Document JvRZmo9Z6ynDnMdN3bveMp4yZ
ANSI C107.M974
American National Standard
guidelines for i handling and disposal of cap acitor- and transformer-grade askarels
containing polychlorinated biphenyls
I
C107.1-1974
ANSI C107.1-1974
American National Standard Guidelines for Handling and Disposal of Capacitor- and Transformer-Grade Askarels
Containing Polychlorinated Biphenyls
Secretariat
National Electrical Manufacturer Association
Approved January 9,1974
American National Standards Institute, Inc
NtV 0 2 4 5 3 3
734588
America! National Standar
An American National Standard implies a consensus of those substantially concerned with its scope and provisions. An American National Standard is intended as a guide to aid the manu facturer, the consumer, and the general public. The existence of an American National Stan dard does not in any respect preclude anyone, whether he has approved the standard or not, from manufacturing, marketing, purchasing, or using products, processes, or procedures not conforming to the standard. American National Standards are subject to periodic review and users are cautioned to obtain the latest editions.
CAUTION NOTICE: This American National Standard may be revised or withdrawn at any time. The procedures of the American National Standards institute require that action be taken to reaffirm, revise, or withdraw this standard no later than five years from the date of publication. Purchasers of American National Standards may receive current information on all standards by calling or writing die American National Standards Institute.
I
\ \
Published by
American Nations! Standards Institute 1430 Broadway, New York, New York 10018
rapyright > 1974 by American National Standards Institute, Inc Jdl rights reserved.
h o part of this publication may be reproduced In any. form, li^ an electronic retrieval eyetem or otherwbe, without the prior written permbalon o f the publisher. Printed in the United States of America
A1M1074/6
NfcV 0 2 4 5 3 *
734589
Foreword (Thl Foreword it not part o f American National Standard Guidelines for Handling and Disposal o f Capacitor-1 nd Transformer-Grade Askarels Containing Polychlorinated Biphenyls, C107.1-1974.)
Recognizing that the polychlorinated biphenyls present in askarels were being identified as envi ronmental pollutants and the urgent need for procedures and guides for their safe use and dis posal, the Board of Directors of the Power Equipment Division of the National Electrical Manu facturers Association (NEMA) in June 1970 appointed a committee to review the general problem and propose recommendations. In September 1970, the NEMA board approved, as recommended by the committee, the sponsorship of an American National Standards Commit tee for the use and disposal of askarels in electrical equipment.
American National Standards Committee C l07 was established in April 1971. NEMA was desig nated as the secretariat. An organizational meeting was held on September 14, 1971. Mr W. B. Papageorge, Monsanto Company, was appointed chairman. Committee members included repre sentatives of capacitor and transformer manufacturers, utilities, governmental departments and agencies, and maintenance and disposal service companies. A steering committee and two sub committees - one to develop guidelines for the capacitor industry, the other for the transfor mer industry - were established.
The scjope and primary objective of the committee was designated as the development of: Pro cedure^ and guides for the safe use, maintenance, and disposal of askarel and askarel-soaked materifds used in electrical equipment.
Additional objectives proposed were as follows: (1) To serve as a source for technical information and advice for federal, state, and local
authorities and for the information of all others concerned. (2) To encourage the development of suitable disposal facilities and maintain a list of their
capabilities and locations, for the information of all concerned. (3) serve as the advisory group for U.S. participation in the International Commission on
Rules for the Approval of Electrical Equipment (CEE), the Internationa) Electrotechnical Com mission (I EC), the Pan American Standards Commission (COPANT), the International Confer ence on Large High Tension Electric Systems (CIGRE), and other international organizations.
The flnaj draft of the guidelines was completed in late November 1972. NEMA issued the guide lines as ijn Official Standards Proposal in January 1973. It was submitted to the American Nations^ Standards Institute for approval as an American National Standard and was approved by the Standards Institute on January 9,1974.
Suggestions for improvement of this standard will be welcome. They should be sent to the American National Standards Institute, 1430 Broadway, New York,N.Y. 10018.
This stan lard was processed and approved for submittal to ANSI by American National Stan dards Committee on Use and Disposal of Askarel and Askarel-Soaked Materials in Electrical Equipme: it, C l07. Committee approval of the standard does not necessarily imply that all com mittee m< mbers voted for its approval. At the time it approved this standard, the Cl 07 Com mittee ha I the following members:
W. P. Papi george, Chairman A. M. Salazar, Secretary
Organization Represented
Name o f Representative
Certified Ballast Manufacturers A sso cia tio n .......................................................................... N. R. Clark A. Pozefsky
Chem-Tro! pollution Services I n c .......................... ............................................. ...
Louis E. Wagner
Doble Engineering Com pany.................................... ............................................................. A. L. Rickley
Electrical Utilities C om p an y............................. .........................................................................A. O. Hauser
I E. M. Moore (Alt)
Electric Light and Power G rou p .................................................................................................F . R. Lengefeld
H. A. Onishi
J. J. Cawley (Alt)
734590
NEV 024535
Or \antiation Represented Electronic Industries Association Environmental Protection Agency. General Services Adm inistration. Gilbert Associates Inc lm tltute o f Electrical and Electronics Engineers, Inc M<ntanto Com pany.
National Bureau o f S tan d ard s.......................... National Electrical Manufacturers Association
Rollins-Purle, Inc ................................................................................................ Tennessee Valley A u th o r ity ............................................................................. U S. Department o f Agriculture, Rural Electrification Administration . U S . Department o f the A rm y ..........................................................................
Name o f Representative
Arnold S. Doty Kenneth J. Hood Charles C. Travis R. J. Schatz E. L. Rabb W. P. Papageorge P. G. Benignut (Alt) Stanley P. Wasik K. C. Chang W. S. Grogan R. D. McClain H. R. Rowe Ken McGee (Alt) H. A. Alsentzer William R. Nicholas John Leutritz, Jr D. M. Crabtree
NEV 02453b
734591
Contents
SECTION
1. Scope
2. General Information......................................
2.1 G eneral.................................................. 2.2 Benefits.................................................. 2.3 Risks. . . ................................................ 2.4 Alternatives........................................... 2.5 Interdepartmental Task Force on PCBs
3. Capacitor G uidelines........................................ 3.1 General ....................................................... 3.2 Capacitor-Grade Askarel......................... 3.3 Plant Housekeeping and Employee Safety 3.4 Control of Water E fflu en ts.................... .. 3.5 Scrap-Disposal Procedures......................... 3.6 Labeling.....................................................
4. Transformer Guidelines.................... .............. 4.1 G eneral.................... ................................ 4.2 Specific Guidelines...................................
5. References.........................
5.1 R eferences to the T ext
5.2 General References . .
6. Revision of American National Standards Referred to in This Document
Table 1 Typical Properties of Arocior 1 0 1 6 ....................................................
Appendixes Appendix A Disposal Services......................................................................
Appendix B Analytical Procedures and Laboratory Service Organizations B l. G eneral............................................................................................... B2. Laboratories....................................................................................... B3. An Analytical Procedure for the Determination of Airborne PCBs. B4. Analysis of Water and Sediment for PCBs........................................
Figures Fig. Bl Arocior 1016 Electron Capture Chromatogram . . . Fig. B2 Comparison of Electron Capture Chromatograms for Arocior 1221, 1242, 1248, 1254, and 1 2 6 0 . . . . . . Fig. B3 Arocior 1221 Electron Capture Chromatogram.. . . Fig. B4 Arocior 1242 Electron Capture Chromatogram. . . . Fig. B5 Arocior 1248 Electron Capture Chromatogram.. . . Fig. B6 Arocior 1254 Electron Capture Chromatogram. . . . Fig. B7 Arocior 1260 Electron Capture Chromatogram.. . . Fig. B8 Sampling Train.......... ................................................. Fig. B9 Calculating Column E fficiency................................. Fig. B10 Calculating the Tailing F acto r...................................
7
7 7 7 7 8 8
8 8
9 9
11 12 13
13 13 15
17 17 17
18
9
19
20 20 20 20 31
21
22 23 24 25 26 27
American National Standard Guidelines for Handling and Disposal of Capacitor- and Transformer-Grade Askarels Containing Polychlorinated Biphenyls
I. Scope
This standard establishes guidelines for the safe use, maintenance and disposal of askarel and askarel-soaked materia] used in capacitors and transformers.
2. General Inform ation
2.1 General. The term "askarel" generally describes a broad class of nonflammable synthetic chlorinated hydrocarbon insulating liquids widely used in capaci tors, transformers, reactors, and accessory equipment operated at pow m frequencies.
Askarels consisting of or containing polychlorinated biphenyls (PCBt) have been used in many applications for more than 40 years, but only recently was evidence discovered that PCBs are widely dispersed in the envi ronment. Systematic investigations of the biological effects of PCBs have been undertaken within the past few years to establish the effects of specific formula tions upon specific species. Some studies have shown that PCBs may be an environmental contaminant. Simultaneously, significant steps have been taken by U.S. industry lo limit further releases of PCBs to the environment.
PCBs have >een used in three broad types of applica tions for the past 40 years, as follows:
(1) "Opeiyendcd" applications; for example, in paints, special ty inks, paper coatings, plastics, etc
(2) "Nom inally closed" applications; for example, as the working fluid in hydraulic or heat-transfer sys tems I
(3) *'C!os id electrical system" applications, specifi cally as the insulating fluid in certain kinds of trans formers and capacitors1
1The Monsanto Compsny Is the sole U.S, producer o f PCBs. It hat discontinu ed supplying the materiel for all applications given in 2.1(1) and 2.1(2).
Evaluations of the benefits, risks, and alternatives Involved in the continued use of PCBs in closed electri cal systems are summarized in 2.2 through 2.4.
2.2 Benefits. Askarel-fllled transformers do not burn or sustain fire under conditions of internal electrical arcing.
Askarel-fllled power and industrial capacitors are significantly smaller, more reliable, more durable, and safer than oil-filled capacitors. As a result, askarels have supplanted mineral oils in more than 90% 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 advan tage of the size, safety, and reliability benefits of askarel capacitors (for example, many types are today less than 14% of the size of equivalent oil capacitors and have a life expectancy of 10 to more than 20 years).
Various federal, state, and local codes, therefore, re quire their continued use in or adjacent to public, com mercial, and industrial buildings, which locations pre sent the greatest potential danger to life and property.
2.3 Risks. In the United States, medical records over a nearly 40-year period show that the only adverse health effects experienced by U.S. workers exposed to askarels, either during the manufacture of these liquids or of electrical equipment containing these liquids, have been limited to occasional cases of nonchronic chioracne or other temporary skin lesions or irritations.
Askarel-fllled transformers and capacitors are de livered to customers as sealed units from which there Is no escape of askarel under normal operation. Although certain types of equipment failures can permit loss of some askarei to the environment, transformer failures are limited to approximately 0.02% of the units in ser vice per year. With respect to capacitors, such tosses are limited to approximately 0.02% of the askarel put into service per year. In addition, limited amounts of PCBs can get into the environment during the manufac ture, delivery, improper use, maintenance, repair, and disposal of transformers and capacitors.
NEV Q2453S
7
734593
AMERICAN NATIONA L STANDARD C I 0 7 .1-1974
Specific controt measures have been instituted by individual manufacturers and are supplemented and strengthened by national standards and procedures such 8S this standard, which provides information to prevent the inadvertent loss of PCBs to the environ ment at all stages from initial askarel manufacture through ultimate dh posai.
2.4 Alternatives. For technical and local and national code reasons, it would be impossible to replace most askaret-Olled transformers now in service with oil-filled units of equivalent i atings without major construction changes that would >e required to compensate for the fire resistance of (he askarel-fllted units. For certain applications and loc liions, dry-type transformers may replace askarel-flllec transformers.
For new installations, although many of the fore going limitations would still apply, building and instal lation design provisions could be made to accommo date the use of oil-fi led, open dry-type, or sealed drytype transformers, provided that necessary technical, code, physical size, ind cost considerations are prop erly evaluated.
The principal alternative to askarels for capacitors is mineral oil, but such replacement would return capac itor technology to its pre-1932 level and would necessi tate the redesign and replacement of such widely used equipment as fluorescent light fixhires and racks for power and inductioji-heating capacitors, which could not now accommodate the increased size of oil capaci tors while maintaining their present ratings.
The cost of askafel liquids is about five to ten times more than mineral oil. Thus, long before there were any environmental concerns about PCBs, there was a strong economic Incentive to find other, less expensive insulating liquids w^th the desirable characteristics of askarels. Since the 1930s at least ten major chemical or electrical companies have invested large amounts of time and money In this search, all with no success. Al though potential substitutes that are more costly than askarels (such as fluprinated liquids) have also received some consideration! little is known about either their electrical performance or possible 01 effects upon the environment. There are today no fluids that can be used as a direct replacement for askarels.
2.5 Interdepartmental Task Force on PCBs. An indepth study of PCBs has recently been completed by five Executive Branch Departments of the federal gov ernment. This Interdepartmental Task Force on PCBs issued their report, entitled Polychlorinated Biphenyls and the Environme it, in May 1972.2 The following
*Available from the atlonal Technical Information Service, U.S. Department of Commerce, Springfield, Va 22151.
conclusion is quoted from page 4 of this report: "TTie use of PCBs 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 PCBs 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 PCBs to all except manufacturers of electrical transformers and capacitors.'*
Reference should be made to the Interdepartmental Task Force Report for additional information and con clusions.
3. Capacitor Guidelines
3.1 General. The environmental effects of askarels are under in-depth study by governmental and other agen cies. Askarels have been considered relatively harmless to humans based on about 40 years of safe industrial usage. There has been no known instance of human in jury when they were used under the normally accepted precautions and conditions of handling in both manu facturing and user applications.
Traces of askarels are being found in the environ ment and in fish and bird life. The long-term genetic and ecological effects are not yet completely under stood. For these reasons, care should be taken to con tain askarels and minimize their entry into the environ ment.
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 de gree of nonflammability, they are used in transformers where personnel safety is of paramount importance.
Capacitor-grade askarel has a lower degree of chlori nation (composed primarily of the 3-chlorine isomers of biphenyl) and a higher degree of biodegradability. Generally, it has not been found in animal life. It is used in capacitors, where the extreme degree of non flammability required in transformers is of less impor tance.
Although capacitor- and transformer-grade askarels both contain members of the PCB family, they do differ in composition, degree of biodegradability, persistence in nature, electrical stability, chemical stability, and degree of nonflammability (both are recognized as non flammable). It is for these reasons that Section 3 of this standard is intended to apply to capacitor-grade askarel.
8
734594
NEV 044539
AMERICAN NATIONAL STANDARD C 107.I-1974
Table! Typical Properties of Afoclor 1016
Property
Color Condition Specific Gravity at 25/ 5.5 C Acidity (mg KOIl/g)
Moisture Refractive index at 25C Inorganic (free) chlorld it Pour point Dielectric constant ( 1 0 (0 Hz at 100C) Reslittvity (500 V dc at I10 0 c , 0.1-lnch gap) Hydrolysis stability test (as chlorides) Thermal stability test (a i chlorides) Distillation range (corrected)
10% distilled by weight 90% distilled by weight Higher-Boiling Homologues Sulfates Dielectric strength at 2$C Flash point* Cleveland o >en cup Fire point Corrosion test (6 hours st 210C with bright aluminum foil) ichange in weight o f aluminum Viscosity at 1 0 0 F (S U S if Specific heat at 25C Coefficient of expansion Fixed chlorine Power factor al 100CV6|) Ht Bulk Drums
Teit Method (See Note) APHA*
ANSI C59.68-1965 (R 1 9 7 3 )|2 ) ANSI Z l l . 131*1964 (R1974) (3) ANSI Z I.59-1958 (R 1971)(4)
ASTMD 1817-66(1972) 15] ANSI C59.55-1963 (R 1973) (6) ANSI 211.5-1966 (R1972) [7] ANSI C 59.2M 967 (R I973) (8) ANSI C59.51-1965 (R1973) (9) ANSI CS9.106-1970 ( 10] A N SIC 59.il 1-1970(111 ANSI A37.9-1974 (12)
ASTMD 3303-74 (1) ANSI C59.2-1974 (13) ANSI C 59.19*1968 (R1973) (14) ANSI 211.6-1973 (15)
ANSI ZI 1.2-1956 (R1971) (16)
ANSI C59.57-1963 (R1973) (17) Carhis Munch (18)
Typical Values 40, max Clear 1.362-1.372 0.010, max
35 ppm, max 1.6215-1.6235 0.05 ppm, max -14C or lower 4.70-4.90 5 0 0 X 10* O cm, min 0.5 ppm, max 0.4 ppm, max
323C, min 356C, max 0.4%, max None 35 kV, min 338F, min None to boiling point
0.0%
71-81 0.30 0.00068 cm , /cm f /C 41.3 i 0.5%
1%, max 4%, max
NOTE: Numbers in brackets refer to correspondingly numbered test m ethods in 5.1, References to the Text. ` American Public Health Association. fSaybolt Universal seconds.
3.2 CapsciforGrade Askarel. In September 1971 a new grade of capacitor imprgnant, Aroclor 1016, was made available to the Industry. This new grade contains a typical concentration of 0.4^6 by weight of the higher boiling homologues o f the chlorinated biphenyls. (See ASTM D 3303-74 [1] .)* Arotjlor 1016 replaces Aroclor 1242 which previously was the major capacitor imprg nant and contained around 7% of the higher-boiling homologues (th more persistant in nature). This 0.4% level of the higher-boiling hon o<logues should be the
` Numbers in b rick ed refer to corresponding numbers in 5.1 References to the Text.
maximum concentration acceptable in any capacitor imprgnant. Aroclor 1242 and 1254, previously used as imprgnants, 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 Underwriters* Labora tories, Inc, nonflammability rating as Aroclor 1242. Its typical properties are given in Table 1.
3.3 Plant Housekeeping and Employee Safety. The procedures and limits given in 3.3 are intended to be minimum requirements to be met by manufacturers and users of capacitors containing askarel. Handling, control, and disposal procedures are given, together
NEV 024540
9
734595
AMERICAN NATIONAL STANDARD C 1 0 7 .M 9 7 4
with exposure llml|s and indicated antidotes and clean contained in Section B3 of Appendix B. This procedure
up procedures.
or its equivalent should be used.
3.3.1 Material. Askarel for use in capacitors should
Breathing vapor or fumes from heated askarel should
consist of homologues and isomers of chlorinated bi
be avoided. Provisions should be made for adequate ven
phenyl with the concentration of thejiigher-boiling
tilation and regulation of manufacturing operations to
homologues at abo it 0.4%. (See STM D 3303-74 [1].) avoid open exposure to askarel (especially at tempera
Aroclor 1016 Is considered to be the standard imprg
tures of 55C or higher). The gases produced when aska
nant meeting these jrequirements.
rel is decomposed by very high temperatures (such as
Commonly useti solvents include benzene, kerosene, that of an electric arc) in the presence of air or organic
acetone, trichloroe hane, trichloroethylene, and perchlo- insulating materials contain a high percentage of hydro
roethylene. Typical vapor pressure data for Aroclor
gen chloride, and small percentages of carbon dioxide,
1016 are:
carbon monoxide, and oxygen. Minute concentrations
0C 0.001 mmHg
of this combination of gases are very unpleasant and ir
25C 0.006 mmHg
ritating, thus giving ample warning of their presence. If
150C * 4.3 mmHg
exposure to high concentrations of askarel is necessary
200C - 29.0 mmHg
under emergency conditions, an approved gas mask or
At 25C and 760 mmHg pressure, saturated air con self-contained breathing apparatus should be worn.
tains approximately 0.09 mg/1.
Such exposure should be under the surveillance of
NOTE: 1 mg/1 90.0 ppm (v/v) 1 ppm (v /v ) 0.011 mg/1
other personnel capable of effecting rescue in case of an accident. If the odor of askarel is detected by the person wearing protective equipment, he should imme
diately go into fresh air. All gas masks, respirators, and
3.3.2 Bulk Fluid Shipment, Receiving, and Transfer. Shipment of askare 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. Containers should be labeled as to con tents and carry a lapel 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 completely cleaned of all traces of askarel. (Cleaning procedures must take cogni zance of precautions against excessive exposure and of the need for proper disposal of contaminated cleansing solvents and materials as set forth in 3.5). Transfer from shipping containers to processing systems should be through closed piping or tubing with appropriate valves, pumps, etc. Provision should be made for trap ping and disposing i f fluid lost by leakage or spills from the transfer system and from the storage containers.
Drums to be retired from use should be cleaned be fore crushing, delivery to scrap dealers, or other dispo sal. Contaminated cleaning fluids and materials should be disposed of as indicated in 3.5.
3.3.3 General Safety Precautions. Although it is generally accepted tnat exposure to capacitor-grade askarel is not hazardous provided that simple precau tions are taken, exposure should still be avoided.
replacement parts should have U.S. Bureau of Mines
approval and be maintained on a regular schedule in
accordance with the manufacturer's recommendation.
3.3.3.2
Liquid. In contrast to the situation in
which mineral insulating oils are handled, there is vir
tually no fire hazard in handling askarel. A limited sol
vent 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 insu
lating oil, some people are allergic to askarel, and con
tinued 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 protec
tion is recommended. The use of porous gloves that
can absorb and retain askarels is to be avoided. Barrier
creams4 or resistant gloves9 should be used if contact
is unavoidable. Use of enclosed transfer and handling
equipment, processing equipment, and mechanical
washers reduces direct contact.
Medicinal washes or mild detergents followed by the
application of cold cream will reduce the irritation re
sulting 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 aska-*1
3.3.3.1
Vapors. The odor of askarel is noticeable
well below the maximum air concentrations considered safe. Up to 1.0 milligram per cubic metre of air has been determined to be the maximum safe level of expo
4 For example, PLY No. 9 Gel (Milburn Company, Detroit, Mich), or Kerodex No. 71 (Ayerit Laboratories, New York, N.Y.), or the equivalent.
sure during an 8-hour workday. (See reference [19].)
1 For example, Edmont - Solvit 5-352 (Menlck o f Bridgeport,
The procedure for performing the necess8iy analyses is
Bridgeport, Conn), or the equivalent.
10 NV 0 2 4 5 4 1
734596
AMERICAN NATIONAL STANDARD C 1 0 7 .1-1974
rel contacts the eyes, the <yes should be irrigated imme diately 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 irritation.)
Persons developing a skin irritation or respiratory tract irritation while working with askarels should be placed under the supervision of a physician.
Ingestion or swallowing of askarels is not generally regarded as a problem of the industry. Should acciden tal ingestion occur, a physician should be consulted. Hands should be washed with warm water and soap be fore eating, drinking, smojdng, or using toilet facilities.
3.3.4 Manufacturing Housekeeping. Manufacturing equipment and operating procedures should safeguard against loss of askarels to |he environment through proper containment and disposal procedures.
Enclosed systems of sealed piping, properly gasketed joints, valves, containers, and processing chambers should be used for any portion of the operation where askarel temperatures may exceed 55C. 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 un controlled conditions or events.
Spills of askarel should be removed promptly by means of absorptive matei ial, such as sawdust, or trapped and removed by pumping or other suitable means.
Waste fluids containing askarel not suitable for recon ditioning or reuse should be collected (by means of traps, drip pans, trays, etcj from the various parts of the manufacturing and processing area (including washers or other cleaning devices). Disposal should be made in accordance with 3.5.
Wiper rags, clothing, ar d other extraneous materials saturated with askarels should be collected within the containment area for properly controlled laundering or disposal (see 3.5).
3.3.5 Disposal of Askirel Wastes. Methods for dis posal of liquids and saturited solids generated by the manufacturing operation ihould be in accordance with those outlined in 3.5, and should include (but not be limited to) the following wastes:
(1) Contaminated liquid askarel that is unsuitable for reclaiming as a dielect ic fluid
(2) Liquid askarel from solvent operations or water and detergent type washers
(3) Saturated earth or other absorbent media from filtering operations
(4) Saturated sawdust or other absorptive materials from spills
(5) Saturated filters fr :>m 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 3.3.6 Miscellaneous Procedures. Other safety con
siderations include the following: (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 purpose within the containment area, and later dis posed 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 designated for disposal must be controlled and handled in accor dance with the intent of the procedures given in 3.3.6(1) and 3.3.6(2), finally being disposed of by one of the means outlined in 3.5.
3.4 Control of Water Effluents. The industry goal is to eliminate askarel in plant water effluent streams. How ever, it is recognized that existing drain systems in capacitor manufacturing plants are probably contami nated 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 standard provide that no askarel wastes of any kind be disposed of in any water effluent streamsand that accidental spills be prevented from getting into such streams.
3.4.1 Concentration Limits. The 1972 Environmen tal Protection Agency proposals are to keep PCB levels in rivers and lakes below 0.01 part per billion. This is currently under review by the EPA and standards are expected to be promulgated in 1974. Plant effluent streams should be managed and controlled in a manner anticipating these government standards.
3.4.2 Monitoring Streams. On a regular basis con sistent with plant situations, all effluent streams should be analyzed. The procedure for performing the neces sary analyses is contained in Section B4 of Appendix B. This procedure or its equivalent should be used.
3.4.3 Methods for Minimizing Effluent Stream Con tamination. The ideal approach is to isolate totally all effluent streams that could be contaminated with aska rels during manufacturing processes and prevent them from being discharged from the plant. Carbon adsorp tion, limestone beds, and solvent extraction are tech-
734597
NEV 02<*5<*2
II
AMERICAN NATK >NAL STANDARD C 107.1-1974
nlques (hat can be applied to reduce the askarel content of effluent streams. These techniques may be most use ful in cleaning upwraater used in plant processing and to permit recycling.
3.5 Scrap-Disposi 1Procedures. Tire manufacture and
use of capacitors involve processes that produce askarel-
saturated solids ar d liquids containing or composed en
tirely of askarel, which should be disposed of as wastes.
Specific sources o ' these materials are described through
out this standard. They may be placed into three cate
gories;
(1) Capacitor i nits impregnated with askarel, pro
duction and field rejects
(2) Manufacturing process liquid wastes containing
askarel
(3) Solid waste purposely or accidently saturated
with askarel
|
Disposal should be done in a manner that is consis
tent with proper concern for the environment and
minimizes any release of askarels to the environment.
3.5.1 Disposal >f Capacitor Units. Scrap capacitor
units can be genen ted during manufacturing processes
or during field service.
Production rejects are those capacitors that are re
jected after the impregnation process in the course of
production by the tapacilor manufacturer. They may
be rejected for mechanical or electrical reasons, or be
cause of obsolescence.
Field rejects are those units that are rejected or, for
other reasons, are to be scrapped after shipment from
the plant where th^y were manufactured.
3.5.1.1 Production Rejects. Rejected capacitors
in capacitor manufacturing plants represent a concen
tration of askarel. It is important that their disposition
be made in a manner consistent with proper concern
for the environment. Therefore, capacitors should be
disposed of only in supervised dry landfill sites that
meet all applicable state requirements.
Care should be exercised to ensure that no loss of
liquid will 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.
3.5.1.2 Field(Rejects. Small capacitors (defined
as containing less than 2 pounds of askarel) are practi
cally always used as components in other electrical or
electromechanical equipment. Typical examples of
large quantity usag of such capacitors are in fluores
cent lamp ballasts and residential air conditioning equip
ment. Failure of suh capacitors may result in scrap
ping of the device oi which it is a part (as in a fluores-
cent ballast) or replacement and scrapping of the indi vidual capacitor (as in a room air conditioner). How
ever, 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, through out the world. Fortunately, the nature of the devices and equipment in which such capacitors are used is such that they are 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 impregnating small capacitors be limited to the recently introduced type, which contains a typical concentration of 0.4% of the higher-boiling homologues. (See ASTM D 3303-74 11J .)
Large capacitors (those incorporating more than 2 pounds of askarel) should be disposed of according to the procedure for production rejects (see 3.5.1.1).
3.5.2 Disposal of Liquid Wastes. All waste askarel or liquid wastes containing askarel should be disposed of in accordance with one of the procedures given in 3.5.2.1 through 3.5.2.3.
3.5.2.1 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 scrubbers to remove the HC1 that will be formed; for example, 2-second dwell time at 2000F and 3% excess oxygen in stack gas, or 1.5-second dwell time at 2700F and 2% excess oxygen in stack gas.
These facilities should meet the applicable require ments of the state in which they are located, and should control effluents within the limits set forth in this standard.
3.5.2.2 Toxic and Hazardous Waste Disposal Sites. Certain landfill sites have been classified by state governments and the federal government as suitable for the disposal of toxic and hazardous liquids. Where such approved sites exist, they may be used for the disposal of liquid wastes described in this standard. (See Appen dix A.)
3.5.2.3 Packaging and Shipment 3.5.2.3.1 Transportation to the disposal facili
ty should be in containers that will prevent leakage and accidental loss of askarel to the environment.
3.5.2.3.2 Containers should be labeled as to contents and precautions relative to loss to the environ ment.
3.5.2.3.3 Containers used for this purpose should not be used for any such materials or retired from service until they are completely cleaned. Any
12 NfcV 734598
v
AMERICAN NATIONAL STANDARD C 1 0 7 .1-1974
solvents used in cleaning these containers will be conlaminated with askarei ant should be disposed of according to the same procet ures described in 3.5.2.
3.5.3 Disposal of Solid Wastes. (See 3.5.1 for scrap capacitors.) All solid wastes that have been saturated with askarei should be disposed of by the following procedure:
(1) The saturated wastes should be placed into leakproof containers and transported to a supervised dry landfill site meeting stite requirements. Alterna tively, they can be disposed of by incineration in state-approved facilities.
(2) Solid absorbents used for spills can be disposed of uncontained in the supervised dry landfill site; trans port to the site should be in closed containers. Alterna tively, incineration can be used in accordance with 3.5.2. (See Appendix A for a listing of facilities.)
3.6 Labeling. Capacitor uiits 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 road way 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.
For the foregoing reasons the methods of providing disposal instructions for s nail capacitors and large ca pacitors are treated separs tely in 3.6.1 and 3.6.2,
respectively. 3.6.1 Small Units. Sm ill capacitors are defined as
those that contain askarel^in quantities up to about 2 pounds each and in which the free liquid does not ex ceed 0.4 pound. They are hermetically sealed in metal lic cases. Such capacitors are applied as a component of a large piece of equipment. Attaching a label to such equipment referencing th s standard or describing dis posal procedures would bs of limited practical value.
3.6.2 Large Units. Larae capacitor units are defined as those that contain mors than 2 pounds of askarei. Hie capacitor manufacturer should affix a label in a conspicuous place, referencing this standard or de scribing disposal procedu es consistent with it. This label should contain, as a minimum, the following Infor mation:
CAUTION: This capadtor contains a polychlori nated biphenyl (PCB). Tc avoid possible environmental contamination, it should t>e disposed of only in super vised dry landfill areas moeting state requirements or in incineration facilities designed for disposal of FCBs. See American National S andard CJ07.1-I974 for fur ther information. Copies ire available from American National Standards Institute, 1430 Broadway, New York. N.Y. 10018.
4. Transformer Guidelines
4.1 General
4.1.1 Types of Transformer Askarels.* Askarels of
various compositional types are currently in use (for
the general properties and types, see ASTM D 2283-
73a (20]). Under arcing conditions, the gases produced,
though predominantly consisting of noncombustible
hydrogen chloride, can contain varying amounts of
combustible gases depending upon the askarei type.
4.1.2 Safety Precautions. Based on about 40 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 expo
sure to askarels is not hazardous provided that simple
precautions are taken, exposure should still be avoided
or minimized.
4.1.2.1
Vapors. The odor of askarei is noticeable
well below the maximum safe air concentrations. De
pending upon the composition of the askarei used,
from 0.5 to 1.0 milligram per cubic metre of air has
been determined to be the upper safe level of expo
sure during an 8-hour workday. (See reference (19].)
The procedure for performing the necessary analyses
is contained in Section B3 of Appendix B. This proce
dure or its equivalent should be used.
Breathing vapor or fumes from heated askarels
slioutd be avoided. High concentrations of vapors can
cause irritation of the eyes, nose, throat, and upper re
spiratory tract. Provisions shall be made for adequate
ventilation and regulation of manufacturing operations
to avoid open exposure of hot askarels (55C or higher).
The gases produced when askarei is decomposed by
very high temperatures (such as that of an electric arc)
in the presence of air or organic insulating materials
contain a high percentage of hydrogen chloride, and
small percentages of other gases. 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 askarels or its
arced products is necessary under emergency conditions,
an approved gas mask of the organic canister type, or
self-contained breathing apparatus, must be worn. Such
exposure should be under the surveillance of other per
sonnel capable of effecting rescue in case of accident.
If the odor of askarei or its arced products is detected
4The following trademarks are among those employed by elec trical manufacturers to designate the askarels used in their products: Asbestol,C hlorexlol, Inerteen, No-Flamol, Pyranol, and Saf T-Kuhl.
734599
NV Q2A5A4
13
AMERICAN NA NONAL STANDARD C 107.1-1974
by the person wearing protective equipment, he should tact occurs, remove by washing with soap and water.
immediately gc into fresh air. All gas masks, respirators, Following eye contact, flush with water. In case of
and replaceiner t parts should have U.S. Bureau of Mines spillage onto clothing, the clothing should be removed
approval and b<! maintained on a regular schedule in ac as soon as practical, skin washed, and clothing laun
cordance with the manufacturer's recommendation.
dered.
4.1.2.2
liquid. In contrast to the situation in 4.1.4 Receiving, Handling, and Storage of Askarels.
which mineral insulating oils are handled, there is no
Askarels are shipped in tank cars, tank trucks, steel
fire hazard in handling askarels. A limited solvent ac
drums, metal cans, and test-sample containers. When
tion (similar tokhat for paint thinner) on the fats and
received, all containers should be inspected for leaks.
oils of the skin with prolonged contact may lead to dry
4.1.4.1 Storage Tanks. Storage tanks should be
ing and chapping of the skin. As with insulating oil,
erected so that inspection can be made for teaks or
some people are^allergic to askarel, and continued expo spills. Construction should be such that inadvertent
sure may result in skin irritation. Both the liquid and . vapor are moderately irritating to eye tissue.
leakage or spills are prevented from reaching streams and sanitary or storm sewers.
Operating procedures should require avoidance of
4.1.4.2 Tank Cars and Tank Trucks. All bulk
contact with any askarels. The use of porous gloves that can absorb and retain askarels is to be avoided. Re sistant gloves and aprons of the neoprene, polyethylene, or fluoroelastomer1 type should be used if contact is
shipment equipment should be inspected for leaks im mediately upon receipt. Drain pans must be provided to prevent spillage from unloading hoses and connec tions. Askarel liquid collected in drain pans should be
unavoidable. In :ase of spillage on the clothing, the clothing should >e removed as soon as practical, the
placed in drums labeled "SCRAP ASKAREL" for dis position.
skin washed, and the clothing laundered. Medicinal wa: hes or mild detergents followed by the
application of cold cream will reduce the irritation re sulting from the contact of an open cut or abrasion
4.1.4.3 Steel Drums, Cans, and Test-Sample Con tainers. On delivery, all such shipments should be care fully inspected for leaks. The containers should be stored indoors in an area especially selected for this
with askarel.
purpose. A curb should enclose the area to provide a
Safety glasses with side shields or a face shield
basin for containing the askarel from one or more con
should be worn when handling'askarels. Eyes that
tainers should the containers be damaged. The area
have been exposed to liquid askarel should be irrigated
must not have a drain that is connected to a sanitary
Immediately with large quantities of running water for
or storm sewer.
! 5 minutes and then examined by a physician if the
If an indoor storage area is not possible, the con
irritation persists. (A drop of castor oil has been found
tainers should be stored under a lean-to.
to reduce irritation.)
4.1.5 Control of Water Effluents. The industry goal
Persons developing a skin irritation or respiratory
is to eliminate askarel in plant water effluent streams.
tract Irritation wl rile working with askarels should be
However, it is recognized that existing drain systems
placed under the supervision of a physician.
from manufacturing plants, repair shops, and installa
Ingestion or swallowing of askarels is not generally
tion sites may be contaminated as a result of past prac
regarded as a pro tlem of the industry. Should acciden
tices. Other sections of this standard provide that no
tal ingestion occ\i r, a physician should be consulted.
askarel wastes of any kind be disposed of in any water
Hands should be ivashed with warm water and soap
effluent streams and that accidental spills be prevented
before eating, drl iking, smoking, or using toilet facili
from getting into such streams.
ties. 4.1.5.1 Concentration Limits. The 1972 Environ
4.1.3 Transport Container Marking. Any container, mental Protection Agency proposals are to keep PCB
such as tank cars, tank trucks, drums, cans, etc, used to levels in rivers and lakes below 0.01 part per billion.
transport transfoijmer askarels, new or used, should be
This is currently under review by the EPA and stan
labeled with the fallowing: CAUTION: This product contains polychlorinated
dards are expected to be promulgated in 1974. Plant effluent streams should be managed and controlled in
biphenyls (PCBs)J Care should be taken to prevent
a manner anticipating these government standards.
entry into the environment through spills, leakage, use, vaporization, or d sposal of liquid or containers. Avoid
4.1.5.2 Monitoring Streams. Alt plant effluent streams should be monitored on a regular basis, consis
prolonged breathi ig of vapors or mists. Avoid contact with eyes or prolonged contact with skin. If sldn con-
tent with plant situations. The procedure for perform ing the necessary analyses is contained in Section B4 of Appendix B. This procedure or its equivalent should
?For example, Vitoii.
be used.
MV 0 2 ^ 5 14
734600
AMERICAN NATIONAL STANDARD C 1 0 7 .M 9 7 4
4.1.5.3
Methods for Minimizing Effluent Streamshould be placed in open-head drums with suitable clo
Contamination. The ideal approach is to isolate totally
sures and with the drum properly labeled for shipment
all effluent streams that coild be contaminated with
to a company offering an acceptable disposal service.
askarels during manufacturing processes and prevent
4.1.6.5
Liquid and Solid Waste Disposal Service
them from being discharged from the plant.
Organizations
4.1.6 Disposal Procedures and Services
4.1.6.5.1 General. Disposal of askarels and
4.1.6.1 Sources of Materials Requiring Special
askarel-soaked materials should be accomplished by
Handling and Disposal Procedures. Liquids containing
means in which there is no significant release of askarel
PCBs and solids containing lor contaminated with PCBs
to the environment. At present, disposal is accomplished
may be obtained from anyJof the following sources:
by carefully controlled incineration of liquids and
transport containers, transformer manufacturing pro
soaked software, and by controlled landfill burial of
cesses, in-test failures, liqui is contaminated beyond
apparatus and other hardware from which askarel has
reclamation, in-service transformer leaks and failures,
been previously drained and washed.
askarel-fllled transformers icrapped for any reason, etc.
Present knowledge indicates that proper incineration
4.1.6.2 Classification for Disposal of Materials
must involve a suitable balance between dwell time and
Containing PCBs. In general, there are three types of
temperature in the incineration plus oxygen availability
materials requiring disposal: liquids, burnable solid
and, finally, suitable scrubbers to remove the HCI that
materials containing PCBs,|and nonburnable solid mate will be formed; for example, 2-second dwell time at
rials contaminated with PCBs.
2000F and 3% excess oxygen in stack gas, or 1.5-
4.1.6.2.1 Liquids. Liquids containing PCBs
second dwell time at 2700 F and 2% oxygen in stack
requiring disposal by high-tempcrature incineration
gas.
may consist of the following:
These facilities should meet the applicable require
(1) PCBs contaminate^ with mineral oil.
ments of the state in which they are located and should
(2) Mineral oil contaminated with PCBs.
control effluents within the limits set forth in this stan
(3) Nonreclaimable contaminated transformer aska dard.
rels, arced askarels, askarels from manufacturing spills,
Controlled landfill or deep-well disposal can be used
and sump accumulation, etc, rich in PCBs, and askarels
where permitted by federal, state, and local regulations.
from holding basins, drip and drain pans; washings, sam
*4.f .6*5.TTfosti. In addition to the normal
ple jars and containers, etc'.
costs of collecting scrap liquids and solids for disposal,
4.1.6.2.2 Burnable Solid Waste Materials Con additional costs borne by the owner of such scrap in
taining PCBs. These mater als can be disposed of by high- clude shipping containers, cost of transport to the dis
temperature incineration nd consist of cellulosic mate posal service organization, and a disposal fee usually
rials, rags, pressboard, wood, sawdust, fuller's earth in
based upon a per-gallon or per-pound charge.
bulk or in cloth bags, blot ter papers, nitrile or cork gas
4.!.6.5.3 Disposal Services. Organizations
kets, etc.
offering disposal services are listed in Appendix A,
4.1.6.2.3 Nonburnable Solid Waste Materials
including their location, facilities available, types of
Containing, or Contamina led with, PCBs. These mate
materia] handled, and disposal procedures used. Speci
rials may consist of coil tt ructures, steel, copper, alu
fic shipping directions, disposal procedures, and costs
minum filter units of the ifeel mesh construction type, should be obtained from the organization.
askarel drums, cans, etc.
Materials of this nature should be allowed to drain
4.2 Specific Guidelines
with the liquid collected i i drip pans, etc. Further re
4.2.1 Plant Housekeeping. It is necessary to assume
moval of adhering PCBs c in be accomplished by wash
that in filling equipment with askarel, and during fur
ing or solvent extraction with kerosene or other ap
ther handling of this equipment, an askarel spill may
proved washing liquids su ;h as perchloroethylene or
occur. Therefore, it is necessary to provide facilities and
tricholoroethylene. Accumulated liquids can be dis
a procedure for cleanup to prevent contamination.
posed of as indicated in 4.1.6.2.1. Solid materials may
4.2.1.1 Atkaitl Filling Area
be handled as normal scrap.
4.2.1.1.1 The location of the askarel filling
4.1.6.3 Shipment of Scrap Liquids for Disposal.
area should be adjacent to the test area and final ship
All liquid scrap material snould be placed in appropriate ping area to minimize the danger of damage of units
metal transport drums, properly labeled, for shipment
during handling.
to a company offering an acceptable disposal service.
4.2.1.1.2 The main manufacturing area for
4.1.6.4 Shipment of Burnable Solid Waste Mate filling equipment with askarel should be provided with
rial Containing PCBs for Disposal. Material of this type
impervious surface floors or suitable basins so con-
NEV 024546
15
734601
AMERICAN NATIONAL STANDARD C107.1-1974
structed that any :nadvertent leakage or spills are pre-
4.2.1.4.4
All used materials, including rags,
vented from reaching streams, sanitary sewers, or storm sawdust, tape, etc, regardless of quantity, shall be put
Msewers. All askareMiandling equipment, such as pumps,
hoses, etc, shall bej of the askarel-resistant type.
nto the appropriate containers for disposition. ^ 4.2.2 Transformer Labeling ( . f C )
4.2.1.1.3
Drip pans shall be provided for hose 4.2.2.1
New Transformers. All new transformers
connections and filling valves,
that contain PCBs shall have a label of adequate durabil
4.2.1.2 Spe{iial Containers for Scrap Materials
ity, permanently and prominently attached to the tank
4.2.1.2.1 Drums labeled "SCRAP ASKAREL" by the manufacturer, giving adequate warning and in
should be available for handling all spilled and waste
structions. A suggested label includes the following:
askarel from sump^, failed units, drip pans, sample jars,
CAUTION: The insulating liquid in this transformer
etc. contains polychlorinated biphenyls (PCBs). Care should
4.2.1.2.2
Open-head drums with suitable cbleo taken to prevent entry into the environment. In case
sures and labeled 'jSCRAP BURNABLE ASKAREL
of malfunction or leaks, consult the instruction manual
WASTE" should bu available for handling contaminated or the manufacturer.
cellulose insulation, rags, paper pressboard, wood, gas
4.2.2.2
In-Service Transformers. The transformer
kets, sawdust, etc.
manufacturer should make available suitable labels with
4.2.1.2.3 Separate containers for handling
a similar warning as shown in 4.2.2.1 for use on exist
steel, copper, and iluminum, each adequately marked, i n g transformers.
shall be provided for the components of contaminated
4.2.3 Information for Transformer Users
core and coil assemblies. These containers are required
4.2.3.1
General. Askarel-filled transformers are
for the various materials when repairing or scrapping
delivered to customers as sealed units from which there
assemblies.
is no escape of askarel under normal operation. Although
4.2.1.2.4 Containers for supplies of material
certain types of equipment failures can permit loss of
for absorbing small -askarel spills or cleanup of larger
some askarel to the environment, such cases are extreme
spills should be projrided.
ly rare.
" " 4.2.1.3 Conditioning of Askards
J
4.2.3.2
Transportation and Receiving. Immedi
\
4.2.1.3.1 Askarel Conditioning Equipment.
ately upon receipt of the equipment and following any
The conditioning unit should be located either in the
transportation or handling accident that could affect
' storage tank area or in the main transformer manufac
the integrity of the tank, bushings, or radiators, the
turing area for fillin i with askarel.
transportation vehicle, tank, and fittings should be
4.2.1.3.2
1hitler's Earth. Conditioningexoafmnienwed for any leakage or spillage that may have
askarel or recycled t skarel requires fuller's earth treat
occurred in shipping. If leakage is evident, the cause
ment. The spent ful er's earth in cartridges or bags,
should be corrected and the spillage soaked up with
when replaced, shov Id be allowed to drain thoroughly
absorbent materials such as sawdust, followed by a
over drip pans to remove as much liquid askarel as pos cleanup of the affected area with rags soaked with kero
sible. The cartridge units of steel mesh construction
sene or other approved solvent such as perchloroethy-
should be placed in the " STEEL CONTAMINATED
lene or trichloroethylene. All materials used should be
WITH ASKAREL" ontainer for disposition. Cloth
collected for proper disposition as described in 4.1.6.
bags filled with fuller's earth should be placed in the
4.2.3.3
Installation and Periodic Inspection. Fol
V "SCRAP BURNABLE ASKAREL WASTE" container
lowing installation, the unit should again be inspected
i . for disposition.
for any damage or leakage. It is recommended that
*^ r s s r 4.2.L4 Teardpwn of Units for Repair or Scrap
periodic in-service inspections be made for any leaks.
4.2.1.4.1 Drain all askarel from the unit either
4.2.3.4 Filling, Filtering, or Drying Askarel.
Into a holding tank y>r reuse or Into the drum labeled
Most askarel units are shipped with the proper amount
d
'"SCRAP ASKAREL" for disposition, and then allow sufficient time for aty of the askarel to drain from the
of askarel, but if it becomes necessary to top off a unit, the manufacturer*! instructions should be followed.
core and coils.
If It is necessary to dry an askarel unit or to treat an
4.2.1.4.2 Remove the core and coil assembly
askarel unit with fuller's earth, instructions should be
from the transforme r. Sufficient absorbent material
followed. When filtering or conditioning askarel, all
the floor to absorb any askarel
of the precautions previously described for drip pans,
fluid that still drips trom the transformer.
proper disposal of filter media, etc, apply.
4.2.1.4.3 Place all materials in the appropriate
4.2.3.S
Sampling. It is common practice to sam
salvage containers di ring the dismantling for later dis
ple askarel from a transformer for periodic maintenance
position,
testing. As previously described, such samples should be
16
734602
nev
AMERICAN NATIONAL STANDARD C 107.1-1974
taken in a manner to avoid any contamination of the
Specific Resistance (Resistivity) of Electrical Insulating
environment. Washings should be collected for proper
Liquids, C59.S1-1965 (R1973) (ASTM D 1169-64
disposal. Field and laboratory test samples, washings,
(1973))
etc, should also be collected for proper disposal.
(10] American National Standard Method of Test for
4.2.3.6
Transformer Disposal. The ultimate dis Hydrolyzable Chlorine Compounds in Chlorinated Aro
posal of an askarel-ftlled t ansformer may be accom
matic Hydrocarbons (Askarels), C59.I06-1970 (ASTM
plished in either of two w lys:
D 1820-65 (1971))
(1) Complete drainage and dismantling with the
proper disposal of the askkrel and askarel-soaked com ponents as described in 4.9.6.
(2) Disposition of askArel transformers by means of
(11] American National Standard Method of Test for Thermal Stability of Chlorinated Aromatic Hydrocar bons (Askarels), CS9.111-1970 (ASTM D 1936-64
junk or scrap dealers. This should be avoided unless a
(1971))
transformer is first drained, followed by soaking the interior with a suitable solvent. Accumulated liquids and washings are to be disposed of as described in 4.1.6.
(12] American National Standard Method of Test for Distillation of Road Tars, A37.9-1974 (ASTM D20-72)
(13] American National Standard Methods of Testing
Electrical Insulating Oils, C59.2-1974 (ASTM D 117-71
(1973))
5. References
5.1 References to the Te^tt
[1J Standard Method ofTest for Rapid Gas Chroma tographic Estimation of Higher Boiling Homologues of Chlorinated Biphenyls fo^ Capacitor Askarels, ASTM D 3303-74
(14] American National Standard Method ofTest for Dielectric Breakdown Voltage of Insulating Liquids Using Disk Electrodes, C59.19-1968 (R1973) (ASTM D 877-67 (1971))
115] American National Standard Method of Test for Flash and Fire Points by Cleveland Open Cup, Z! 1.61973 (ASTM D 92-72, IP 36/67)
[2] American National tandard Method ofTest for
Specific Gravity of Aska: els, C59.68-1965 (R1973) (ASTM D 1810-63 (1973);)
[3] American National ^tandard Method of Test for Neutralization Number by Color-Indicator Titration, Z11.131-1964 (Rl 974) (ASTM D 974-64 (1973), IP 139/65)
(16] American National Standard Method of Test for Saybolt Viscosity, Z11.2-1956 (R1971) (ASTM D 8856(1973))
(17] American National Standard Method of Test for Coefficient of Thermal Expansion of Electrical Insu lating Liquids of Petroleum Origin, and Askarels, C59.57-1963 (R1973) (ASTM D 1903-63 (1973))
MJ American National ptandard Method ofTest for Neutralization Number by Potentiometric Titration, ZI 1.59-1958 (R 1971KASTM D 664-58 (1968), IP 177/64)
[5] Standard Method o^ Test for Density of Rubber Chemicals, ASTM D 1817-66 (1972)
(18] MUNCH, R. H. Measuring the dissipation factor, dielectric constant, and resistivity of liquids. Insulation/ Circuits, vol 16, Mar 1970, pp 46-49.
119] Chlorodiphenyls. Hygienic Guide Series. West mont, N.J.: American Industrial Hygiene Association, Jan-Feb 1965.
|6] American National Standard Method of Test for Inorganic Chlorides in Askarels, C59.55-1963 (R1973) (ASTM D 1821-63 (1978))
(20] Standard Specification for Chlorinated Aromatic Hydrocarbons (Askarels) for Transformers, ASTM D 2283-73a
(7) American National Standard Method of Test for Pour Point of Petroleurr Oils, Z! 1.5-1966 (R1972) (ASTM D 97-66 (1971). IP 15/67)
(8) American National Standard Method ofTest for Power Factor and Dielectric Constant o f Electrical Insulating Liquids. C59{22-1967 (R1973) (ASTM D 924-65 (1973))
(9] American National Standard Method of Test for
5.2 General References
Aroclor Polychlorinated Polyphenyls (Biphenyls), Technical Bulletin O-FF/IR. St. Louis: Monsanto In dustrial Chemicals Company, Nov 1971.
DRINKER, C. K. Further observations on the possible systemic toxicity of certain of the chlorinated hydro carbons. Journal o f Industrial Hygiene and Toxicology, vol 21,1939, pp 155-159.
NEV 02454
17
734603
AMERICAN NATION AL STANDARD C 107.1-1974
DRINKER, C. K.; V.ARREN, M, F.; and BENNET, G. A. The problem >f possible systemic effects from certain chlorinated tydrocarbons. Journal o f Industrial Hygiene and Toxicdh'ogy.vo\ 19.1937, pp 283-311.
ELKINS, H. B. The Chemistry o f Industrial Toxicology. New York: John Wiley & Sons, Inc, 1959.
GREENBURG, L ; LAYERS, M. R.; and SMITH, A. R. The systemic effect^ resulting from exposure to certain chlorinated hydroci^rbons. Journal o f Industrial Hygiene and Toxicology, voi 21,1939, pp 29-38.
Threshold Limit Values for Chemical Substances and Physical Agents in the Workroom Environment. Cincin nati: American Conference of Governmental Industrial
Hygienists, 1973.
TREON, J. F.; CLEVELAND, F. P.; CAPPEL, J.; and ATCHLEY, R. W. The toxicity of the vapors of Aroclor 1242 and Aroclor 1254. American Industrial Hygiene Association Quarterly, vol 17,1956, pp 204-213.
6. Revision of American National Standards Referred to in This Document
When the American National Standards referred to in this document are superseded by a revision approved by the American National Standards Institute, Inc, the re vision shall apply.
'I*1 si4
$
A
734604 18 NV 024549
A n n a n H Iv O C
(These Appendixes ire not pert o f American National Stindird Guidelines for Handling ind DitpocaJ of C i >acltor- and Transformer-Grade AtkirelsContaining Polychlorinated Biphenyls C l 07.1-1974, but are included for information purposes only.)
Appendix A Disposal Services
In addition to the supervised dry landfill sites that may be used for the disposal of askarel-containing scrap, the following additional k lown facilities and services have been established, and others may be available.9
Chem-Trol Pollution Services, Inc P.O. Box 200 1550 Balmer Road Model City, N.Y. 14107 Phone:716 754-8231
This organization has facilities and services capable of handling:
(1) Liquids. Askarels alone or mixed with solvents or oils. Disposal by high-te mperature incineration.
(2) Solids (software), >iskarel-soaked compounds, . rags cartons, absorbing earlhs, etc. Disposal by incineration or scientific landfill.
(3) Solids (hardware), Capacitors, transformer tanks, cores, askarel-soaked meta s. Disposal by scientific landfill. Has solvent extraction capability.
Monsanto Company 800 North Lindbergh Boulevard St. Louis, Mo 63166 Phone: 314 694-3352
This organization has facilities and services capable of handling askarel liquids done or mixed with other oOs or solvents by high-ten^]iperature incineration, Liquid is pumped through gun with atomizing steam Into incinerator. Temperatji!res are maintained at 2000F2500F with auxiliary natlira! gas. Exit gases are quenched to 180F by coi^tiact with water. Gas is then passed through a high-enerj jy venturi scrubber for removal of particulates. Befone exhausting to air (1 10F),
gases are passed through a packed column scrubber to remove HCI.
Nuclear Engineering Company Eastern Division P.O. Box 146 Morehead, Ky 40351 Phone: 606 784-6611
Nuclear Engineering Company Disposal Division Sheffield, Dl. 61361 Phone:815 454-2624
This organization provides containerization, trans portation, and disposal services of all liquids and solids (including hardware). Disposal is in controlled chemical and scientific landfill area. Licensed by Atomic Energy Commission for radioactive waste disposal. The organi zation also has two West Coast locations, in the states of California and Washington.
Rollins Environmental Services, Inc P.O. Box 2349 Wilmington, Del 19899 Phone:302 658-8451
This organization has facilities and services capable of handling:
(1) Liquids. Askarel alone or mixed with solvents or oils. Disposal is by high-temperature incineration.
(2) Solids (software). Askarel-soaked compounds, rags, cartons, absorbing earths, etc. Disposal is by incin eration at combustion temperatures up to 2500*F. In cineration gases are scrubbed, and entrained solids are removed before exhausting to air.
Rollins Environmental Services maintains disposal facilities in the following areas:
Philadelphia/Camden :
9The listing given herein Is rep tentative o f tome o f the sources
Rollins Environmental Services, Inc
\
th it provide thli service, and li not presumed to be com plete,
Any other orginteationi that aflih to be listed should notify the Standards Institute so that th*ey may be Included in the next
Route 322 Logan Township
edition o f this standard.
Bridgeport, N J. 08014
NEV 02A550
19
734605
APPENDIX
lo Iwoq. U1 bfii jii/t null nt ?su b b ili. ivij.l/tiJE (tfiOi'i * kv::*A lo ticq n iw. :*h, >'>; >\ ,i n - /
m p f j y *? re \ r*y f .
') bviwiiit Ir*, y.'o'.1M't'iiu
) 'u:''*. -, : ' ir.- ".? r' > ^ ^
* ^ 'i* 4 * '
EalohVou^' M`
i..!.WOU*tpnf iii/'itr t*\>I*.' 't)i ..! i :>i
Rollins Environmental Services, Inc
Rollins Environmental Services, Inc
Scenic Highw ly & West Cheatham Lane
Tidal Road & Highway 134
Scotlandville
Deer Park, Tex 77536
East Baton Rouge Parish, La 70807
fl|
u)
nu. 'in;* I , I iiimnil?
fcv- amft
1/:.*!; mi I!>!**.yri* I/'-i.': -Ml ; V,! ; ,
Appendix B
.)')h
ij ' gtiirffiiO'-.
i:. ?;.** *.?1. vr*'
.1 \
?'>;im `x I**;>t
>:,k\
Analytical Proi<edures^nd ^ ^ o ^ to r y Service Organization5 ; t: v4 VL;,.:
ir/K'iviU o;
Bl. General
ci! /< ! .0 / 1
IM\H1 '**-0o r.rfO*,!' 1
Analytical procedures fordeitftiliiiingPCB* ttiia ft,:,h^
water, and sedimeints are given in Section* B3 and B 4 / J ! &( } 0 .is; AA*r>\' i'ir*'
i O i M 'i r!>. :m ,'!
VM r-.i-.'is- li*' C
for the isolation and determination of PCBs in water, (
soil/sediment, and biological materials. Absolute con-,,
firmation of PCB structures is not obtained with tills, ,
method. Where needed, additional structure proof *
should, be obtained using technique such as mass Spec
trometry for further identification of gas chroma tog-1
raphy fractions. .,/ ! - ' ;e. w 1
. .;
iw;?.: 1)1L ib.*!'.: -M' *i- .v f vy ^ , *t;
i" -
Jh<|^pUpvfj^
*ff .iej>rse(ativepf those ;>
r.:v< orf f .b\y> k il* r-vi;,v
j:.
i:.-1 )
C ^ r ^ C h e ^ I f i v f P O W ^ W o \. ' . t.
1375 Eighth Street
^ 1, , ^ |,.:i: r.v1jli*'> 1.
La Salle, III. 6130
Phone* 815 223-1 >00 1r',itA /
ivr ;jv. *v.'i /.(1:!,
Umnelics, Inc. (Sibsidiaiy of Carus Corpoittion)' ; '
6132 West Fond du Lac Avenue
1
Milwaukee, WIs 53218
! : , 'v 'v r! : u ` '9 w f i
^W u/lH 4>)r?'fi9 _c.h!Vi au.!
. * . 1:
Collob Analytical Service Corporation
47 w au ito aito i& r i,*s V1
ia,r*'i; A i:!,!
Berkeley Heigh,#.7. 0 7 9 2 2 ',i ,! vf ^
noiie:;2 o r 4 ^ 3 3 r i'-,J1,-,f; A
ItLI'I /I
.0V ,?tiViCVJytKft.'fdl#
" ' (;
1' ^; *ln
-!l o l o i ` l'iMiji
d !v;i iv r m iln c
B3ri,Ahhkltica!Pr6cedurfor the Deteritilnation of Airborne PCBs
B3.1 Scope. This procedure 'Iii tedhni^iiet''* ' * used by the Monsanto Industrial CbttPical. Company .I I
_______
jhil . < ? ; kuystt
9The listing given herein is representative o f some o f th aotifees that provide this service, and is not presumed tp he qopipIetA. Any other organir.atiqns that wish to.^e jilted should notify, jhe Standards Institute so that they mak b e lftcliided in the ttext edition o f this standard.
Cl
20
B3.2 Prindple.^Xirborne
pre absorbed in tojuenc
by'draWln^tlie ;ii/^ to u ^ h ;one pYmore fritted bubblers
bt impingert lli^'cj/ltnders1f i l l e d * t o l u e n e . After a |
suitable amount of air is sampled, the scrubbing solvent
ii diluted or cohcehtrated, and inte^fering components,
if jWeienC id rdmbyed j)^ chemickl treatment and * *
column absorption bKro&etography. th e amount and
type of PCBs present are determined by electron cap
ture gas chromatography (EC/GC). .
#vr.* <>\
B3.3 Reagent*
*>'*
* '
(1) Hexane: Pesticide grade.
\
*! u't
(2) Toluene: Pesticide grade. * ' v *' " ' 1' 11 " `
(3) Sodiurp sulfate: Anhydrous, granular, Analytical
reagcnt (AR) grade, Heat at .40QC for I hour prior to
use.
r: i V
*i
:!V1: /!(*
ij(4) AlupdiU adsorption: f o r chromatographic angj-i
. ryijSjiBO/JQOmesh< N a t ali 400C fora minimum period
of 4 hours *nd deactivate with 5%(w/w) distilled water.
For Situjmini column preparation fill a chromatographic
column with hexane up to the point, where the reservoir;
joint the jopUimn, end push glass wool plug ip the bot
tom with a glass rod. In a 50-mi beaker measure 35 mJ
(about 30 grams) of deactivated alumina, and pour this
slowly into the column. Tap or vibrate the column to ' 1 settle ^ e ^ u m i^ ,a h d to p th e k lb m in t with 2 to 3 ettf.
of a^ydrpvw sodium sulfate., Waiih the column With 50
to 100 ml of hexane prior to the addition of the sample.
(5) Distilled water: Extracted with hexane to re-
NEV O i A b S l
734606
APPENDIX
NOTE: Instrument: Hewlett-Packard 5750 Detector: **Ni, electron capture
Column: 6-mm X 6-foot, 4%XE-60 on 8 0/100 mesh,
Chromotorb W. HP, AW-DMCS. Column temperature: 200C Injection temperature: 220C Detector temperature: 250C Carrier gas: He, 60 ml/min Purge gas: lOTbCHj/argon, 120 ml/min Pulse interval: 50 jis Injection volume: 5 $i\ Standard concentration: 1,00 jig/ml Range: 10 Attenuation: 8
AROCLOR K>I6
i............. mr mm 09
2
i ........T
34
5
MINUTES
6
7
Fig. B1 Aroclor 1016 Electron Capture Chromatogram
6
9
move hexane-soluble electron rapturing impurities. (6) Sulfuric acid: AR grade^ specific gravity * 1.84. (7) Potassium hydroxide: AR grade. (8) Ethanol: Formula 2B. (9) Alcoholic potassium hy Iroxide, 2.5% (w/v): Dis
solve about 12.5 grams of AR |rade KOH in 500 ml of ethanol.
(10) Sulfuric acid-water, 9: 1 (v/v): Carefully add 270 ml of AR grade sulfuric ac d< to 30 ml of distilled water In a 500-ml iced beaker.
(11) PCB standards: Aroclor 1016,1221,1242, 1248,1254, and 1260. (See F i|;. B1 through B7.)
B3.4 Apparatus (1) Gas scrubbing bottles, h igh form, ground-glass
joint, fritted coarse disks. (2) Separatory funnels equipped with ground-glass
stoppers and TFE-fluorocarbon stopcocks; capacities of 125,250,500,1000, and 2000 ml.
(3) Kunderna-Danish evapoi stive concentrators,
500-ml capacity, equipped with three-ball Snyder col umns and graduated 5-ml capacity vials.
(4) Chromatographic columns, glass, 10 Inches X 20 mm (OD), with a 5-inch X 50-mm (OD) reservoir at the top, equipped with TFE-fluorocarbon stopcocks.
(5) Rat-bottomed boiling flasks, 125 ml capacity. (6) Liebig condenser, 200 mm in length. (7) Hot plates. (8) Water bath. (9) 10-pl syringes. (10) Diy-test meter or wet-test gas meter. (11) Laboratory vacuum pump. (12) Rotating vacuum evaporator. (13) Usual laboratory glassware.
B3.S Sampling. The air to be sampled for airborne PCBs 1s drawn through a gas scrubber (or scrubbers) and a dry-test meter using a laboratory vacuum pump. See Fig. B8. The sampling flow rate is controlled by bleeding in air via a needle valve located between the
NEV 02*552
21
734607
APPF.NDIX
AROCLOR 1221
--H
AROCLOR 1242 AROCLOR 1248
4
J -
126
26
26
1
AROCLOR 1254
J? 127 26
29
AROCLOR 1260
SO
iI
0 24
tT
I I'
I
-'T-
6 0 (0 12 14 16 16 2 0 2 2 2 4 2 6 2 6 3 0 3 2 3 4 3 6 38
MINUTES
Fig. B2 Comparison of Electron Capture Chromatograms for
Aroclor 1221,1242,1248,1254, and 1260
734608
J22 NEV 024553
APPENDIX
NOTE: Inttniment: Hewlett-Packard 5750 Detector: #*Ni electron capture Column: 6-mm X 6-foot, 4% XE-60 on 80 /1 0 0 m edi,
Chromotorb W, HP, AW-DMCS Column temperature: 170C Injection temperature: 220C Detector temperature: 250C Carrier gat: He, 6 0 ml/mln Purge gat: 10%CH4/argon, 120 ml/mtn Pulte interval: 5 0 /it Injection volume: 5 jil Standard concentration: 1.48/ig/m l Range: 10 Attenuation: 4
4
RELATIVE RESPONSE
AROCLOR 1221
TT
O 2 3 4 56 MINUTES
F IB 3 Aroclor 1221 Electron Capture Chromatogram
NEV 0 2 4 5 3 4
734609
23
APPENDIX
1
6
NOTE: Instrument: Hewlett-Packard 5750 Detector: *9Ni electron capture Column: 6*mm X 6-foot, 4% XE-60 on 8 0 /1 0 0 mesh,
Chromosorb W, HP, AW-DMCS Column temperature: I90C Injection temperature: 220C Detector temperature: 250C Carrier gas: He, 6 0 mi/min Purge gas: 10%CH4/argon, 120m l/m in Pulse interval: 50 jis Injection volume: 5 jit Standard concentration: 1.03 jjg/ml Range: 10 Attenuation: 8
RELATIVE RESPONSE
F i|B 4 Aroclor 1242 Electron Capture Chromatogram
NEV 0 2 4 5 5 5
24 734610
APPENDIX
NOTE: Instrument: Hewlett-Packard 5750 Detector: N i electron capture Column: 6-mrn X 6-foot, 4% XE-60 on 8Q/100 mesh,
Chromosorb W, HP, AW-DMCS Column temperature: 190C Injection temperature: 220C Detector temperature: 250C Carrier gas: He, 60 m l/min Purge gas: 10% CH ^argon, 120 ml/min Pulse interval: 50 ns Injection volume: 5 gil Standard concentration: 1 .3 ln g /m l Range: 10 Attenuation: 4
RELATIVE RESPONSE
AROCLOR 1248
67 MINUTES
Fi. B5 Aroclor 1248 Electron Capture Chromatogram
NEV 0 24556
734611
APPENDIX
NOTE: Instrument: Hewlett-Packard 5750 Detector: **Ni electron capture Column: 6-mm X 6-foot, 4% XE-60 on 8 0 /1 0 0 m eih,
Chromosorb W, HP, AW-DMCS Column temperature: 205C Injection temperature: 220C Detector temperature: 250C Carrier gat: He, 60 mt/min Purge gas: 10%CH4/argon, I2 0 m l/m in Pulse interval: 50 ps Injection volume: S pi Standard concentration: 1.02p g/m l Range: 10 Attenuation: 8
15 -
RELATIVE RESPONSE
I .1 mmymmmm O I2
-- g 3A
, T" 1
56
7
MINUTES
t 'mmm ' i* " *''"I" * ' I 8 9 IO It
Fig. B6 Aroclor 1254 Electron Captur Chromatogram
T 12
NtV Q i A b l
734612
APPENDIX
NOTE: Instrument: Hewlett-Packard $750 Detector: *' NJ electron ctpture Column: 6-mm X 6-foot, 4% XE-60 on 8 0/100 mesh,
Chromosorb W, HP, AW-DMCS Column temperature: 220C Injection temperature: 220C Detector temperature: 250C Carrier gas: fie, 6 0 ml/min Purge gas: 10%CH4/argon, 120 ml/min Pulse interval: 50 p i Injection volume: 5 pi Standard concentration: 0.98 pg/m! Range: 10 Attenuation: 8
RELATIVE RESPONSE
T
I " I ......... I
I
I
I
I1
0 I l 3 4 5 6 7 8 9 IO II 12
MINUTES
Fig. B7 Aroclor 1260 Electron Capture Chromatogram
NEV 024558 I 734613
APPENDIX
AIR BLEED
SAMPLE INLET
DRY-TEST METER
EXHAUST
Fig. B8 Sampling Train
pump and the mete t. At the end of the sampling period
the metered gas volumes are corrected for temperature
and pressure to cutjic metres at 2SC and 760 mmHg.
It is important tjo note that neither the capacity nor
the efficiency of the gas scrubber(s) for removal of air
borne PCBs have been experimentally evaluated. For
this reason, it is beit to minimize the sampling (low
rate and maximize the sampling time period to obtain
measurable amounts of PECs. When high flow rates
must be employed pr 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 s;rubber have been experimentally
established, this procedure should be used only to
measure relative PC Blevels sampled under equivalent
conditions.
B3.6 Procedure (1) After scrubbing the desired amount oT air, re
cord the metered volume, pressure, and temperature. (2) Quantitative y transfer the scrubbing solvent
to a round-bottomel flask and reduce the volume to approximately 2 ml by rotary vacuum evaporation.
(3) Quantitatively transfer the concentrate to a 30-ml beaker with tne aid of several small portions of toluene.
(4) Inject a fraction of a microlitre of the concen trate into the gas chromatograph to check for interfer ences and determine the approximate level of PCBs present. If no interferences are present, dilute or con centrate the sample to a known volume, as determined by the electron capture chromatogram, and proceed with the gas chromatographic analysis.
(5) If interferences are present, proceed with the chemical treatment ^nd column chromatographic cleanup procedures.
(6) Transfer the incentrate to a 125-mi extraction
flask with the aid of several small portions of solvent. (7) Evaporate the concentrate just to dryness with
a gentle stream of dry, filtered air and add 25 ml of 2.5% alcoholic potassium hydroxide.
(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 the aid of 25 ml of distilled water.
(10) Rinse the extraction flask with 25 ml of hex ane and add it to the separatory funnel.
(11) Stopper the separatory funnel and shake vigor ously for at least 1 minute. Allow the layers to separate, and transfer the lower aqueous phase to a second sepa ratory 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 por tion of hexane. Discard the saponification solution and combine the hexane extracts.
(14) Carefully add 25 ml of the sulfuric acid solu tion (9:1 concentrated sulfuric acid-water) to the hex ane extracts.
(15) Stopper the separatory funnel and shake vigor ously for at least I 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.
(17) Filter the hexane extract through a 4-inch funnel, plugged with glass wool that is covered with a layer of sodium sulfate, into a Kunderna-Danish evap orative concentrator.
(18) Add a small boiling chip, put the Snyder col umn in place, and reduce the hexane volume to less
734614
n V 04^559
i
I
APPENDIX
than 5 ml by heating the apparatus in a 80*C to 90C water bath.
(19) After cooling, n move the 5-ml graduated tube and transfer the hexane extract to an alumina adsorp tion column, washing it in with several 5-ml portions of hexane.
(20) Carefully add 100 ml of hexane to the column reservoir, Bnd 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 volumet ric flask, dilute to volume with hexane, and proceed with the gas chromatogrnphic analysis.
(22) If the column eluent is collected in a KundernaDanish evaporative concentrator, reduce solvent volume, cool, dilute to volume, a id proceed with gas chromato graphic analysis.
B3.7 Electron Capture (las Chromatographic Procedure (1) Instrument: Gas chromatograph (for example,
Hewlett-Packard Model i 750, or the equivalent) (2) Detector: High-temperature **Ni, electron cap
ture cell (3) Column: 6-mm X 6<-foot glass column, 4% XE-
60 on 80/100 mesh, Chromosorb W, HP, AW-DMCS (4) Column temperature: 160Cto 190QC (5) Injection port temperature: 195C to 215C (6) Detector temperature: 300C (7) Pulse interval: 5 0 /is (8) Flow rates: Heliu n carrier, approximately 60
ml/min; argon-methane \ urge, approximately 120 ml/ min
Using EC/GC as the d iterminative step, inject, in duplicate, 1 to 10 gil of each solution into the chroma tograph. By comparison with standard solutions in jected, in duplicate, under the same operating condi tions, determine the amount and type of Aroclor using the Individual or total peak height and area methods.
B3.8 Sample Concentre! ion. Concentration of sample extracts is necessary, prior to cleanup by chromato graphic or chemical means, to reduce sample size and increase sensitivity. The ]referred method of concern trating allows minimum oss through volatilization or chemical decomposition ind requires a minimum time. The three methods of sol vent volume reduction most commonly used are evap Hatton by exposure to a stream of air, evaporation employing a KundernaDanish evaporative conct ntrator equipped with a Snyder column, and evaj oration under reduced pres sure. All three technique;have been used without en countering any significant losses from volatization or chemical alternation. However, the Kunderna-Danish evaporative concentrator! and the stream-of-air methods are easier to use.
B3.9 Column Adsorption Chromatography and Chemi cal Cleanup. Silica gel, a magnesia silica gel,f and alu mina deactivated with 0%, 1.0%, 1.5%, 2.0%, and 5% water were investigated as adsorbants for the elimina tion of interferences. Alumina (5% water) was found to be more effective and reproducible than either silica gel or a magnesia silica gel.9 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 400C, to ensure a reproducible activity.
Saponification, and subsequent extraction of the sample with sulfuric acid, is an effective way to remove a number of chlorinated hydrocarbon interferences as well as other matrix interferences. PCBs are not affected.
B3.10 Column Performance. Column performance is the key to effective gas chromatographic analysis and, as such, the choice of column materials is particularly important. Ideally, the support employed should be inert, mechanically strong, and of high surface area. Chromosorb W, HP, AW-DMCS fulfills these require ments and is recommended for this work.
A variety of polar and nonpolar 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% 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, consequently, low levels of materials is column conditioning. With polar phases such as XE-60 and QF-1, operating a new column overnight at a temperature 25C to 50C higher than that to be used during analysis results in a more stable column. A no-flow conditioning technique is employed to condition nonpolar 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 com pleted as in the case of the polar liquid phase. Two pre cautions should be observed: during conditioning, the column should not be connected to the detector, and the maximum safe temperature of the liquid phase should not be exceeded.
Since all liquid substrates bleed to one degree or another and columns eventually degrade, all new col umns should be characterized with two column perfor mance indicators: the number of theoretical plates (N) and a tailing factor (7}. p,p'-DDT is employed to check these parameters because it is known to degrade on
9For example, Fiorita.
N6V 0 2 4 5 6 0
734615
APPENDIX
THEORETICAL PLATES, N l6 ( /y )2
INJECTION
Fig. BIO
Calculating the Tailing Factor
TAILING, T o/2b
PEAK HEIGHT
"poor" columns. In this manner, one can determine whether the perfomance of a new column is satisfac tory and when the c >lumn performance begins to fall off. A column is con tidered good if the number of theo retical plates per foe t Is of the order of 400 to 500, with tailing factors c f 1.0 to 1.3. Calculation of these parameters is shown in Fig. B9 and BIO. Additionally, there should be no significant extraneous peaks upon injection of a pure pip'-DDT standard.
Other chromatographic conditions that can be ad justed are column te nperature and flow rates. Al though resolution o f a mixture increases with decreas ing temperature, a tepperature should be chosen that allows the elution ofjiil components within a conve nient 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.
30
Any system of instrument and column suitable for chlorinated pesticide analysis is satisfactory for PCB analysis. The use of the high-temperature #3Ni electron capture cell is highly recommended. The ability to oper ate at higher temperatures prevents maintenance prob lems due to contamination from high-boiling compo nents. Glass columns also should be employed.
B3.11 Detection and Measurement. Quantitative deter minations employing the electron capture detector are nonstoichlometric measurements 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 employed:
Case 1. EC gas chromatogram of PCB unknown, unchanged with respect to standard PCB with no evi dence of interferences
NEV
734616
Case 11. EC gas chromatogram of PCB unknown, altered with respect to standard PCB with no evidence of interferences
Case 111. EC gas chromate gram of PCB unknown, unchanged with respect to standard PCB with evidence of interference
The amount of PCBs in Case 1 samples is determined by preparing a plot of the m^Jor peak height or area versus concentration. With Cfse 111 samples, a peak free from interference is used. When dominant interferences are present, one or more of the chemical cleanup proce dures is employed.
In all cases, the response or the electron capture detector must be linear for quantitative analysis.
B3.12 Contamination. In determining PCBs in biologi cal materials by electron capture gas chromatography, laboratory sources of contam nation can be a major problem. The samples and extracts should never be allowed to come in contact with materials other than glass, TFE-fluorocarbon, or metal. Laboratory glassware should be thoroughly washed With hot, soapy water, and rinsed with distilled water, acetone, and then hex ane. All equipment should als6 be rinsed again with hexane just prior to use, and blanks should be frequent ly carried through all steps of he procedures to ensure against the possibility of contamination.
B3.13 Sensitivity (!) Concentration: 2 ppb (parts per billion) (2) Absolute sensitivity: O J X HT* gram (3) Volume injected: 5 jil (4) Final volume of extract: 5 ml (5) Sample size: 250 ml
B4. Analysis of Water and Sediment for PCBs
B4.1 Scope. This methodology^ used by the Monsanto Industrial Chemical Company for the determination of the amount and type of PCBs in water and sediment samples. Absolute confirmation of PCB structures is not obtained with this method. Structure proof can be ob tained using additional techniqujes such as mass spec trometry to further identify the gas chromatography fractions.
B4.2 Principle. The PCBs in wat er and sediment sam ples are extracted into an organi: solvent. Interfering components are then removed from the extracts by chemical treatment and column idsorption chroma tography. The amount and type &fPCBs present are determined by electron capture | ;as chromatography (EC/GC).
APPENDIX
B4.3 Reagents
(1 ) Hexane: Pesticide grade.
(2) Acetonilrile: Pesticide grade. (3) Sodium sulfate: Anhydrous, granular, analytical reagent (AR) grade. Heat at 400 C for 1 hour prior to use. (4) Alumina adsorption: For chromatographic anal ysis, 80/200 mesh. Heat at 400C for a minimum of 4 hours and deactivate with 5% (w/w) distilled water. For alumina column preparation fill 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 mea sure 35 ml (about 30 grams) of deactivated alumina, and pour this slowly into the column. Tap or vibrate the column to settle the alumina, and top the alumina with 2 to 3 cm of anhydrous sodium sulfate. Wash the column with 50 to 100 ml of hexane prior to the addi tion of the sample. (5) Distilled water: Extracted with hexane to re move hexane-soluble electron capturing impurities (6) Sulfuric acid: AR grade, specific gravity * 1.84. (7) Potassium hydroxide: AR grade. (8) Ethanol: Formula 2B. (9) Alcoholic potassium hydroxide, 2.5% (w/v): Dissolve about 12.5 grams of AR grade KOH in 500 ml of ethanol. (10) Sulfuric acid-water, 9:1 (v/v): Carefully add 270 ml of AR grade sulfuric acid to 30 ml of distilled water in a 500-ml iced beaker. (11) PCB standards: Aroclor 1242,1248,1254, and 1260. (See Fig. B2 and Fig. B4 through B7.)
B4.4 Apparatus
(1) Separatory funnels equipped with ground-glass
stoppers and TFE-fluorcarbon stopcocks; capacities of
125,250,500,1000, and 2000 ml.
(2) Kundema-Danish evaporative concentrators,
500-ml capacity, equipped with three-ball Snyder col
umns and graduated 5-ml capacity vials.
(3) Chromatographic columns, glass, 10 Inches X 20
mm (OD) with a 5-inch X 50-mm (OD) reservoir at the
top, equipped with TFE-fluorocarbon stopcocks.
(4) Sintered glass Alter funnels, 600-m) capacity,
90-mm disk diameter, medium porosity.
(5) Flat-bottomed boiling flasks, 125-ml capacity.
(6) Liebig condenser, 200 mm in length.
(7) Hotplates.
(8) Water bath.
(9) Reciprocating variable-speed shaker.
(10) 10^1syringes.
734617
(11) 32-oz all-glass mortars and pestles.
(12) 8-inch X 12-inch X 2-inch (2-1/2 qt) heat-
resistant glass baking dishes.
NEV 024562
31
APPENDIX
(13) U.S. Standard sieve, No. 30. (14) Usual laboratory glassware.
B4.5 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 given in B4.5.I and B4.5.2.
B4.5.1 Water.j Where possible, the entire water sam ple, 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 B4.6.)
B4.5.2 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 mor tar and ground. Tie ground sediment should be sieved, remixed, and a 250-gram portion taken for analysis. (See B4.7.)
B4.6 Extraction <f Water Samples (1) After agila ling, transfer the entire aqueous sam
ple or a 250-ml aliquot into a graduated glass cylinder. Record the volumf 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 hexanJ and add each to the separatory fun nel.
(3) Stopper th^ separatory funnel and shake vigor ously for at least 1 minute. Allow the foyers to separate, and transfer the lo ver aqueous phase to a second separa tory funnel.
(4) Extract the water sample a second time with a 50-mi portion of hexane. After the foyers have sepa rated, add the first hexane extract to the second sepa ratory funnel, and transfer the aqueous layer to the original separatory funnel.
(5) Repeat the extraction with a third 50-ml por tion of hexane. Dis :ard the aqueous foyer and combine the hexane extract!
(6) Filter the c<mbined extracts through a 4-inch funnel, plugged wit i glass wool that is covered with sodium sulfate. Col ect the flltrate in a KundemaDanish evaporative concentrator, add a small boiling chip, put the Snyder column In place, and reduce the hexane volume Loless than 5 ml by heating the apparatus in an 80 Cto 90C water bath. (CAUTION: Solvent vapors mus be vented into a hood.)
(7) After coolin remove the 5-ml graduated tube and transfer the hexane extract to an alumina adsorp tion column, washir g it in with several 5-ml portions of hexane.
(8) Carefully ado 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 con centrator.
(9) If the column eluent is collected in a volumetric flask, dilute to volume with hexane, and proceed with the gas chromatographic analysis.
(10) If the column eluent is collected in a KundernaDanish evaporative concentrator, reduce solvent volume, cool, dilute to volume, and proceed with the gas chro matographic analysis.
B4.7 Extraction of Sediment and Soil Samples (1) Decant off any excess water and transfer the
entire sediment sample to a glass baking dish. Air-dry at ambient temperature (heat should be applied).
(2) When dry, transfer the soil/sediment to a mor tar and grind. Sieve the ground material through a No. 30 mesh sieve and weigh 250 grams (to the nearest 0.01 gram) into a 16-ounce narrow-neck screw-cap (alumi num-foil liner) glass bottle.
(3) Moisten the soil with about 10 ml of water 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 acetronitrile extract into a 600-ml sintered glass filter funnel containing a 1/4-inch foyer of anhydrous sodium sulfate. Collect the flltTate in a 600-ml beaker (vacuum filtration may be necessary).
(5) After the acetronitrile has completely drained into the beaker, wash the bottle twice with 50-ml portions of acetonitrile, adding each wash to the funnel after the previous wash has completely percolated through the sediment.
(6) Quantitatively transfer the extract to a KundernaDanish evaporative concentrator, add a small boiling chip, put the Snyder column in place, and reduce the solvent volume to less than 5 ml by heating the appara tus in an 80C to 90C water bath. (CAUTION: Solvent vapors must be vented into a hood.)
(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.
(8) Evaporate the extract just to dryness with a gentle stream of dry, filtered nitrogen and add 25 ml of 2.5% alcoholic potassium hydroxide.
(9) Add a boiling chip, put a water condenser in place, and allow the solution to reflux for 45 minutes.
(10) After cooling, transfer the solution to a 250ml separatory funnel with the aid of 25 ml of distilled water.
(11) Rinse the extraction flask with 25 ml of hex ane and add it to the separatory funnel.
(12) Stopper the separatory funnel and shake it
32
734618
APPENDIX
vigorously for at least 1 tninute. Allow the layers to separate, and transfer me lower aqueous phase to a second separatory fumul.
(13) Extract the sap >nlflcation solution with a sec ond 25-ml portion of h<xane. After the layers have separated, add the first lexane extract to the second separatory funnel and t ansfer the aqueous alcohol hyer to the original separatory funnel.
(14) Repeat the extraction with a third 25-ml por tion of hexane. Discard the saponification solution and combine the hexane extracts.
(15) Carefully add p ml o f the sulfuric acid solu tion (9:1 concentrated sulfuric acid-water) to the hex
ane extracts. (16) Stopper the separatory funnel and shake vigor
ously for at least 1 minute. Allow the layers to separate, and discard the lower Iqueous acid layer. Repeat this step until the acid layer is colorless.
(17) Wash the hexane with a 25-ml portion of water. Discard the water wash.
(18) Filter the hexane extract through a 4-inch fun nel, plugged with glass wool that is covered with a layer of sodium sulfate, Into a Kunderna-Danish evaporative concentrator.
(19) Add a small t oiling chip, put the Snyder col umn in place, and reduce the hexane volume to less than 5 ml by heating the apparatus in an 80C to 90C water bath.
(20) After coolin];, remove the 5-ml graduated tube and transfer the hexa le extract to an alumina adsorp tion column, washing it in with several 5-ml portions of hexane.
(2 !) 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 con centrator.
(22) If the coiun n eluent is collected in a volumet ric flask, dilute to vc iume with hexane, and proceed with the gas chroma ographic analysis.
(23) If the column eluent is collected in a KundernaDanish evaporative concentrator, reduce solvent vol ume, cool, dilute tojvolume, and proceed with gas chro matographic analyisis.
B4.8 Electron Capture Gas Chromatographic Proce dure
(1) Instrument: Gas chromatograph (for example, Hewlett-Packard M >del 5750, or the equivalent)
(2) Detector: High-temperature 4SNi, electron cap ture cell
(3) Column: 6-mm X 6-foot glass column, 4% XB* 60 on 80/100 mesh, Chromosorb W, HP, AW-DMCS
(4) Column temperature: 160C (5) Injection p^rt temperature: I95C
(6) Detector temperature: 300C (7) Pulse interval: 50 jis (8) Flow rates: Helium carrier, approximately 60 ml/min; argon-methane purge, approximately 120 ml/ min Using EC/GC as the determinative step, inject, in duplicate, 1 to 10 tA of each solution into the chroma tograph. By comparison with standard solutions in jected, in duplicate, under the same operating condi tions, determine the amount and type of Aroclor using the individual or total peak height and area methods. The electron capture detector should also be used to guide the isolation procedures. Water and sediment ex tracts can be checked for the presence of PCBs or inter ferences, or both, by injection of microlitre portions of the extracts at various points in the extraction and concentration schemes. In this manner it can be determined whether the sample needs to be concen trated or diluted and whether the cleanup procedures should be employed.
B4.9 Extraction. The extraction of PCBs from water, employing hexane as the extractant, has been found to be quantitative and sufficiently simple and rapid for use as a routine procedure.
The evaluation of this method was based on spiking water samples with standard acetone solutions of PCBs. The spiking method consisted of adding the PCB in 25 to 50 jd of acetone to 500 ml of tap water in a 32ounce narrow-neck screw-cap jar. After the sample was thoroughly mixed, duplicate 225- to 250-ml aliquots were taken and subjected to the proposed sample prep aration and worked up as outlined. The results were quantified by preparing a calibration curve using stan dard hexane solutions of the PCBs used to spike the water samples. The major isomer peak height was used to construct the calibration plot.
The average recovery and deviation achieved sub stantiated the applicability of the method for the quanti tative recovety and analysis of PCBs from water at the ppb-ppm level.
No PCB recovery experiments from spiked sediment and soil samples have been performed. Instead, several of the residual solids representative of some of the types of sediment or soil analyzed were reextracted with hexane/acetone (40:60) in a soxhlet extractor to test for the efficiency of the acetonitrile extraction step. The hexane, after isolation by dilution with dis tilled water, was then carried through the purification steps. Recoveries by soxhlet extraction have indicated that the acetonitrile extraction of PCBs was essentially quantitative in the cases checked.
B4.10 Sample Concentration. Concentration of sample extracts is necessary, prior to cleanup by chromato-
NEV 024564
33
734619
APPENDIX
graphic or chem leal meant, to reduce sample size and increase sensitiv ty, The preferred method of concen trating allows m nimum loss through volatilization or chemical decom >osition and requires a minimum time. The three metheds of solvent volume reduction most commonly used ire evaporation by exposure to a stream of air, evaporation employing a Kunderna-Danish evapo rative concentrator equipped with a Snyder column, and evaporation under reduced pressure. All three tech niques have been used, and no significant losses from volatilization or hemical alternation have been encoun tered. However, the Kunderna-Danish evaporative con centrator and the stream-of-air methods are easier to use.
B4.1 1 Column A Jsorption Chromatography and Clientcal Cleanup. Silici igel, a magnesia silica gel,9 and alu mina deactivated vith 0%, 1.0%, 1.$%, 2.0%, and 5% water were Investigated as adsorbents for th elimina tion of interferemjes. Alumina (5% water) was found to be more effective and reproducible than either silica gel or a magnesia silica gel,9 The activity of alumina varies with age an<| lot; therefore 5% water is added to the alumina, after heating for a minimum of 4 hours at 400C, to ensure a reproducible activity.
Saponification, nnd subsequent extraction of the sample with sulfuree acid, is an effective way to remove a number of chlori lated hydrocarbon interferences as well as other matri t interferences. PCBs are not affected.
B4.12 Column Per formance. Column performance is the key to effective! gas chromatographic analysis and, p such, the choice f column materials is particularly important. Ideally, e support employed should be inert, mechanically trong, and of high surface area, For these reasons, romosorb W, HP, AW-DMCS is recommended for is work.
A variety of poll and nonpolar liquid phases have been investigated, following columns have been found to provide a ate separation, etc, for use in PCB analysis by ton capture: 4% (w/w) DC-200, SF-96, OV-17, SB: >,SE-54, XE-60, Apiezon L, and 6% QF-1. DC-200 d XB-60 or QF-1 are the most suitable o f these liquid is.
Another important consideration when working with an extremely sensitive detector and, consequently, low levels of materia is column conditioning. With polar phases such as !CE-60 and QF-1, operating a new column overnight at temperature 25 C to 50 C higher than that to be used luring analysis results in a more stable column. A no-: low conditioning technique is employed to condition Ilonpoiar columns. Hie column is
9For example, Fioristi.
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 com pleted as in the case of the polar liquid phase. Two pre cautions should be observed: during conditioning, the column should not be connected to the detector, and the maximum safe temperature of the liquid phase should not be exceeded.
Since all liquid substrates bleed to one degree or another and columns eventually degrade, ail new col umns should be characterized with two column perfor mance indicators: the number of theoretics' 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 whether the performance of a new column is satisfac tory and when the column performance begins to fall off. A column is considered good if the number of theo retical plates per foot is of the order of 400 to 500, with tailing factors o f 1.0 to 1.3. Calculation of these parameters is shown in Fig. B9 and B10. Additionally, there should be no significant extraneous peaks upon injection of a pure p,p'-DDT standard.
Other chromatographic conditions that can be ad justed are column temperature and flow rates. Although resolution of a mixture increases with decreasing tem perature, a temperature should be chosen that allows the elution of all components within a convenient time period. The temperatures given are optimum for 42% chlorinated biphenyl; temperatures are increased when specifically analyzing for the higher chlorinated biphe nyls; that is, 54%, 60%, etc. The flow rates shown are optimum for a given instrument, column, and detector system. These should be adjusted if better results can be achieved.
Any system of instrument and column suitable for chlorinated pesticide analysis Is satisfactory for PCB analysis. The use of the high-temperature *s Ni electron capture cell is highly recommended. The ability to oper ate at higher temperatures prevents maintenance prob lems due to contamination from high-boiling compo nents. Glass columns also should be employed.
B4.13 Detection and Measurement. Quantitative deter minations employing the electron capture detector are nonstoichiometric measurements made by comparing peak heights or areas for known concentrations with those for unknown compositions. Except for sharp peaks, peak area measurements are usually more repro ducible than peak height measurements but are extreme ly time consuming unless a recording integrator is em ployed. However, peak height measurements are as accurate as disk integration of triangulation and, if the
34
734620
NEV 02A565
peak shape represents a Gaussian curve, the height may
be considered independent of the base. Consequently,
peak height measurements are generally used. Three
variations of the peak height or area quantification pro*
cedures have been employed.
Case 1. EC gas chromatogram of PCB unknown,
unchanged with respect to standard PCB with no evi
dence of interference^
Case 11. EC gas chromatogram of PCB unknown,
altered with respect tj> standard PCB with no evidence
of interferences
Case III. EC gas chromatogram of PCB unknown,
unchanged with respect to standard PCB with evidence
of interference
I
The amount of PCBs in Case 1samples is determined
by preparing a plot 01 the major peak height or area
versus concentration. For Case 11, a plot is prepared of
the total sum of all major peaks versus concentration.
With Case 111 samplesj a peak free from interference is
used. When dominantinterferencesare present,one or
more of the chemical cleanup procedures is employed.
APPENDIX
In all cases, the response of the electron capture detector must be linear for quantitative analysis.
B4.14 Contamination. In determining PCBs in water, soil, and sediment by electron capture gas chromatog raphy, laboratory 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, TFE-fluorocarbon, or metal. Laboratory glassware should be thoroughly washed with hot, soapy water and 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 ensure against the possibility of contamination.
B4.15 Sensitivity (1) Concentration: 2 ppb (2) Absolute sensitivity: 0.5 X l(Tf gram (3) Volume injected: 5 pi (4) Final volume of extract: 5 ml (5) Sample size: 250 ml
NEV 024566
35
734621
American National Standards
The sta >dord In this booklet Is one of neorly 6,600 tfondordt approved to dote by the Aimerlcan Noftonal Standards Institute formerly the USA Standords In* elitiste.
The Standords Institute provides the machinery for creating voluntary standords. It lerves to eliminate duplication of standards activities and to weld con* ftictino stundord* into single nationally occepted standards under the designa tion "American National Standards."
Each standard represents general agreement among maker seller ond user groups os to the best current practice with regard to some specific problem. Thus the completed standords cut ocross the whole fabric of production distribution and const mption of goods ond services. American Notionol Standards by reason of Institut t procedures reflect a national consensus of manufacturers consumers ond scien Ific, technical ond professional organisations ond governmental agen cies. The completed stondords are used widely by industry ond commerce ond often by municipal state and federal governments.
The Sticndords Institute under whose auspices this work is being done Is the United Sintes clearinghouse and coordinating body for standards activity on the national level. If is o federation of trade associations technical societies professionol grioops,,ond consumer organisations. Some 1,000 companies are affllloted with the nstitute as company members.
The Ar terican National Standords Institute is the United States member of the Inlernatic no! Organisation for Standardisation (ISO) the International Electro technical Commission (IEC), ond he fa n American Standards Commission (COPANT). Through these chonnels American Industry makes its position felt on he Interr ofionol level. American Notional Standards are on file In the libraries of the no ional standords bodies of more thon 50 countries.
Far m m e list of all American National Standards writes
American National Standard trattario, Ine
1431 Broadway
Now York, N. Y. 10011
NEV 024507 734622
PCBs - The E le c t r ic a l In d u stry
Steering Committee - ANSI - C107 * St. Louis, Mo. 11/11/71
Pertinent comments relative to'PCBs for use by the electrical in dustry and for consideration by the sub-committees on capacitors and transformers, include: 1. The electrical Industry has no suitable fire-resistant dielec
tric fluid x'eplacement for PCBs, polychlorinated biphenyls used in the askarol class of transformers and capacitors.
2. Because of this essential need and as the capacitors and trans formers are hermetically sealed, Monsanto continues to supply selected PCB fluids for use only in this particular electrical apparatus and only as "make-up" fluid (no new systems) in a few carefully regulated closed system heat transfer applica tions.
3. Because the higher chlorinated PCBs persist in the environ ment, Monsanto has removed essentially all of the penta and hexachlorobiphenyl compounds from capacitor askarel. T h e n e w product used exclusively is called Aroclor 1016. Also the hexachlorobiphenyl compounds have been removed from use in the askarel type transformer fluids.
4. Strict and effective steps have been taken to avoid introduc tion of PCBs into the environment at Monsanto's plants and by
-2
the facilities used where askarel typo transformers and capa-
eitors are made.
5. By discontinuing sole of PCBs for non-electrical applications,
about 75 percent of the more persistent types have been re
moved from commerce.
6. The posture of the PDA Includes:
a) "We reject the need and in fact the feasibility as some
have proposed for.an outright ban on the substances.
Although the use of PCBs requires control, an outright
ban is not feasible and would not be in the best in
terest of the oonsumer,"
b) "All available evidence indicates that PCBs (in terms of
acute toxicity) are classifiable as being of moderate
toxicity.". It was noted that PCBs are less toxic than
DDT which is one of the safest pesticides to humans in
acute toxicity terms.
7. When fod orally to standard test animals PCBs were found
essentially non-toxic,
8. FDA guide lines for maximum levels of PCB allowed in food
produots are:
Fish
5 PPm,
Chickens
5 ppm
Milk
0,2 ppm
Eggo
0.5 ppm
Catfish meal 0.3 P P
NEV 024592
734644
7 f. i- r " ' - 7 o
-3 -
9.' Prolonged exposure of PC3 liquid or vapor to the skin should
be avoided to prevent possibility of chloroacne.
10. .Prolonged exposure to vapors from hot PCBs should be avoided
to prevent possible damage to the liver and kidney. 0.5 to 1.0
mg per cubic meter of aij* haB been determined to be the maximum
safe level of exposure during an 8 hour work day.
11. There is no evidence from extensive animal studies that PCBs
are carcinogenic,
12. When PCBs are decomposed by an electric arc the gas formed is
virtually entirely hydrogen chloride, if phosgene gas is
formed at all, the amount is barely dlscernable.
13. Steps taken and judgements made to dispose of scrap PCB mate
rials from the electrical industry include:
a) Monsanto and others provide special high temperature
incineration and gas scrubber facilities to completely
destroy scrap PCB fluids. The scrap fluid may be sent
to Monsanto Co., Sauget, 111., attention supervisor Dept.
A246 for inoineration at 3 cents per pound.
b) All Monsanto PCB product labels carry this message which
is also being placed onto askarel transformers.
c) It is the concensus that it is not feasible to collect
and incinerate failed capacitors, at this time. They
should be buried in a land-fill remote from lakes, streams
or other sources of water.
The Incineration equipment already designed to take the
place of land-fills has been demonstrated fully caDabi*
NEV 024593
734645
`2
-4 -
of destroying the smaller capacitors as used for fluores cent ballast and motor-run purposes in air conditioners, etc. ThiB equipment is also capable of destroying the impregnated paper and plastic film core structures re moved from the larger power capacitors. It is foreseen that eventually this type equipment will come into use to replace many land-fills, Until such time the faied capacitors should be buried in land-fills. d) The solubility of PCBs in water is extremely low, in th range of 50 to 200 parts per billion, and the concensus is that PCB fluids do not migrate when buried in the soil. e) Solid Bcrap transformer insulation including colls and cores should be drained free from PCBs followed by flush ing or solvent extraction, using such solvents as perchloroethylne, or trichloroethylene employed in vapor degreasing. The scrap fluid mixtures should then be in cinerated under conditions similar to those provided by Monsanto to destroy the PCBs,
P. 0. Benignus 11/10/71
NEV 02^594
734646
1 A m ;: ! a