C=Sites on construction completion list.

P=Sites with partial deletion(s).

[62 FR 15576, Apr. 1, 1997]

EFFECTIVE DATE NOTES: 1. At 66 FR 28096, May 22, 2001, table 1 to appendix B of part 300 was amended under State of Louisiana by removing the site name "Gulf Coast Vacuum Services" and the city "Abbeville, Louisiana, effective July 23, 2001.

2. At 66 FR 28099, May 22, 2001, table 1 of appendix B to part 300 was amended by removing the site for "Cleveland Mill, Silver City, NM", effective July 23, 2001.

3. At 66 FR 28102, May 22, 2001, table 1 of appendix B of part 300 was amended by remov

ing

the site for "Brodhead Creek, Stroudsburg, PA.", effective July 23, 2001.

4. At 66 FR 28106, May 22, 2001, table 1 of appendix B to part 300 was amended under Salem Acres Superfund Site by removing the "Salem Acres Superfund Site, Salem, Massachusetts', effective July 23, 2001.

5. At 66 FR 28110, May 22, 2001, table 1 of appendix b of part 300 was amended by revising the entry for "California Gulch", effective July 23, 2001. For the convenience of the user, the superseded text is set forth as follows.

3 Oil Standard Solutions: Concentrations in Final DCM Extractions

4 Synthetic Seawater [Toxicity Test]

5 Test Oil Characteristics: No. 2 Fuel Oil 6 Analytes Listed Under the Corresponding Internal Standard Used in Calculating RRF's

7 Primary Ions Monitored for Each Target Analyte During GC/MS Analysis

8 Analytes and Reference Compounds

9 Operating Conditions and Temperature Program of GC/MS

10 Two-Way ANOVA Table

11 Product Test Data, Total Aromatics 12 Summary Statistics for Product Test Data, Total Aromatics

13 Example Two-Way ANOVA Table

14 Pairwise Protected LSD Mean Separation

1.0 Introduction

1.1 Scope and Application. The methods described below apply to "dispersants, surface washing agents, surface collecting agents, bioremediation agents, and miscellaneous oil spill control agents" involving subpart J (Use of Dispersants and Other Chemicals) in 40 CFR part 300 (National Oil and Hazardous Substances Pollution Contingency Plan). They are revisions and additions to the EPA's Standard Dispersant Effectiveness and

Toxicity Tests (1). The new Swirling Flask Dispersant Effectiveness Test is used only for testing dispersants. The Revised Standard Dispersant Toxicity Test is used for testing dispersants, as well as surface washing agents, surface collecting agents, and miscellaneous oil spill control agents. The bioremediation agent effectiveness test is used for testing bioremediation agents only.

1.2 Definitions. The definitions of dispersants, surface washing agents, surface collecting agents, bioremediation agents, and miscellaneous oil spill control agents are provided in 40 CFR 300.5.

2.0 Swirling Flask Dispersant Effectiveness Test

2.1 Summary of Method. This protocol was developed by Environment Canada to provide a relatively rapid and simple testing procedure for evaluating dispersant effectiveness (2). It uses a modified Erlenmeyer flask to which a side spout has been added for removing subsurface samples of water near the bottom of the flask without disturbing a surface oil layer. Seawater and a surface layer of oil are added to the flask. Turbulent mixing is provided by placing the flask on a standard shaker table at 150 rpm for 20 minutes to induce a swirling motion to the liquid contents. Following shaking, the flask is immediately removed from the shaker table and maintained in a stationary position for 10 minutes to allow the oil that will reform a slick to return to the water's surface. A sample of water for chemical analysis is then removed from the bottom of the flask through the side spout, extracted with methylene chloride (dichloromethane-DCM), and analyzed for oil content by UV-visible absorption spectrophotometry at wavelengths of 340, 370, and 400 nm (2). 2.2 Apparatus.

2.2.1

Modified Erlenmeyer Flask. Use 125ml glass Erlenmeyer flasks that have been modified to include an attachment of a glass side spout that extends from the bottom of the flask upward to the neck region, as shown in Figure 1.

2.2.2 Shaker Table. Use a shaker table with speed control unit with variable speed (40-400 rpm) and an orbital diameter of approximately 0.75 inches (2 cm) to provide turbulence to solutions in test flasks.

2.2.3 Spectrophotometer. Use a UV-visible spectrophotometer capable of measuring absorbance at 340, 370, and 400 nm. A Hitachi Model U-2000 or equivalent is acceptable for this purpose.

2.2.4 Glassware. Glassware should consist of 5-, 10-, 25-, 100-, and 500-ml graduated cylinders; 125-ml separatory funnels with Teflon stopcocks; and 10-, 100-, and 1,000-ml volumetric flasks and micropipettes.

2 Not calculable when viscosity at 100 °C is less than 2.0. 2.3.3 Methylene Chloride (DichloromethaneDCM), pesticide quality. For extraction of all sample water and oil-standard water samples.

2.4 Pretest preparation. 2.4.1 Preparation and analysis of oil standards. 2.4.1.1 Standard solutions of oil for calibrating the UV-visible spectrophotometer are prepared with the specific reference oils and dispersant used for a particular set of experimental test runs. For experiments with no dispersant, only oil is used to make the standard solution. For experiments with the oil plus dispersant, the standard is made with a 1:10 (v:v) mixture of the dispersant to the test oil (i.e., a dispersant-to-oil ratio of 1:10). This ratio is used in the test tank with dispersant added. The presence of water and certain dispersants in DCM extracts can affect absorbance readings in a spectrophotometer. All standard solutions of oil (and dispersant, if present) should be prepared in a stepwise manner that reflects the analytical protocol used for the experimental water samples.

2.4.1.2 To prepare the standards, prepare a parent oil-DCM standard by mixing 1 part oil (plus 1/10 part premixed dispersant, if applicable) to 9 parts DCM (i.e., 1:10 dilution of the oil v:v). Add a specific volume of the parent oil-DCM standard to 30 ml of synthetic seawater in a separatory funnel. Extract the oil-water mixture with 5-ml volumes of DCM after 15 seconds of vigorous shaking followed

by a 2 minute stationary period to allow for phase separation for each extraction. Repeat the extraction using a total of three 5-ml portions of DCM. Adjust the final DCM volume for the combined extracts to 20 ml with DCM in a 25-ml graduated cylinder.

2.4.1.3 The quantities of oil used to achieve the desired concentrations in the final 20-ml DCM extracts for the standard oil-solutions are summarized in table 3. Specific masses for oil amounts in standards are determined as volumes of oil multiplied by the density of the oil.

2.4.2 Linear stability calibration of UV-Visible spectrophotometer.

1 Assuming an oil density of 0.9 g/ml and an extraction efficiency of 100% for oil from the 30-ml of seawater.

2.4.2.2 Instrument stability for the initial calibration is acceptable when the RFS for the five highest standard extracts of oil are <20% different from the overall mean value for the five standards. If this criterion is satisfied, analysis of sample extracts can begin. RFS for the lowest concentration (0.05 mg oil/ml DCM) are not included in the consideration because the absorbance is close to the detection limit of the spectrophotometer (with associated high variability in the value) for the 1-cm path-length cell used for measurements. Absorbances ≥3.5 are not included because absorbance saturation occurs at and above this value.