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After our initial review of the test procedures required in these specifications, it was apparent that some test methods might be more affected by the presence of used oil or recycled oils than others. I will limit my discussion to a few illustrative examples. It should be noted that the tests described are applicable to both recycled crankcase oils and industrial oils.

In general, test procedures for fuel oils have been evaluated on the basis of (a) applicability to recycled oils and recycled oil/fuel oil blends; (b) if applicable, the extent to which the presence of recycled oil affects the precision of each procedure set forth in the test method; and (c) the special properties of recycled oils affecting equivalent performance which may require additional tests not necessary for "new" oils. For our laboratory evaluations of the test procedures, we used a variety of composite automotive crankcase drainings and recycled fuel oils.

I would now like to consider some specific test procedures.

Sampling of Fuel Oils

Fuel oil specifications and standards vary considerably in their requirements for sampling, ranging from no requirements to fairly detailed requirements. The presence of waste oils has two potential effects on sampling: a less homogeneous mixture due to separation on standing and a lowered stability of the fuel oil. Since a sampling procedure may be required, we are considering one based on MIL-F-859E. For bulk lots (where a bulk lot is defined as an indefinite quantity of hydrocarbon oil of one grade), upper, middle, and lower samples will be taken using thief or bottle samples as described in ASTM method D 270. Samples may be composited to a single sample if homogeneous. Further, the procedure states that homogeneity will be determined on the basis of density, ASTM method D 1298. Lots will be considered homogeneous if the specific gravity determinations for the upper, middle, and lower samples do not vary from the average by more than 0.0012 density units or 0.3° API (American Petroleum Institute) gravity.

Carbon Residue

Carbon residue is normally specified only for distillate fuel oils, grade Nos. 1 and 2, and is measured on the 10-percent residue after distillation. The carbon residue test appears to give excellent results in predicting the performance of distillate fuels heavier than grade No. 1. The simpler Ramsbottom method, ASTM D 524, is generally used in preference to the Conradson method, ASTM D 189. High carbon residue would indicate a tendency to form excessive carbon on burning, greatly reducing the efficiency of vaporizing pot-type burners or fouling nozzles in small residentialtype burners. The carbon residue test is used primarily to control the carbon-forming tendency of No. 2 fuel. No. 1 normally would be so low in carbon residue as to be of little significance. The test values are often affected by the presence of used or recycled oils. This is due to the fact that the test is run on 10-percent residuum remaining after distillation and, thus, concentrates the high boiling fractions in the residuum. The repeatability of the method falls within the stated limits for the method.

Ashing Procedures

Two general methods are used for determination of ash in petroleum products, ASTM D 482 and D 874. Regular ash, D 482, is generally called for with the residual grades. However, according to the procedure it is not intended for waste crankcase oils or additive-containing oils where D 874 is specified. D 874, sulfated ash, has been used as an indication of additive level in oils, but again, is not recommended for used automotive oils according to the procedure.

For the residual fuels, ash results from a variety of inorganic compounds present in the crude oil, as well as contaminants acquired during transportation or storage. Used automotive oils added to fuel oils would be expected to contribute to the ash primarily due to high lead content, plus various additive metals such as calcium, barium, zinc, and magnesium. Ash in residuals is important as it can cause hightemperature corrosion of boilers, refractory erosion, or excessive deposits.

During our investigation of these ashing methods, we found that the regular and sulfated ashes give approximately the same values for the virgin oils. The Bartlesville Energy Research Center (BERC) annual heating oil survey showed a typical maximum of 0.5 percent ash for virgin No. 6 residual oil [6]. Since most used oils have considerably

higher ash contents than 0.5 percent, it could be expected that ash-forming constituents would be of concern with regard to the substantial equivalency of recycled fuel oils to virgin fuel oils.

To determine if there is singificant metal loss during ashing using the sulfated ash procedure, the metal content of used automotive oils was determined and compared with the metal content of the ash determined using atomic absorption spectroscopy. Although we have not completed analysis of the ashes, the data to date, based on a materials balance for lead, calcium, zinc and magnesium, indicate D 874 is satisfactory for use with used and recycled oils.

Lead Analysis

At the present levels of consumption of leaded gasoline, significant concentrations of lead may be anticipated for some time in used automotive crankcase oils. It is well documented that lead is an environmental hazard. Lead content, negligible in virgin fuel oils, occurs in concentrations of 0.5 to 1.5 percent in typical crankcase drain oils. Considerable effort by the EPA has gone into studies of the environmental impact of burning fuels containing lead and the feasibility of lead removal where emission controls are not available. Obviously, if it is determined by the FTC and/or EPA that lead is important in recycled fuel oils, a test procedure for lead will be required.

Various analytical methods have been evaluated in our Analytical Chemistry Division to establish their applicability to recycled oils. Determination of lead in recycled oils is difficult because the lead is present both in the solid phase and, presumably, also in the form of oil-soluble lead compounds. Sampling to obtain a representative and homogeneous sample requires considerable care.

At the present time, we have found a number of problems with existing analytical methods for lead in used crankcase oils, and are in the process of searching for a method with acceptable accuracy and precision.

Summary

In the limited time available, I have been able to mention only a few of the test procedures we have been working on. Others include water and sediment, copper corrosion and a test procedure for heating value. Several test methods require additional resear For example, polynuclear aromatic hydrocarbons (PAH's), or polycyclic organic matter, have been of interest due to the toxicity of some of these compounds. Work on development of a test procedure for PAH is discussed in another presentation at this conference.

We are also investigating chlorine and bromine test procedures. It is at present unclear whether these halogens are important for equivalence with virgin fuel oils. The complete report of our efforts in this phase of the NBS Recycled Oil Program will soon be available.

In conclusion, I would like to acknowledge our student help in the laboratory, Messrs. Richard Doitteau and Steve Serkiz, and to express our appreciation to the Association of Petroleum Re-refiners for their support of a research associate at the NBS. The very numerous contributions from the NBS staff in assisting with the program are appreciated, as well as the cooperation of various agencies and organizations outside the NBS.

References

[1] Success at Oil Creek Washington, D.C.).

[2]

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Fuel Oils, Commercial Standard CS 12-48 (Sixth Edition, U.S. Department of
Commerce, Washington, D.C., 1948).

[3] Petroleum Products Handbook, V.B. Guthrie, ed. (McGraw-Hill, New York, 1960).

[4]

Private communication (1977). (E. French, Defense Supply Agency).

[5]

National Petroleum News Factbook Issue 69, 63 (1977).

[6]

Shelton, E. M., Heating Oils, BERC PPS-76/4 (1976).

SESSION IV. LEGISLATION AND STUDIES

National Bureau of Standards Special Publication 556. Proceedings of
a Workshop on Measurements and Standards for Recycled 011 - II held
at NBS, Gaithersburg, Maryland, November 29 and 30, 1977. (Issued
September 1979)

RECENT FEDERAL AND STATE LEGISLATIVE DEVELOPMENTS
IN USED OIL RECYCLING

William A. Irwin and Karla Heimann

Environmental Law Institute 1346 Connecticut Avenue, N.W. Washington, D.C. 20036

United States legislation, both Federal and State, governing collection, recycling, and disposal of used oil has developed dramatically in the last 2 years. This has occurred in response to increased awareness of the needs to conserve a valuable resource and to protect environmental and public health from risks posed from improper reuse or disposal.

This article summarizes existing Federal laws under which used oil might be regulated; bills currently pending in the Senate and the House of Representatives; the model used oil recycling act; and, finally, State legislative initiatives--some enacted, some not--for controlling used oil collection, recycling, or disposal.

Existing Federal Laws

Various issues raised by recycling used oil are addressed by recent Federal laws. It is perhaps not likely, but certain oil products might be regulated as new or existing chemical substances or mixtures under the Toxic Substances Control Act, passed in October 1976. The operative standard throughout that statute is whether a substance poses an unreasonable risk of injury to health or the environment. Notorious substances like PCB's [polychlorinated biphenyls] come to mind in this connection, but there is no reason to think that products or derivatives made from oil--in new or used form--are beyond its scope.

If the Administrator of the Environmental Protection Agency (EPA) finds that the manufacture, distribution in commerce, processing, use, or disposal of a chemical substance or mixture may present an unreasonable risk of injury to health or to the environment, he may subject it to testing under section 4 or to regulation under section 6 of the Toxic Substances Control Act.

It is more likely that used oil would be regulated under the 1976 amendments to the Solid Waste Disposal Act, amended as the Resource Conservation and Recovery Act (RCRA). Flammability and toxicity are two of the criteria listed in section 3001 of the RCRA as providing the basis for regulations to be issued by the EPA which will identify characteristics of hazardous wastes and will list particular hazardous wastes or processes which produce them. Since used oil, or contaminated used oil, is sometimes flammable or toxic (or both), it has been considered a candidate for control under the hazardous waste provisions of the RCRA. While it would be justifiable to regulate used oil which is flammable or toxic as a hazardous waste, it would not be accurate to put all used oil on a list of hazardous wastes. Section 1004 (5) defines hazardous wastes as substances that "...pose a substantial present or potential hazard to human health or the environment when improperly treated, stored, transported, or disposed of, or otherwise managed," or that "...cause, or significantly contribute to an increase in mortality or an increase in serious irreversible, or incapacitating reversible, illness." If a substance does not meet these tests or the section 3001 criteria, then by definition it is not a hazardous waste, and no amount of administrative convenience or discretion can make it legal to treat it as such.

As a practical matter, the RCRA's controls over generators, transporters, and disposers of hazardous wastes are admirably thorough (see sections 3002-3005). If the EPA determines that used oil qualifies as such a waste, then all sources and handlers of used oil would have to be regulated in hazardous waste management programs called for by subchapters C and D. For this reason, it is unlikely that any State would be eager to manage or that the Federal Government would be able to manage such

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