures above, finally being disposed of by one of the means outlined in Part V of this section. G. References 1. Monsanto Industrial Chemicals Company; Technical Bulletin 0-FF/1R, Aroclor Polychlorinated Polyphenyls (Biphenyls) (November 1971). 2. American Conference of Governmental In dustrial Hygienists: Threshold Limit Values for 1964. AMA Archieves of Environmental Health 9:545 (1964). 3. Treon, J. F,, F. P. Cleveland, J. Cappel, and R.W. Aichley: The Toxicity of the Vapors of Aroclor 1242 and Aroclor 1254. American Industrial Hygiene Association Quarterly 17:204 (1956). 4. Elkins, H. B.: The Chemistry of Industrial Toxicology. John Wiley and Sons, Inc., New York (1959), Section 2 Page 5 OSW 010218 STLCOPCB4001671 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 5. Drinker, C. K., M. F. Warren, " and G. A, Bennet: The Problem of Possible Systemic Effects from Certain Chlorinated Hydrocarbons. Journal of Industrial Hy giene and Toxicology 19:283 (1937), 6. Drinker, C. K.: Further Observations on the Possible Systemic Toxicity of Certain of the Chlorinated Hydrocarbons. Journal of Industrial Hygiene and Toxicology 21:155 (1939). 7. Greenburg, L,, M. R. Mayers, and A.R. Smith; The Systemic Effects Re sulting from Exposure to Certain Chlorinnated Hydrocarbons. Journal of Industrial Hygiene and Toxicology 21:29 (1939), 8. Hygienic Guide Series " Chlorodiphenyls" (January-February 1965) by die American Industrial Hygiene Association, 210 Haddon Avenue, Westmont, N. J. 08108. IV. CONTROL OF WATER EFFLUENTS The industry goal is to eliminate askarel In plant water effluent streams. However, it Is recognized that existing drain systems in capac itor manufacturing plants are probably contam inated as a result of past practices, and askarel traces may continue to show up In effluent streams for some time. However, the level should continue to decrease with the proper containment of askarel wastes and no further discharges into drain systems. Other sections of this Guide provide that no askarel wastes of any kind be disposed of in any water effluent streams and that accidental spills be prevented from getting Into such streams. Section 2 Page 6 A. Concentration limits The 1972 EPA proposals are to keep PCB levels in rivers and lakes below 0,01 parts per billion. Plant effluent streams should be man aged and controlled In a manner consistent with this goal. B. Monitoring Streams On a regular basis consistent with plant sit uations, all effluent streams should be analyzed. The procedures for performing the necessary analy ses are contained in Section 5, Analysis of Water and Sediment for Polychlorinated Biphenyls. This procedure or its equivalent should be used. C. Methods for Minimizing Effluent Stream Contamination The ideal approach is to totally isolate all effluent streams that could be contaminated with askarels during manufacturing processes and pre vent them from being discharged from the plant. Carbon adsorption, limestone beds, and solvent extraction are techniques which can be applied to reduce the askarel content of effluent streams. These techniques may be most useful in cleaning up water used in plant processing and to permit recycling. V. SCRAP DISPOSAL PROCEDURES The manufacture and use of capacitors involve processes which produce askarel-saturated solids and liquids containing or composed entirely of askarel, which should be disposed of as wastes. Specific sources of these materials appear through out this document but may be placed into three categories: DSW 010219 STLCOPCB4001672 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 1. Capacitor units impregnated with askarel, production and field rejects. 2. Manufacturing process liquid wastes con taining askarel. 3. Solid waste purposely or accidently saturat ed with askareL Disposal should be done in a manner which is consistent with proper concern for the environment and which minimizes any release of askarels to the environment. A. Disposal of Capacitor Units Scrap capacitor units can be generated during manufacturing processes or during field service. Production rejects are those capacitors which are rejected after the impregnation process in the course of production by the capacitor manufac turer. They may be rejected for mechanical or electrical reasons, or because of obsolescence. Field rejects are those units which are re jected or which, for other reasons, are to be scrapped after shipment from the plant where they were manufactured. 1. Production Rejects--Rejected capacitors in capacitor manufacturing plants represent a concentration of askareL It is important that their disposition be made in a manner consistent with proper concern for the en vironment. Therefore, capacitors should be disposed of only in supervised dry land fill sites which meet all applicable State requirements. Care should be exercised in Insure that no loss of liquid wi 11 occur during transportation to the disposal site. Incineration of scrap capacitors in facilities designed to accept such solids should provide an alternative means of disposal as such services become available in the future. 2, Field Rejects--Small capacitors (defined as containing less than 2 pounds of askarel) are practically always used as components in other electrical or electromechanical equip ment. Typical examples of large quantity usage of such capacitors are in fluorescent lamp ballasts and residential air conditioning equipment. Failure of such capacitors may result in scrapping of the device of which it is a part (as in a fluorescent ballast) or re placement and scrapping of the individual capacitor (as in a room air conditioner). However, the majority of such capacitors do not fail in service, but are scrapped as a result of wearing out or obsolescence of the devices in which the capacitors are used as components. Thus, the matter of disposal is characterized by a low concentration of small quantities of askarel throughout the country and, indeed, throughout the world. Fortunately, the nature of the devices and equipment in which such capacitors are used is such that they ate normally disposed of in dry landfills as a matter of convenience. Since it is impractical at present to exercise any meaningful control over the disposition of the bulk of such devices and equipment, it is imperative that askarel used for im pregnating small capacitors be limited to the recently introduced type which contains a typical concentration of 0.4 percent of the higher coiling homologs. * Large capacitors (those incorporating more than 2 pounds of askarel) should be disposed of according to the procedure for production rejects (see par. A. 1). * Monsanto Method T- 02302. Section 2 Page 7 DSW 010220 STLCOPCB4001673 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA B. Disposal of Liquid Wastes * All waste askarel or liquid wastes containing askaral should be disposed of in accordance with one of the following procedures: 1. Incineration--'Present knowledge indicates that proper incineration must involve a suitable balance between dwell time and temperature in the incinerator plus oxygen availability and, finally, suitable scrub* bent to remove the HC1 which will be formed; e.g,, (1) 2-second dwell time at 2000*F and 3 percent excess oxygen in stack gas; (2) 1 1/2-second dwell time at 2700`F and 2 percent excess oxygen in stack gas. These facilities should meet the applicable requirements of the State in which they are located and should control effluents within the limits set forth in this document. c. Containers used for this purpose should not be used for any other materials or retired from service until they are com pletely cleaned. Any solvents used in cleaning these containers will be con taminated with askarel and should be disposed of according to the same pro cedures herein described. C. Disposal of Solid Wastes (See par. A for Scrap Capacitors) All solid wastes which have been saturated with askarel should be disposed of by the following procedure: 1. The saturated wastes should be placed into leak-proof containers and transported to a supervised dry landfill site meeting State requirements. Alternatively, they can be disposed of by incineration in State-approved facilities. 2. Toxic and Hazardous Waste Disposal SitesCertain landfill sites have been classified by State and Federal Governments as suit able for the disposal of toxic and hazard ous liquids. Where such approved sites exist, they may be used for the disposal of liquid wastes described in this document. (See Section 4.) 3. Packaging and Shipment-- a. Transportation to the disposal facility should be in containers which will pre vent leakage and accidental loss of askarel to the environment, b. Containers should be labeled as to contents and precautions relative to loss to the environment. Section 2 page 8 2. Solid absorbents used for spills can be dis posed of uncontained In the supervised dry landfill site; transport to the site should be in closed containers. Alternatively, in cineration can be used in accordance with par. B (See Section 4 for facilities). VI. LABELING Capacitor units vary greatly in size and in end use or application. Small capacitor units are fre quently applied as a component of another piece of equipment such as a fluorescent lighting ballast, a roadway or area lighting luminaire, a motor, etc. In such applications a label on the capacitor unit referencing approved disposal procedure would not normally be visible when the piece of equipment is disposed of. DSW 010221 STLCOPCB4001674 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA For the foregoing reasons the method of providing disposal instructions for small capacitors and large capacitors is treated separately. 1. Small Units (Incorporating Less Than 2 Pounds of Askarel)--Small capacitors are de fined as those which contain askarel in quan tities up to about two (2) pounds each and in which the free liquid does not exceed 0.4 pound. They are hermetically sealed in me tallic cases. Such capacitors are applied as a component of a larger piece of equipment. Attaching a label to such equipment refer encing this Guideline or describing disposal procedures would be of limited practical value. 2. Large Capacitor Units (Incorporating More Than 2 pounds of Askarel)--The capacitor manufacturer should affix a label in a con spicuous place, referencing this document or describing disposal procedures consistent with it. This label should contain, as a minimum, the following information: CAUTION THIS CAPACITOR CONTAINS A POLY CHLORINATED BIPHENYL (PCB). TO AVOID POSSIBLE ENVIRONMENTAL CON TAMINATION, IT SHOULD BE DISPOSED OF ONLY IN SUPERVISED DRY LANDFILL AREAS MEETING STATE REQUIREMENTS OR IN INCINERATION FACILITIES DE SIGNED FOR DISPOSAL OF PCB'S. SEE AMERICAN NATIONAL STANDARDS INSTITUTE GUIDELINES C107.1- ( ) FOR FURTHER INFORMATION. (WHEN APPROVED, COPIES WILL BE AVAILABLE FROM ANSI, 1430 BROADWAY, NEW YORK, NEW YORK 10018.) DSW 010222 Section 2 Page 9 STLCOPCB4001675 GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORMER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS SECTION 3 TRANSFORMER GUIDELINES .' > 'rrJ- v- I-4 !** >1 - *< % 0SW 010223 ) STLCOPCB4001676 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA SECTION 3 TRANSFORMER GUIDELINES I. GENERAL GUIDELINES A. Definitions-- Types of Transformer Askarels The term askarel generally describes a broad class of nonflammable synthetic chlorinated hydro carbon insulating liquids widely used in transformers, reactors, and accessory equipment operated at power frequencies. Askarels of various compositional types are in use Qor the general properties and types, see ASTM Specification for Chlorinated Aromatic Hy drocarbons (Askarels) for Transformers, D 2280. Under arcing conditions the gases produced, while consisting of predominantly noncombustible hydro gen chloride, can contain varying amounts of com bustible gases depending upon the askarel type. 1. Vapors-- The odor of askarel is noticeable well below the maximum safe air concen trations. Depending upon the composition of the askarel used, from 0.5 to 1.0 milli gram per cubic meter of air has been de termined to be the upper safe level of ex posure during an 8-hour work day. (See American Industrial Hygiene Association Hygienic Guide Series--January/February, 1965.) The procedures for performing the necessary analyses are contained in Sec tion 5, "A Tentative Procedure for the Determination of Airborne-Polychlorinated Biphenyls." This procedure or its equiva lent shall be used. The following trademarks are used by electrical manufacturers to designate the askarels used in their products: Asbestol Chlorextol Inerteen No- Flamol Pyranol Saf-T-Kuhl B. Safety Precautions Based on about forty years of safe industrial usage, askarels have been considered as relatively harmless materials to humans. There has been no known instance of human injury when askarels are used under the normally prescribed conditions of precaution and handling. Although it has been generally thought that ex posure to askarels is not hazardous provided simple ( precautions are taken, exposure should still be avoided and minimized. Breathing vapor or fumes from heated askarels should be avoided. High concen trations of vapors can cause irritation of the eyes, nose, throat and upper respiratory tract. Provisions shall be made for ade quate ventilation and regulation of manu facturing operations to avoid open exposure of hot askarels (55*c or higher). The gases produced when askarel is decomposed by very high temperatures (such as that of an electric arc) in the presence of air or organic insu lating materials contain a high percentage of hydrogen chloride, and small percentages of other gases. Minute concentrations of diis combination of gases are very unpleasant and irritating, thus giving ample warning of their presence. If exposure to high concen trations of askarels or its arced products is necessary under emergency conditions, an approved gas mask of the organic canistertype or self-contained breathing apparatus must be worn. Such exposure should be under the surveillance of other pereonnel capable of rescue in case of accident. If the odor of askarel or its arced products is detected by the person wearing protective Section 3 Page 1 DSW 010224 STLCOPCB4001677 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS. FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA equipment, he should immediately go into fresh air. All gas masks, respirators and replacement parts should have Bureau of Mines approval and be maintained on a regular schedule in accordance with the manufacturer's recommendation. 2. Liquid--Unlike mineral insulating oil, there is no fire hazard in handling askarels. A limited solvent action (similar to that for paint thinner) on the fats and oils of the skin with prolonged contact may lead to drying and chapping of the skin. As with insulating oil, some people are allergic to askarel and continued exposure may result in skin irritation. Both the liquid and vapor are moderately irritating to eye tissue. Operating procedures should require avoid ance of contact with any askarels. The use of porous gloves which can absorb and retain askarels is to be avoided. Resistant gloves and aprons of the neoprene, polyethylene, viton type should be used if contact is un avoidable. In case of spillage on the cloth ing, the clothing should ' - removed as soon as practical, the skin v and the cloth ing laundered. Medicinal washes or mile ctetergents followed by the application of cold cream will reduce the irritation resulting from the contact of an open cut or abrasion with askarel. Safety glasses with side shields or a face shield should be worn when handling askarels. Eyes which have been exposed to liquid askarel should be irrigated immediately with large quantities oi running water fot 15 min utes and then examined by a physician if the irritation persists. (A drop of castor oil has been found to reduce irritation.) Section 3 Page 2 Persons developing a skin irritation or respir atory tract irritation while working with askarels should be placed under supervision of a physician. Ingestion or swallowing of askarels is not generally regarded as a problem of the in dustry. Should accidental ingestion occur, a physician should be consulted. Hands should be washed with warm water and soap before eating, drinking, smoking or using toilet facilities. C. Transport Container Marking Any container such as tank cars, tank trucks, drums, cans, etc., used to transport transformer askarels, new or used, should be labeled with the following: CAUTION THIS PRODUCT CONTAINS POLYCHLORINATED BIPHENYLS (PCB'S). CARE SHOULD BE TAKEN TO PREVENT ENTRY INTO THE ENVIRONMENT THROUGH SPILLS, LEAKAGE, USE, VAPORI ZATION, OR DISPOSAL OF LIQUID OR CON TAINERS. AVOID PROLONGED BREATHING OF VAPORS OR MISTS. AVOID CONTACT WITH EYES OR PROLONGED CONTACT WITH SKIN. IF SKIN CONTACT OCCURS, REMOVE BY WASHING WITH SOAP AND WATER. FOL LOWING EYE CONTACT, FLUSH WITH WATER. IN CASE OF SPILLAGE ONTO CLOTHING, THE CLOTHING SHOULD BE REMOVED AS SOON AS PRACTICAL. SKIN WASHED. AND CLOTHING LAUNDERED. D. Receiving, Handling and Storage of Askarels Askarels are shipped in tank cars, tank trucks, steel drums, metal cans and test sample containers. When received, all containers should be inspected for leaks. DSW 010225 STLCOPCB4001678 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 1. Storage Tanks-- Storage tanks-should be erected so that inspection can be made for leaks or spills. Construction should be such that inadvertent leakage or spills are pre vented from reaching streams and sanitary or storm sewers. 1. Concentration Limits--The 1972 EPA pro posals are to keep PCB levels in rivers and lakes below 0.01 parts per billion. Plant effluent streams should be managed and controlled in a manner consistent with this goal. 2. Tank Cars and Tank Trucks--All bulk ship ment equipment should be inspected for leaks immediately upon receipt. Drain pans must be provided to prevent spillage from unload ing hoses and connections. Askarel liquid collected in drain pans should be placed in "SCRAP ASKAREL" drums for disposition. 2. Monitoring Streams--All plant effluent streams should be monitored on a regular basis, consistent with plant situations. The procedures for performing the neces sary analyses are contained in Section 5, "Analysis of Water and Sediment for Poly chlorinated Biphenyls." This procedure or its equivalent shall be used. 3. Methods for Minimizing Effluent Stream 3. Steel Drums, Cans, and Test Sample Con Contamination-- The ideal approach is to tainers--On delivery, all such shipments totally isolate all effluent streams that could I should be carefully inspected for leaks. be contaminated with askarels during manu The containers should be stored indoors in facturing processes and prevent them from an area especially selected for this purpose. being discharged from the plant. A curb should enclose the area to provide a basin for containing the askarel from one or more containers should the containers be damaged. The area must not have a drain which is connected to a sanitary or storm F. Disposal Procedures and Services sewer. 1. Sources of Materials Requiring Special If an indoor storage area is not possible, the Handling and Disposal Procedures--Liquids containers should be stored under a lean- to. containing PCB's and solids containing or contaminated with PCB's may be obtained from any of the following sources: transport containers, transformer manufacturing processes, in-test failures, liquids con E. Water Effluents-- Sampling, Concentration taminated beyond reclamation, in-service limits and Analytical Procedures________ transformer leaks and failures, askarel- The industry goal is to eliminate askarel in fllled transformers scrapped for any reason, plant water effluent streams. However, it is etc. recognized that existing drain systems from man ufacturing plants, repair shops and Installation 2. Classification for Disposal of Materials sites may be contaminated as a result of past Containing PCB's--In general, there are practices. Other sections of this Guide provide three types of materials requiring disposal: that no askarel wastes of any kind be disposed of liquids, burnable solid materials contain \ in any water effluent streams and that accidental spills be prevented from getting into such streams. ing PCB's and nonburnable solid materials contaminated with PCB's. Section 3 Page 3 DSW 010226 STLCOPCB4001679 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA a, Liquids. Liquids containing PCB's re quiring disposal by high-temperature incineration may consist of the follow ing: (1) PCB's contaminated with mineral oiL (2) Mineral oil contaminated with PCB's. (3) Nonreclaimable contaminated trans former askarels, arced askarels, askarels from manufacturing spills, and sump accumulation, etc., rich in PCB's, and askarels from holding basins, drip and drain pans, wash ings, sample jars and containers, etc. b. Burnable Solid Waste Material Contain ing PCB's. These materials can be dis posed of by high-temperature incinera tion and consist of cellulosic materials, rags, pressboard, wood, sawdust, fuller's earth in bulk or in cloth bags, blotter papers, nitrile or cork gaskets, etc. c. Nonburnable Solid Waste Materials Containing or Contaminated With PCB's. These materials may consist of coil structures, steel, copper, alu minum filter units of the steel mesh construction type, askarel drums, cans, etc. Materials of this nature should be allowed to drain with the liquid collected in drip pans, etc. Further removal of adhering PCB's can be accomplished by washing or solvent extraction with kerosene or Section 3 Page 4 other approved washing liquids such as perchloroethylene or trichloroethylene. Accumulated liquids can be disposed of as indicated in par. F. 2. a. Solid ma terials may be handled as normal scrap. 3. Shipment of Scrap Liquids for DisposalAll liquid scrap material should be placed in appropriate metal transport drums, prop erly labeled, for shipment to a company offering an acceptable disposal service. 4. Shipment of Burnable Solid Waste Ma terial Containing PCB's for DisposalMaterial of this type should be placed in open head drums with suitable closures and with the drum properly labeled for shipment to a company offering an ac ceptable disposal service. 5. Liquid and Solid Waste Disposal Service Organizations-- a. General. Disposal of askarels and askarel-soaked materials should be accomplished by means in which there is no significant release of askarel to the environment. At present, disposal is accomplished by carefully-controlled incineration of liquids and soaked soft ware, and by controlled landfill burial of apparatus and other hardware from which askarel has been previously drained and washed. Present knowledge Indicates that proper Incineration must involve a suitable balance between dwell time and tem perature in the incinerator plus oxygen availability and, finally, suitable scrub bers to remove the HCl which will be formed; e.g., (1) 2-second dwell time at 2000"F and 3 percent excess oxygen in stack gas; (2) 1 1/2-second dwell time at 2700*F and 2 percent excess oxygen in stack gas. DSW 010227 STLCOPCB4001680 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA These facilities should meet the appli cable requirements of the State in which they are located and should conaol efluents within the limits set forth in this document. Controlled landfill or deep-well dis posal can be used where permitted by Federal, State and local regulations. b. Costs. In addition to the normal costs of collecting scrap liquids and solids for disposal, additional costs borne by the owner of such scrap Include shipping containers, cost of transport to the dis posal service organization, and a dis posal fee usually based upon a per gallon or per pound charge. c. Disposal Services. Organizations offering disposal services are listed in Section 4, including their location, facilities available, types of material handled, and disposal procedures used. Specific shipping directions, disposal procedures and costs should be obtained from the organization. IL SPECIFIC GUIDELINES A. Transformer Manufacturers, Service Shops, etc. --Housekeeping It is necessary to assume that in filling equip ment with askarel and during further handling of this equipment an askarel spill may occur. There fore, it is necessary to provide facilities and a pro cedure for clean-up to prevent contamination. 1. Askarel Filling Area-- a. The location of fire askarel filling area should be adjacent to the test area and final shipping area to minimize the danger of damage of units during han dling. b. The main manufacturing area for fill ing equipment with askarel should be provided with impervious surface floors or suitable basins so constructed that any Inadvertent leakage or spills are prevented from reaching streams, san itary, or storm sewers. All askarelhandling equipment such as pumps, hoses, etc., shall be of the askarelresistant type. c. Drip pans shall be provided for hose connections and filling valves. 2. Special Containers for Scrap Materials-- a. Drums labeled "SCRAP ASKAREL" should be available for handling all spilled and waste askarel from sumps, failed units, drip pans, sample jars, etc. b. Open-head drums with suitable closures and labeled "SCRAP BURNABLE ASKAREL WASTE" should be available for handling contaminated cellulose in sulation, rags, paper pressboard, wood, gaskets, sawdust, etc. c. Separate containers for handling steel, copper, and aluminum, each adequately marked, shall be provided for the com ponents of contaminated core and coil assemblies. These containers are re quired for the various materials when repairing or scrapping assemblies. d. Containers for supplies of material for absorbing small askarel spills or clean-up of larger spills should be provided. Section 3 Page 5 DSW 010228 STLCOPCB4001681 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 3. Conditioning of Askarels-- ' a. Askarel Conditioning Equipment. The conditioning unit should be located either in the storage tank area or the main transformer manufacturing area for filling with askareL b. Fuller's Earth. Conditioning of new askarel or recycled askarel requires fuller's earth treatment. The spent fuller's earth in cartridges or bags, when replaced, should be allowed to thoroughly drain over drip pans to re move as much liquid askarel as possible. The cartridge units of steel mesh con struction should be placed in the " STEEL CONTAMINATED WITH ASKAREL" con tainer for disposition. Cloth bags filled with fuller's earth should be placed in the "SCRAP BURNABLE ASKAREL WASTE" container for disposition. 4. Teardown of Units for Repair or Scrap-- a. Drain all askarel from the unit either into a holding tank for reuse or into the drum labeled "SCRAP ASKAREL" for disposition, and then allow suffi cient time for all of the askarel to drain from the core and coils. b. Remove the core and coil assembly from the transformer. Sufficient ab sorbent material should be placed on the floor to absorb any askarel fluid that still drips from the transformer. c. Place all materials in the appropriate salvage containers during the dis mantling for later disposition. d. All used materials, including rags, sawdust, tape, etc., regardless of quantity, shall be put into the ap propriate containers for disposition. Section 3 Page 6 B. Transformer Labeling 1. New Transformers--All new transformers that contain PCB's shall have a label of adequate durability permanently and prominently at tached to the tank by the manufacturer, giving adequate warning and instructions. A suggested label includes the following: CAUTION THE INSULATING LIQUID IN THIS TRANS FORMER CONTAINS POLYCHLORINATED BIPHENYLS (PCB'S). CARE SHOULD BE TAKEN TO PREVENT ENTRY INTO THE ENVIRONMENT. IN CASE OF MALFUNCT ION OR LEAKS, CONSULT THE INSTRUC TION MANUAL OR THE MANUFACTURER. 2. In-service Transformers--The transformer manufacturer should make available suitable labels with a similar warning as shown in par. B. 1 for use on existing transformers. C. Transformer Users--Shipping, Installation, Maintenance, Sampling, Apparatus Disposal 1. General--Askarel-filled transformers are delivered to customers as sealed units ftom which there is no escape of askarel under normal operation. While certain types of equipment failures can permit loss of some askarel to the environment, such cases ate extremely rare. 2. Transportation and Receiving--Immediately upon receipt of the equipment and following any transportation ot handling accident which could affect the integrity of the tank, bush- DSW 010229 STLCOPCB4001682 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Ings or radiators, the transportation vehicle, tank and fittings should be examined for any leakage or spillage that may have occurred in shipping. If leakage is evident, the cause should be corrected and the spillage soaked up with absorbent materials such as sawdust, followed by a clean-up of the affected area with rags soaked with kerosene or other ap proved solvent such as perchloroethylene or trichloroethylene. All materials used should be collected for proper disposition as described in Section 3 Part I, par. F. " Disposal Pro cedures and Services." precautions previously described for drip pans, proper disposal of filter media, etc., apply. 5. Sampling--It is common practice to sample askarel from a transformer for periodic maintenance testing. As previously de scribed, such samples should be taken in a manner to avoid any contamination of the environment. Washings should be col lected for proper disposal. Field and labo ratory test samples, washings, etc., should also be collected for proper disposaL 6. Transformer Disposal--The ultimate dis 3. Installation and Periodic Inspection--Fol lowing installation, the unit should again be inspected for any damage or leakage. posal of an askarel-filled transformer may be accomplished in either of two ways: It is recommended that periodic in-service a. Complete drainage and dismantling I inspections be made for any leaks. with the proper disposal of the askarel and askarel-soaked components as de 4. Filling, Filtering, or Drying Askarel-- scribed earlier in Section 3, Part 1, par. F, " Disposal Procedures and Most askarel units are shipped with the proper amount of askarel but if it becomes neces Services." sary to top off a unit, the manufacturer's b. Disposition of askarel transformers by instructions should be followed. means of junk or scrap dealers should be avoided unless a transformer is first If it is necessary to dry or fuller's-earth- drained, followed by soaking the interior treat an askarel unit, the manufacturer's with a suitable solvent. Accumulated instructions should be followed. When fil liquids and washings are to be disposed tering or conditioning askarel, all of the of as described earlier. I Section 3 Page 7 OSW 010230 STLCOPCB4001683 It cf1 .. r r i \ f i .* GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORMER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS SECTION 4 DISPOSAL SERVICES - ";V-' DSW 010231 STLCOPCB4001684 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA SECTION 4 DISPOSAL SERVICES In addition to the supervised dry landfill sites which may be used for the disposal of askarelcontalning scrap, the following additional known facilities and services have been established, and others may be available. Chem-Trol Poludon Services, Inc., 4818 Lake Avenue BlasdelL New York 14219 Phone 716" 826-5850 This organization has facilities and services capable of handling: 1. Liquids--Askarels alone or mixed with solvents or oils. Disposal by high tem perature incineration. 2. Solids (Software)--Askarel-soaked com pounds, rags cartons, absorbing earths, etc. Disposal by incineration or scientific landfill. 3. Solids (Hardware)--Capacitors, transformer tanks, cores, askarel-soaked metals. Dis posal by scientific landfilL Has solvent extraction capability. Monsanto Company 800 No. Lindbergh Boulevard St. Louis, Missouri 63166 Phone 314-694-3352 This organization has facilities and services capable of handling askarel liquids alone or mixed with other oils or solvents by high-temper ature incineration. Liquid is pumped through a gun with atomizing steam into incinerator. Temperatures are maintained at 2000-2500*F with auxiliary natural gas. Exit gases are quenched to 180*F by contact with water. Gas is then passed through a high-energy venturi scrubber for removal of particulates. Before exhausting to air (110*F), gases are passed through a packed column scrubber to remove HCL Nuclear Engineering Company Eastern Division P. O, Box 146 Morehead, Kentucky 40351 Phone 606-784-6611 Disposal Division Sheffield, Illinois Phone 815-454-2624 This organization provides containerization, transportation and disposal services of all liquids and solids (including hardware). Disposal is in controlled chemical and scientific landfill area. AEC licensed for radioactive waste disposal. Has two West Coast locations in states of Washington and California in addition to above. Rollins-Purle, Inc. Box 3349 Wilmington, Delaware Phone 302-478-5150 19899 This organization has facilities and services capable of handling: ; 1. Liquids--Askarel alone or mixed with solvents or oils. Disposal is by hightemperature incineration. 2. Solids (Software)--Askarel-soaked com pounds, rags, cartons, absorbing earths, etc. Disposal is by incineration at com bustion temperatures up to 2500*F. In cineration gases are scrubbed, and en trained solids removed before exhausting to air. ' Section 4 Page 1 DSW 010232 STLCOPCB4001685 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Disposal facilities axe available at' the following locations: Logan: Rollins-Purle, Inc. Route 322 Logan Township Bridgeport, New Jersey 08014 Baton Rouge: Rollins- Purle, Inc. Scenic Highway & W. Cheatham Lane Scotlandville East Baton Rouge Parish Louisiana 10807 Houston: Rollins-Purle, Inc. Tidal Road & Highway 134 Deer Park, Texas 77536 Section 4 Page 2 DSW 010233 STLCOPCB4001686 "\ ( GUIDELINES FOR HANDLING AND DISPOSAL OF CAPACITOR- AND TRANSFORMER-GRADE ASKARELS CONTAINING POLYCHLORINATED BIPHENYLS fc. SECTION 5 APPENDIX ANALYTICAL PROCEDURES AND LABORATORY SERVICE ORGANIZATIONS . u. v.'* Hi DSW 010234 I STLCOPCB4001687 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA. OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA ' SECTION 5 APPENDIX ANALYTICAL PROCEDURES AND LABORATORY SERVICE ORGANIZATIONS Analytical procedures for determining PCB's in air, water, and sediments are given in Parts I and II of Section 5. The following laboratories are representative of those offering services for PCB analyses: Carus Chemical Cotp. 1375 Eighth Street LaSalle, Illinois 61301 Phone 815-223-1500 Limnetics, Inc, (Subsidiary of Carus Corp.) 6132 West Fond du Lac Avenue Milwaukee, Wisconsin 53218 Phone 414-461-9500 Gollob Analytical Service Corp, 47 Industrial Road Berkeley Heights, New Jersey 07922 Phone 201-464- 3331I. I. A TENTATIVE PROCEDURE FOR THE DETERMINATION OF AIRBORNE-POLYCHLORINATED BIPHENYLS A, Scope This procedure is based on techniques used by the Monsanto Industrial Chemical Company for the isolation and determination of polychlorinated biphenyls (PCB's) in water, soil/sediment, and biological materials. Absolute confirmation of PCB structures is not obtained with this method. Where needed, addi tional structure proof should be obtained using techniques such as mass spectrometry to further identify GC fractions. B. Principle Airborne PCB's are absorbed in toluene by drawing the air through one or more fritted bubblers or impingers in cylinders filled with toluene. After sampling a suitable amount of air, the scrubbing solvent is diluted or concentrated, and interfering components, if present, are removed by chemical treatment and column absorption chromatography. The amount and type of PCB's present is deter mined by electron capture gas chromatography (EC/GC). Section 5 Page 1 OSW 010235 STLCOPCB4001688 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA C. Reagents - Hexane............................. .......................................... Toluene...................................................................... Sodium sulfate................... ...................................... Alumina adsorption.................................................. Distilled water ................. ....................................... Sulfuric acid.............................................................. Potassium hydroxide........................................... .. Ethanol............................................................... .. 2.5% (w/v) alcoholic potassium hydroxide .... 9/1 (v/v) sulfuric acid-water................................ PCB Standards............... ............................................ Section 5 Page 2 Nanograde, Mallinckiodt Chemical Works, Catalog No. 4159. Nanograde, Mallinckrodt Chemical Works, Catalog No. 8092. Anhydrous, granular: AR grade, Mallinckrodt Chemical Works, Catalog No. 8042. Heat at 400*C for 1 hour prior to use. (For chromatographic analysis) 80/200 mesh, Fisher Scientific Company, Catalog No. A540. Heat at 400*C for a minimum period of 4 hours and deactivate with 5% (w/w) distilled water. Alumina column preparation: Fill a chromato graphic column with hexane up to die point where the reservoir joins the column and push a glass wool plug to the bottom with a glass rod. In a 50 ml beaker measure 35 ml of de activated alumina ( 30g), and pour this slowly into the column. Tap or vibrate the column to settle the alumina and top the alumina with 2-3 cm of anhydrous sodium sulfate. Wash the column with 50-100 ml of hexane ptiot to the addition of the sample. Extracted with hexane to remove hexane soluble electron capturing impurities. Analytical Reagent Grade, SG = 1. 84. Analytical Reagent Grade. Formula 2B. Dissolve 'l* 12.5 grains of AR grade KOH in 500 ml of ethanoL Carefully add 270 ml of AR grade sulfuric acid to 30 ml of distilled water in a 500 ml iced beaker. Aroclor 1016, 1221, 1242, 1248, 1254 and 1260. See Fig. 5-3 through 5-9 (pages 17 to 23), DSW 010236 1 \ STLCOPCB4001689 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS. FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA P. Apparatus 1. Gas scrubbing bottles, high form, ground glass joint, fritted coarse discs, 2. Separatory funnels equipped with ground glass stoppers and Teflon stopcocks: 125, 250, 500, 1000 and 2000 ml capacities. 3. Kunderna-Danish evaporative concentrators, 500 ml capacity equipped with 3-ball Snyder columns and graduated 5 ml ca pacity vials: Ace Glassware Company, Catalog No. 6707. 4. Chromatographic columns, glass, 10" x 20 mm (OD) with a 5" x 50 mm (OD) reservoir at the top, equipped with Teflon stopcocks. 5. Flat- bottomed boiling flasks, 125 ml ca pacity: Ace Glassware Company, Catalog No. 6896, Code - 04. 6. Liebig condenser, 200 mm in length: Ace Glassware Company, Catalog No. 5915, Code - 12. 7. Hot plates, Corning PC-100* Fisher Scientific Company. 8. Water bath, Thelco, Precision Scientific, Model No. 84, Fisher Scientific Company. 9. 10 v 1 Hamilton syringes, catalog No. 701N. 10. Dry test meter or wet test gas meter. 11. Laboratory vacuum pump. 12. Rotating vacuum evaporator, 13. Usual laboratory glassware. E. Sampling (See Fig. 5-1) The air to be sampled for airborne PCB's is drawn through a gas scrubber (s) and a dry test meter using a laboratory vacuum pump. The sam pling flow rate it controlled by bleeding in air via a needle valve located between the pump and the meter. At the end of the sampling period, the metered gas volumes are corrected for temperature and pressure to cubic meters at 25*C and 760 mm Hg- Sample Inlet Air Bleed Dry Test Meter Fig. 5-1 SAMPLING TRAIN Exhaust Section 5 Page 3 DSW 010237 STLCOPCB4001690 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA It U Important to note that neither the capacity nor the efficiency of die gas scrubber(t) for removal of airborne PCB't have been experimentally eval uated. For this reason, it is best to minimize the sampling flow rate and maximize the sampling time period to obtain measurable amounts of PBC*s. When high flow rates must be employed or a larger capacity may be needed, it is recommended that several gas scrubbers be used in tandem. It is cautioned that, until the efficiency and capacity of the toluene gas scrubber has been ex perimentally established, this procedure should be only used to measure relative PCB levels sampled under equivalent conditions. F. Procedure 1. After scrubbing the desired amount of air, record the metered volume, pressure, and temperature. 2. Quantitatively transfer the scrubbing solvent to a round-bottomed flask and reduce the volume to approximately 2 ml by rotary vacuum evaporation. 3. Quantitatively transfer die concentrate to a 30-ml beaker with the aid of several small portion of toluene. 4. Inject a fraction of a p 1 of the concen trate into the gas chromacograph to check for interferences and determine the approx imate level of PCB's present. If no interferences are present, dilute or concentrate * die sample to a known volume, as deter mined by die electron capture chromato gram, and proceed with die gas chroma tographic analysis. 5. If interferences are present, proceed with the chemical treatment and column chro matographic clean-up procedures. Section 5 Page 4 6. Transfer the concentrate to a 125-ml ex traction flask with the aid of several small portions of solvent. 7. Evaporate the concentrate just to dryness with a gentle stream of dry fllteted air and add 25 ml of 2.5% alcbolic potassium hy droxide. 8. Add a boiling chip, put a water condenser in place, and allow the solution to reflux for 45 minutes. 9. After cooling, transfer the solution to a 250-ml separatory funnel with die aid of 25 ml of distilled water. 10. Rinse the extraction flask with 25 ml of hexane and add ft to the separatory funnel. 11. Stopper the separatory funnel and shake vigorously for at least 1 minute. Allow the layers to separate and transfer the lower aqueous phase to a second sepa rator funnel, 12. Extract the saponification solution with a second 25-ml portion of hexane. After the layers have separated, add the first hexane extract to the second separatory funnel and transfer the aqueous alcohol layer to the original separatory funneL 13. Repeat the extraction with a third 25-ml portion of hexane. Discard the saponifi cation tolndon and combine die hexane extracts. 14. Carefully add 25 ml of the sulfuric acid solution (9:1 concentrated sulfuric acid/ water) to the hexane extracts. DSW 010238 STLCOPCB4001691 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL 18 AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS. FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 15. Stopper the separatory funnel ahd shake vigorously for at least 1 minute. Allow the layers to separate and discard the lower aqueous acid layer. Repeat this step until the acid layer is colorless. 16. Wash the hexane with a 25-ml portion of water. Discard the water wash. 11. Filter the hexane extract through a 4" funnel plugged with glass wool which is covered with a layer of sodium sulfate into a Kunderna- Danish evaporative con centrator. 18. Add a small boiling chip, put the Snyder column in place, and reduce the hexane volume to less than 5 ml by heating the apparatus in a 80-90C water bath. 19. After cooling, remove die 5-ml graduated tube and transfer the hexane extract to an alumina adsorption column, washing it in with several 5-ml portions of hexane. 20. Carefully add 100 ml of hexane to the column reservoir and collect the total eluent in either a 250-ml volumetric flask or a Kunderna-Danish evaporative concentrator. 21. If the column eluent is collected in a volumetric flask, dilute to volume with hexane, and proceed with the gas chro matographic analysis. 22. If the column eluent is collected in a Kunderna-Danish evaporative concentrator, reduce solvent volume, cool, dilute to volume, and proceed with gas chromato graphic analysis. G. " Electron Capture Gas Chromatographic Procedure Instrument ........... F & M 402 Biomedial Gas Chromatograph Detector............... High Temperature Ni63 Electron Capture Cell 6 mm x 6' Glass Column, 4% XE-60 on 80/100 mesh Chromosorb W, HP, AW-DMCS Column Temper ature ............... 160-190'C Detector Temper ature ........ 300*C Injection Port Temperature.. 195-215'C Pulse ..................... 150 Flow Rates........... Helium Carrier oj 60 ml/min Argon-Methane Purge ml/min 120 Using EC/GC as the determinative step, inject in duplicate 1-10 \i 1 of each solution into the chromatograph. By comparison with standard so lutions injected, in duplicate, under the same operating conditions, determine the amount and type of Aroclor using the individual or total peak height and area methods. H, Sample Concentration Concentration of sample extracts is necessary, prior to clean up by chromatographic or chemical means, to reduce sample size and increase sensi tivity. The preferted method of concentrating allows minimum loss through volatilization or chemical decomposition and requires a minimum time. The three methods of solvent volume re duction most commonly used are evaporation by exposure to a stream of air, evaporation employ ing a Kunderna-Danish evaporative concentrator equipped with a Synder column, and evaporation under reduced pressure. All three techniques have been used without encountering any significant losses from voladzation or chemical alternation. Section 5 Page 5 DSW 010239 STLCOPCB4001692 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL 18 AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA. OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA I. Column Adsorption Chromatography and Chemical Clean Up Silica gel, Florisil and alumina deactivated with 0, 1.0, 1.5, 2.0 and 5 percent water were investigated as adsorbents for the elimination of interferences. Alumina (5% water) was found to be more effective and reproducible than either silica gel or Florisil. The activity of alumina varies with age and lot; therefore, 5% water was added to the alumina, after heating for a minimum of 4 hours at 400*C, to insure a re producible activity. Saponification and subsequent extraction of the sample with sulfuric acid is an effective way to remove a number of chlorinated hydrocarbon in terferences as well as other matrix interferences. PCB's are not affected. J, Column Performance Column performance is the key to effective gas chromatographic analysis and, as such, die choice of column materials is particularly im portant. Ideally, the support employed should be inert, mechanically strong, and of high surface area. Chromosorb W,*HP, AW-DMCS fulfills these requirements and is recommended for this work. A variety of polar and non-polar liquid phases have been investigated. The following columns have been found to provide adequate separation, etc., for use in PCB analysis by electron capture: 4% (w/w) DC-200, SF-96, OV-17, SE-30, SE-54, XE-60, Apiezon L, and 6h QF-1. DC-200 and XE-60 or QF-1 have been found to be the most suitable of these liquid phases. Another important consideration when working with an extremely sensitive detector and conse quently low levels of materials is column con ditioning, With polar phases such as XE-60 and Section 5 Page 6 QF-1, operating a new column overnight at a temperature 25-50*C higher than that to be used during analysis results in a more stable column. A no-flow conditioning technique is employed to condition non-polar columns. The column is purged with carrier gas. heated for 30 minutes at an elevated temperature without carrier flow and then cooled to room temperature. At the end of this cycle, the carrier flow is resumed and the conditioning is completed as in the case of the polar liquid phase. Two precautions: during con ditioning, the column should not be connected to the detector, and one should not exceed the max imum safe temperature of the liquid phase. Since all liquid substrates bleed to one degree or another and columns eventually degrade, all new columns should be characterized with two column performance indicator?--the number of theoretical plates (N) and a tailing factor (T). p, p'-DDT is employed to check these parameters because it is known to degrade on "poor" columns. In this manner, one can determine if the perform ance of a new column is satisfactory and when the column performance begins to fall off. A column is considered good if the number of theo retical plates per foot is on die order of 400-500 with tailing factors of 1.0-1.3. Calculation of these parameters is shown in Fig. 5-2, page 8. Additionally, there should be no significant ex traneous peaks upon injection of a pure p, p'-DDT standard. Other chromatographic conditions that can be adjusted are column temperature and flow rates. Although resolution of a mixture Increases with decreasing temperature, a temperature should be chosen that allows the elution of all components within a convenient time period. The flow rates shown are optimum for a given instrument, column and detector system. These should be adjusted if better results can be achieved. DStt 010240 I STLCOPCB4001693 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Two gas chromatographic systems have been used for PCB analysis--F & M Model 402 and 5750. Any system of instrument and column suitable for chlorinated pesticides is satisfactory for PCB analysis. The use of the high temper ature Ni^3 electron capture cell is highly recom mended. The ability to operate at higher tem peratures prevents maintenance problems due to contamination from high boiling components. Glass columns should also be employed. The amount of PCB's in Case I samples is deter mined by preparing a plot of the major peak height or area versus concentration. With Case 111 sam ples, a peak free from interference is used. When dominant interferences are present, one or more of the chemical clean-up procedures is employed. In all cases, the response of the electron cap ture detector must be linear for quantitative analysis. K, Detection and Measurement Quantitative determinations employing the elec tron capture detector are non-stoichiometric measments made by comparing peak heights or areas for known concentrations with those for unknown compositions. Three variations of the peak height or area quantification procedures have been em ployed: Case 1 -- EC gas chromatogram of PCB un known unchanged with respect to standard PCB with no evidence of interferences. Case II---- EC gas chromatogram of PCB un known altered with respect to standard PCB with no evidence of interferences. Case III-- EC gas chromatogram of PCB un known unchanged with respect to standard PCB with evidence of in terference. L, Contamination in determining PCB's in biological materials by electron capture gas chromatography, labora tory sources of contamination can be a major problem. The samples and extracts should never be allowed to come in contact with materials other than glass. Teflon or metal. Laboratory glassware should be thoroughly washed with hot, soapy water, rinsed with distilled water, acetone, and then hexane. All equipment should also be rinsed again with hexane just prior to use, and blanks should be frequently carried through all steps of the procedures to insure against the possibility of contamination. M. Sensitivity Two parts per billion. Absolute sensitivity--0. 5 x 10"3 grams. Volume injected--5 p L Final volume of extract--5 mL I Sample size--250 mL DSW Section 5 Page 7 010241 STLCOPCB4001694 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 1, Theoretical Plates, N N = 16 (x/y)2 . Calculating Column efficiency 2. Tailing, T T = a/2b Calculating the Tailing Factor Section 5 Page 8 Fig. 5-2 COLUMN PERFORMANCE INDICATORS DSW 010242 STLCOPCB4001695 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA II. ANALYSIS OF WATER AND SEDIMENT FOR POLYCHLORINATED BIPHENYLS A. Scope This methodology Is used by the Monsanto Industrial Chemical Company for die determination of the amount and type of polychlorinated biphenyls (PCB's) in water and sediment samples. Absolute confir mation of PCB structures is not obtained with this method. Structure proof can be obtained using addi tional techniques such as mass spectrometry to further identify the GC fractions. B. Principle The PCB's in water and sediment samples are extracted into an organic solvent. Interfering compo nents are then removed from the extracts by chemical treatment and column adsorption chromatography. The amount and type of PCB's present is determined by electron capture gas chromatography (EC/GQ. C. Reagents Hexane........................................................................ Nanograde. Mallinckrodt Chemical Works, Catalog No. 4159. Acetonitrile..................... ...................... .................... Nanograde, Mallinckrodt Chemical Works, Catalog No. 2442. Sodium sulfate.......................................................... Anhydrous, granular: AR grade Mallinckrodt Chemical Works, Catalog No. 8042, Heat at 400*C for 1 hour prior to use. Alumina adsorption.................................................. (For chromatographic analysis) 80/200 mesh, Fisher Scientific Company, Catalog No. A540. Heat at 400'C for a minimum period of 4 hours and deactivate with 5% (w/w) distilled water. Alumina column preparation: nil a chromato graphic column with hexane up to the point where the reservoir joins the column and push a glass wool plug to the bottom with a glass rod. In a 50 ml beaker measure 35 ml of de activated alumina (r\_/30g). and pour this slowly into the column. Tap or vibrate the column to settle the alumina and top the alumina with 2-3 cm of anhydrous sodium sulfate. Wash the column with 50-100 ml of hexane prior to the addition of the sample. (Continued) Section 5 Page 9 DSW 010243 STLCOPCB4001696 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA Distilled water Sulfuric acid............... Potassium hydroxide................................................ Ethanol............................... ......................................... 2.5% (w/v) alcoholic potassium hydroxide ... 9/1 (v/v) sulfuric acid-water ......................... .. PCB Standards Extracted with hexane to remove hexane soluble electron capturing impurities. Analytical Reagent Grade, SG = 1. 84. Analytical Reagent Grade. Formula 2EL Dissolve rsj 12.5 grams of AR grade KOH in 500 ml of ethanoL Carefully add 270 ml of AR grade sulfuric acid to 30 ml of distilled water in a 500 ml iced beaker. Aroclor 1242. 1248, 1254 and 1260. (See Fig. 5-4, page 18, and Fig. 5-6 through 5-9, pages 20 to 23.) D. Apparatus .* 20 1. Separatory funnels equipped with ground glass stoppers and Teflon stopcocks; 125, 250, 500, 1000 and 2000 ml capacities. 2. Kundema-Danish evaporative concentrators, 500 ml capacity equipped with >ball Snyder columns and graduated 5 ml car pacity vials: Ace Glassware Company, Catalog No. 6707. 3. Chromatographic columns, glass, 10" x 20 mm (OD) with a 5" x 50 mm (OD) reservoir at the top, equipped with Teflon stopcocks. 4. Sintered glass filter funnels, 600 ml ca pacity, 90M. 5. Flat-bottomed boiling flasks, 125 ml car pacity: Ace Glassware Company, Catalog No. 6896, Code - 04. - Section 5 Page 10 6. Liebig condenser, 200 mm in length: Ace Glassware Company, Catalog No. 5915, Code - 12. 7. Hot plates, Corning PC-100: Fisher Scientific Company. 8. Water bath, TTielco, Precision Scientific, Model No. 84, Fisher Scientific Company. 9. Reciprocating variable speed shaker, Eberbach Corporation, Fisher Scientific Company. 10. 10 it 1 Hamilton syringes, Catalog No. 701N. 11. 32 oz all-glass mortals and pestles. 12. 8" x 12" x 2" (2 1/2 qt) Pyrex baking dishes. 13. U. S. Standard Sieve, No. 30, Fisher Scientific Company. 14. Usual laboratory glassware. DSW 010244 STLCOPCB4001697 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA E. Sampling It is to be assumed that a rather wide variety of sampling techniques may be employed in col lecting samples submitted for analysis. For this reason water and sediment samples should be treated as follows: 1. Water--Where possible the entire water sample, including the container in which it was collected, should be extracted with hexane. With larger samples, where this is not physically possible, the containers should be simply agitated and a 250 ml portion used for the analysis. (See par. F.) 2, Sediment--Any excess water should be de canted and the entire sediment transferred to a glass baking dish to air dry at room temperature. The dried material should be transferred from the dish into a mortar and ground. The ground sediment should be sieved, remixed, and a 250 g portion taken for analysis. (See par. G.) F. Extraction of Water Samples 1. After agitating, transfer the entire aqueous sample or a 250 ml aliquot into a gradu ated glass cylinder. Record the volume of the sample and quantitatively transfer it to a separatory funnel with distilled water. 2. Rinse the graduated cylinder with two 50-ml portions of hexane and add each to the separatory funnel. 3. Stopper the separatory funnel and shake vigorously for at least 1 minute. Allow the layers to separate and transfer the lower aqueous phase to a second separa tory funnel.4 * * 4. Extract the water sample a second time with a 50-ml portion of hexane. After the layers have separated, add the first hexane extract to the second separatory fttnnel and transfer the aqueous layer to the original separatory funnel. 5. Repeat the extraction with a third 50-ml portion of hexane. Discard the aqueous layer and combine the hexane extracts. 6. Filter the combined extracts through a 4" funnel plugged with glass wool which is covered with sodium sulfate. Collect the filtrate in a Kunderna-Danish evaporative concentrator, add a small boiling chip, put the Snyder column in place, and reduce the hexane volume to less than 5 ml by heating the apparatus in a 80-90*C water bath. (CAUTION: SOLVENT VAPORS MUST BE VENTED TO A HOOD.) 7. After cooling, remove the 5-ml graduated tube and transfer the hexane extract to an alumina adsorption column, washing it in with several 5-ml portions of hexane. 8. Carefully add 100 ml of hexane to the column reservoir and collect the total eluent in either a 250-ml volumetric flask or a Kunderna-Danish evaporative concentrator. 9. If the column eluent is collected in a volumetric flask, dilute to volume with hexane, and proceed with the gas chro matographic analysis. 10. If the column eluent is collected in a Kunderna-Danish evaporative concentrator, reduce solvent volume, cool, dilute to volume, and proceed with the gas chro matographic analysis. Section 5 Page 11 DSW 010245 STLCOPCB4001698 OFFICIAL STANDARDS PROPOSAL THI8 OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA. OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA G. Extraction of Sediment and Soli Samples 1. Decant off any excess water and tranfer the entire sediment sample to a glass baking dish. Air dry at ambient temperature (heat should not be applied). 2. When dry, transfer the soil/sediment to a mortar and grind. Sieve the ground mate rial through a No. 30 mesh sieve and weigh 250 g (to the nearest 0.01 g) into a 16-oe narrow neck screw cap (aluminum foil liner) glass bottle. 3. Moisten the soil with water (sv 10 ml) and add 150 ml of acetonitrile. Cap the bottle tightly, and mechanically shake it for a minimum period of 1 hour. 4. Quantitatively transfer the acetonitrile ex tract into a 600-ml sintered glass filter fun nel containing a 1/4" layer of anhydrous sodium sulfate. Collect the filtrate in a 600- ml beaker (vacuum filtration may be necessary). 5. After the acetonitrile has completely drained into the beaker, wash the bottle twice with 50-ml portions of acetonitrile, adding each wash to the funnel after die previous wash has completely percolated through the sed iment. 6. Quantitatively transfer the extract to a Kundema- Danish evaporative concentrator, add a small boiling chip, put the Snyder col umn in place, and reduce the solvent volume to less than 5 ml by heating die apparatus in a 80-90*C water bath. (CAUTION: SOLVENT VAPORS MUST BE VENTED INTO A HOOD.)7 7. After cooling, remove the 5- ml graduated tube and transfer the concentrate of extracts to a 125-ml extraction flask with the aid of several small portions of solvent. Section 5 Page 12 8. Evaporate the extract just to dryness with a gentle stream of dry filtered nitrogen and add 25 ml of 2.5% alcoholic potassium hy droxide. 9. Add a boiling chip, put a water condenser in place, and allow the solution to reflux for 45 minutes. 10. After cooling, transfer die solution to a 250 ml separatory funnel with the aid of 25 ml of distilled water. 11. Rinse the extraction flask with 25 ml of hexane and add it to the separatory funnel. 12. Stopper the separatory funnel and shake vig orously for at least 1 minute. Allow the layers to separate and transfer the lower aqueous phase to a second separatory funnel, 13. Extract the saponification solution with a second 25- ml portion of hexane. After the layers have separated, add die first hexane extract to the second separatory funnel and transfer the aqueous alcohol lay er to the original separatory funnel. 14. Repeat the extraction with a third 25-ml portion of hexane. Discard the saponifi cation solution and combine the hexane ex tracts. 15. carefully add 25 ml of the sulfuric acid solution (9:1 concentrated sulfuric acid/ water) to the hexane extracts. 16. Stopper die separatory funnel and shake vig orously for at least 1 minute. Allow the layers to separate and discard the lower aqueous acid layer. Repeat this step until the acid layer is colorless. 17. Wash the hexane with a 25- ml pordon of water. Discard the water wash. DSW 010246 i ) STLCOPCB4001699 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA 18. Filter the hexane extract through a 4" funnel plugged with glass wool which is covered with a layer of sodium sulfate into a Kunderna-Danish evaporative concentra tor. 19. Add a small boiling chip, put the Snyder column in place, and reduce the hexane volume to less than 5 ml by heating the apparatus in a 80-90*C water bath. Column Temper ature................. 160*C Detector Temper ature ................. 300*C Injection Port Temperature .. 195*C Pulse....................... 150 Flow Rates........... Helium Carriers 60 ml/min Argon-Methane Purge /\j 120 ml/min 20. After cooling, remove the 5-ml graduated tube and transfer the hexane extract to an Using EC/GC as the determinative step, inject alumina adsorption column, washing it in in duplicate 1-10 pi of each solution into the with several 5-ml portions of hexane. chromatograph. By comparison with standard so lutions injected, in duplicate, under the same op 21. Carefully add 100 ml of hexane to the col erating conditions, determine the amount and type umn reservoir and collect the total eluent of Aroclor using the individual or total peak 4 in either a 250-ml volumetric flask or a Kunderna-Danish evaporative concentrator. height method. 22. If the column eluent is collected in a volu metric flask, dilute to volume with hexane, and proceed with the gas chromatographic analysis, 23. If the column eluent is collected in a Kunderna-Danish evaporative concentrator, reduce solvent volume, cool, dilute to vol ume, and proceed with gas chromatographic analysis. The electron capture detector should also be used to guide the isolation procedures. Water and sedi ment extracts can be checked for the presence of PCB's and/or interferences by Injection pi portions of the extracts at various points in die extraction and concentration schemes. In this manner, it can be determined if the sample needs to be concentrated or diluted and if the clean-up procedures should be employed. H. Electron Capture Gas Chromatographic* 6 Procedure______________________________ I, Extraction The extraction of PCB's from water, employing Instrument........... F & M 402 Biomedical Gas Chromatograph Detector............... High Temperature Nl63 hexane as the extractant, has been found to be quantitative and sufficiently simple and rapid for use as a routine procedure. Electron Capture Cell 6 mm x 6' Glass Column, 4% XE-60 on 80/100 mesh The evaluation of this method was based on spik Chromosorb W, HP, AW-DMCS ing water samples with standard acetone solutions of I PCB's, The spiking method consisted of adding the (Continued) PCB's in acetone (25-50 pi) to 500 ml of tap water Section 5 Page 13 DSW 010247 STLCOPCB4001700 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OP NEMA in a 32-os narrow-neck screw cap jar.' After thorougly mixing the sample, duplicate 225-250 ml aliquots were taken and subjected to the proposed sample preparation and worked up as outlined. The results were quantified by preparing a calibration curve using standard hexane solutions of the PCB's used to spike die water samples. The major iso mer peak height was used to construct the calibra tion plot. The average recovery and deviation achieved substantiated the applicability of the method for the quantitative recovery and analysis of PCB's from water at the ppb-ppm level. No PCB recovery experiments from spiked sedi ment and soil samples have been performed. In stead, several of the residual solids representative of some of the types of sediment or soil analyzed were re-extracted with hexane/acetone (40/60) in a soxhlet extractor to test for the efficiency of the acetonitrile extraction step. The hexane, after iso lation by dilution with distilled water, was then carried through the purification steps. Recoveries by soxhlet extraction have indicated that the ace tonitrile extraction of PCB's was essentially quan titative in the cases checked. J. Sample Concentration Concentration of sample extracts is necessary, prior to clean up by chromatographic or chemical means, to reduce sample size and increase sensi tivity. The preferred method of concentrating al lows minimum loss through volatilization or chem ical decomposition and requires a minimum time. The three methods of solvent volume reduction most commonly used are evaporation by exposure to a stream of air, evaporation employing a Kundema- Danish evaporative concentrator equipped with a Snyder column, and evaporation under re duced pressure. All three techniques have been used, and no significant losses from volatilization or chemical alternation have been encountered. However, the Kunderna-Danish evaporative con centrator and the stream-of- air methods are easier to use. K. Column Adsorption Chromatography and Chemical Clean Up__________ Silica gel, Florisil and alumina deactivated with 0, 1.0, 1.5, 2.0 and 5 percent water were investigated as adsorbents for the elimination of interferences. Alumina (5% water) was found to be more effective and reproducible than either , silica gel or FlorisiL The activity of alumina varies with age and lot; therefore, 5% water is added to the alumina, after heating for a mini mum of 4 hours at 400*C, to insure a reproduc ible activity. Saponification and subsequent extraction of the sample with sulfuric acid is an effective way to remove a number of chlorinated hydrocarbon interI ferences as well as other matrix interferences. PCB's are not affected. L Column Performance Column performance is the key to effective gas chromatographic analysis and, as such, the choice of column materials is particularly im portant. Ideally, the support employed should be inert, mechanically strong, and of high surface area. For these reasons, Chromosorb W, HP, AW-DMCS is recommended for this work. A variety of polar and non-polar liquid phases have been investigated. The following columns have been found to provide adequate separation, etc., for use in PCB analysis by electron capture: 4% (W/W) DC-200, SF-96, OV-17, SE-30, SE-54, XE-60, Apiezon L, and 6% OF-1. DC-200 and XE-60 or QF-1 are the most suitable of these liquid phases. Another important consideration when working with an extremely sensitive detector and conse quently low levels of materials is column condi tioning. With polar phases such as XE-60 and QF-1, operating a new column overnight at a temperature 25-50*C higher than that to be used during analysis results in a more stable column. Section 5 Page 14 DSW 010248 ) STLCOPCB4001701 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OF A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA A no*flow conditioning technique ii employed to condition nort-polar columns. Hie column is purged with carrier gas, heated for 30 minutes at an el evated temperature without carrier flow and then cooled to room temperature. At the end of this cycle, die carrier flow is resumed and the condi tioning is completed as in the case of the polar liq uid phase. Two precautions: during conditioning, the column should not be connected to the detec tor, and one should not exceed the maximum safe temperature of the liquid phase. Two gas chromatographic systems have been used for PCB analysis--F & M Model 402 and 5750. Any system of Instrument and column suitable for chlorinated pesticides is satisfactory for PCB anal ysis. The use of the high temperature Ni63 elec tron capture cell is highly recommended. The ability to operate at higher temperatures prevents maintenance problems due to contamination from high boiling components. Glass columns should also be employed. M. Detection and Measurement Quantitative determinations employing the elec Since all liquid substrates bleed to one degree or tron capture detector are non-stoichiometric meas another and columns eventually degrade, all new urements made by comparing peak heights or areas columns should be characterized with two column for known concentrations with those for unknown performance indicators--the number of theoretical compositions. Except for sharp peaks, peak area / plates (N) and a tailing factor (T). p, p'-DDT measurements are usually more reproducible than is employed to check these parameters because it peak height measurements but are extremely time is known to degrade on "poor" columns. In this consuming unless a recording integrator is employed. manner, one can determine if the performance of a new column is satisfactory and when the column However, peak height measurements are as accu rate as disc integration of triangulation and, if the performance begins to fall off. A column is con peak shape represents a gaussian curve, the height sidered good if the number of theoretical plates per may be considered independent of the base. Con foot is on the order of 400-500 with tailing factors sequently, peak height measurements wer e gener of 1.0-1. 3. Calculation of these parameters is ally used. Three variations of the peak height shown in Fig. 5-2, page 8. Additionally, there quantification procedure were employed. should be no significant extraneous peaks upon in jection of a pure p,p'-DDT standard. Case I -- EC gas chromatogram of PCB un known unchanged with respect to Other chromatographic conditions that can be adjusted are column temperature and flow rates. standard PCB with no evidence of interferences. Although resolution of a mixture increases with de creasing temperature, a temperature should be Case II -- EC gas chromatogram of PCB un chosen that allows the elution of all components known altered with respect to stand within a convenient time period. The temperatures ard PCB with no evidence of inter given are optimum for 42% chlorinated biphenyl; ferences. temperatures are increased when specifically ana lyzing for the higher chlorinated biphenyls, i. e., 5470, 60%, etc. The flow rates shown are optimum Case III-- EC gas chromatogram of PCB un for a given instrument, column and detector system. known unchanged with respect to ( These should be adjusted if better results can be achieved. standard PCB with evidence of in terference. DSW Section 5 page 15 010249 STLCOPCB4001702 OFFICIAL STANDARDS PROPOSAL THIS OFFICIAL STANDARDS PROPOSAL IS AN OFFICIAL DRAFT OP A PROPOSED STANDARD DEVELOPED WITHIN NEMA, OR IN COOPERATION WITH OTHER INTERESTED ORGANIZATIONS, FOR CONSIDERATION BY ORGANIZATIONS OUTSIDE OF NEMA The amount of PCB'i in Case I samples is de termined by preparing a plot of the major peak height vetsus concentration. For Case II, a plot is prepared of the total sum of all major peala versus concentration. With Case III samples, a peak free from interference is used. When dom inant Interferences are present, one or more of the chemical clean-up procedures is employed. In all cases, the response of the electron capture detector must be linear for quantitative analysis. N, Contamination In determining PCB's in water, soil and sedi ment by electron capture gas chromatography, lab oratory sources of contamination can be a major problem. The samples and extracts should never be allowed to crime in contact with materials other than glass. Teflon or metal. Laboratory glassware should be thoroughly washed with hot, soapy water, rinsed with distilled water, acetone, and then hexane. All equipment should also be rinsed again with hexane just prior to use, and blanks should be frequently carried through all steps of the procedures to insure against die possibility of contamination. O. Sensitivity Two parts per billion. Absolute sensitivity--0.5 x 10"9 grams. Volume Injected--5 pL Final volume of extract*-5 mL Sample size--250 mL ) i Section 5 Page 16 DSM 010250 ) STLCOPCB4001703 AROCLOR 1016 H&P 402 Ni-63 EC 1/4" x 6' 4% XE-60 on 80/100 Chromosorb W HP Col. Temp. - 200C . inj. Temp. - 220C , Det. Temp. - 250C Carrier Gas - He 60 ml/min. Purge Gas - 10% CH^Argon 120 ml/min. Pulse Interval - 50 usee Amt. Injected - 5 yl Std. Cone. - 1 pg/ml. Range - 10 Attn. - 8 a t-'-t f.....-r 0 1 2 3 '4 56 ir 78 "T 9 MINUTES DSW 010251 Fig. 5-3 Section 5 Page 17 STLCOPCB4001704 < AROCLOR 1221 AROCLOR 1242 AROCLOR 1248 AROCLOR 1254 AROCLOR 1260 lI 'I 32 3<* 36 38 T <* a <.2 DSW 010252 STLCOPCB4001705 AROCIOR 1221 HSP 402 Ni-63 EC 1/4" x 6' 4% XE-60 on 80/100 Chromosorb W HP Col. Temp. - 170C Inj Temp. - 220C ' Det. Temp. - 250C Ccirrier Gas - He 60 ml/min. Purge Gas - 10% CH./Argon 120 ml/min. Pulse Interval - 50 ysec Amt. Injected - 5 yl _6 Std. Cone. - 1.48 x 10 g/ml Range - 10 Attn. - 4 4 % 40 30 20 DSW 010253 MINUTES r "r--t---------- 1 i . 6543210 Fig. 5-5 Section 5 Page 19 STLCOPCB4001706 ) AROCLOR 1242 H&P 402 Ni-63 EC 1/4" x 6' 4% XE-60 on 80/100 Chromosorb W HP Col. Temp. - 190C Inj* Temp. - 220C Det. Temp. - 250C Carrier Gas - He 60 ml/min. Purge Gas - 10% CH4/Argon 120 ml/min. Pulse Interval - 50 psec Amt. Injected - 5 pi Std. Cone. - 1.03 x 10" g/ml Range - 10 Attn. - 8 % 50 40 30 l0 20 4 10 t fi MINUTES i t *" i i | | 76543210 i Section 5 page 20 Fig* 5-6 > DSW 010254 STLCOPCB4001707 AROCLOR 1248 H&P 402 Ni-63 EC 1/4" x 6' 4% XE-60 on 80/100 Chromosorb W HP Col. Temp. - 190C Inj. Temp. - 220C ' Det. Temp. - 250C Carrier Gas - He 60 ml/min. Purge Gas - 10% CH,}/Argon 120 ml/min. Pulse Interval - 50 ysec Amt. Injected - 5 ul Std. Cone. - 1.31 x 10-6 g/ml Range - 10 Attn. - 4 10 (1 % 50 " i ..... ...... i........ i 13 12 11 MINUTES 10 i " >1 98 T --1 1 "t 7 65 Fig. 5-7 ' ' I1 I 43210 Section 5 page 21 DSW 010255 STLCOPCB4001708 AROCLOR 1254 H&P 402 Ni-63 EC 1/4" x 6' 4% XE-60 on 80/100 Chromosorb W HP Col. Temp. - 205C . Inj. Temp. - 220C . Det. Temp. - 250C Carrier Gas - He 60 ml/min. Purge Gas - 10% CH^Argon 120 ml/min, Pulse Interval - 50 ysec Amt. Injected - 5 yl Std. Cone. - 1.02 x 10"6 g/ml Range - 10 Attn. - 8 % 40 - 30 12 11 MINUTES 10 Section 5 Page 22 6543210 Fig. 5-8 OSW 010256 STLCOPCB4001709 AROCLOR 1260 H&P 402 Ni-63 EC 1/4" x 6' 4% XE-60 on 80/100 Chromosorb W HP Col. Temp. - 220C . Inj. Temp. - 220C .. Det. Temp. - 250C Carrier Gas - He 60 ml/min. Purge Gas - 10% CHs/Argon 120 ml/min. Pulse Interval - 50 usee Amt. Injected - 5 pi Std. Cone. - 0.98 x 10"6 g/ml Range - 10 i l i 1------------ r-.' --t r--,, 12 11 10 9 8 7 6 5 MINUTES 4 3 2 10 ' Fig. 5-9 Section 5 Page 23 DSW 010257 STLCOPCB4001710 NATIONAL MEMBER COMPANIES OF THE ELECTRICAL MANUFACTURERS ASSOCIATION Allit-Chalmers Manufacturing Co. t Milwaukee, Wis. 53201 Central Moloney Transformer Division T Colt Industries - Pine Bluff, Ark. 71601 ' Chance, A. B., Co. t Transformer Division Washington, Mo. 63090 Dovzer Electric Inc. t (Division of Sola Basic Industries) Mount Vernon, HI. 62864 Esco Manufacturing Co. t Greenville, Tex. 75401 Federal Pacific Electric Co. New Bedford, Mass. 02744 * Newark, N. J. 07101 f General Electric Co. Hudson Falls, N.Y. 12839 * Pittsfield, Mass. 01201 t Hevi-Duty Electric T (Division of Sola Basic Industries) Goldsboro, N. C. 27530 High Voltage Power Corp. t Westboro, Mass. 01581 I-T-E Imperial Corp. t Philadelphia, Pa. 19130 Kuhlman Electric Co., A Division of t Kuhlman Corp. Birmingham, Mich. 48012 Magnetics Inc, T Sandy Lake, Pa. 16145 McGraw-Edison Power Systems Division So. Milwaukee, Wis, 63172 * Canonsburg, Pa, 15317 f * Member of Capacitor Section, t Member of Transformer Section. Niagara Transformer Corp. t Buffalo, N. Y. 14225 Northern Engineering Division t Sta-rite Industries Inc. Baraboo, Wis. 53913 Sangamo Electric Co. * Springfield. I1L 62708 Sierra Transformer Co., t Cerritos, Calif. 90701 Sorgel Electric Corp. t Subsidiary of Square D Co. Milwaukee, Wis. 53204 Spokane Transformer Co. T Spokane, Wash. 99202 Sprague Electric Co. * North Adams, Mass. 01247 Standard Transformer Co., Division of f American Gage and Machine Co. Warren, Ohio 44481 Tierney Electrical Manufacturing Co. t Seattle, Wash. 98108 Uptegraff, R. E., Manufacturing Co. t Scottdale, Pa. 15683 Wagner Electric Corp. T St. Louis, Mo. 63133 Westinghouse Electric Corp. Bloomington. Ind. 47402 * Sharon, Pa. 16146 T Zinsco Electrical Products t St. Louis, Mo. 63113 DSW 010258 Printed in U. S. A. ) STLCOPCB4001711