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### PART VII. SUMMARY OF TES T PROCEDURES, METHODS, AND REPORTING REQUIREMENTS FOR DI STILLATION FEED COMPOSITION ANALYSIS

The EPA petroleum refinery test program is re questing variability data for the feed to the distillation column. This part provides an ove rview of approved methods, target pollutants and units of measure, and reporting requirements for the analysis of the feed to your distillation column or first processing unit. 1 All recipients must complete and submit test results by August 31, 2011.

The distillation feed composition analyses re quested include: mercury, chlorine, sulfur, antimony, arsenic, beryllium, cadmium, chromi um, cobalt, lead, manganese, nickel, and selenium.

You will need to collect triplicat e samples of the feed to your distillation column three times, each time approximately 30 days from the last. Samples must be collected early enough in the testing period to ensure you can provide resu lts by August 31, 2011. For example, you may elect collect the first sample during early April, the second during early May, and the third during early June. Once you collect samples, composite the samples, and then analyze and report each composited sample. Directions for collecting, pr eparing, and analyzing th e distillation feed samples are outlined below.

Note: If you have multiple distillation co lumns and the feed to each is similar ( i.e. , the feed to one distillation column is representative of the f eed to all distillation columns at the refinery), you may collect samples from just one distillati on column. If you have multiple distillation columns and the feed to all of them is not the same, you must sample the feed from those that have significantly different feed streams. For ex ample, if you have thre e distillation columns and two have the same feed, you may sample from one of those two as well as the third and then note that the samples from the first ar e representative of the second.

1. How to collect a distillation feed sample : Table 1 outlines a summary of how samples should be collected.

1 The terms “distillation feed” or “feed to a distillation column” is used generically in this part to refer to the feed to the first major processing unit at the refinery. For most refineries, the distillation feed will be the feed to the atmospheric crude distillation unit. For refineries that do not have atmospheric crude distillation units, the distillation feed will be the feed to the vacuum distillation unit (if one is used). For refineries that do not have either an atmospheric crude distillation unit or a vacuum distillati on unit, samples of the feed used in the first major processing unit should be used ( e.g. , a refinery that receives only unfinished oils that are processed in a catalytic cracking unit and then further processed to make finished motor gasoline would sample the feed to the catalytic cracking unit).Form Approved __/__/__ OMB Control No. ____-____

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2 Table 1. Summary of Sample Collection Procedures
Sampling Location Sampling Procedures
Site-Specific Sampling and Analysis Manual Sampling Follow collection methods outlined in ASTM D4057 Automatic Sampling Follow collectio n methods outlined in ASTM D4177 Crude Oil Supplier Analysis Crude Oil Supplier If you only process one type of crude oil and your crude oil supplier will provide all of the requested information, the crude oil supplier must collect the sample as specified above an d prepare the sample according to methods specified in Steps 2 and 3 of this part.

2. Prepare sample for analysis : To prepare your samples for mercury and selected metal analyses, use SW-846-3020A or any SW-846 sample digestion procedures giving measures of total metal. For other analyses, use the guidance in ASTM D7455-08 for appropriate sample preparation.

3. Analyzing distillation feed sample : Table 2 outlines a list of approved methods for analyzing distillation feed samples. If you would like to use a method not on this list, please contact EPA for approval of an alte rnative method. Please see Section 4.0 of Component 4 for a list of persons to contact with questions regarding test methods and reporting.

Table 2. List of Analytical Method s for Distillation Feed Analysis

Analyte Method Target Reported Units

of Measure Higher Heating Value ASTM-5865-03a, ASTM D240, ASTM E711-87 (1996) Btu/lb

Density/API Gravity ASTM D287-92, ASTM D1217-993, ASTM D1481-93, ASTM D4052-96 lb/ft 3 AND API Gravity

Mercury Concentration SW-846-7470A, EPA Method 1631E, SW-846-1631E, SW-846-1631, EPA 821-R-01-013, or equivalent ppm

Chlorine Concentration ASTM E776-87 (1996, 2004, or 2009), SW-846-9250, SW-846-5050, -9056, -9076, or -9250 ppm

Sulfur Concentration ASTM D129-00 (2005), ASTM D1552-01 or -08, ASTM D2622-98 or -10 ppm

Total Selected Metals Concentration SW-846-6020, -6020A, , SW-846-6010B, SW-846- 7740 for Se, SW-846-7060 or -7060A for As ppm

4. Reporting distillation feed analysis data : You must report the anal ysis results in Table 3. The electronic version of Ta ble 3 is included in the el ectronic ICR that can be downloaded from the ICR website ( https://refineryicr.rti.org ). The template also asks you to note if the crude oil or intermediate slat e that makes up the feed to the distillation column during the time of your sample is si gnificantly different than the crude oil or intermediate slate you used during 2010.Form Approved __/__/__ OMB Control No. ____-____

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3 You must keep the following records for 3 years:

• Documentation that distillation feed sa mples were obtained in accordance with the above sampling protocol;

• Documentation of the proper chain of cu stody for each distillation feed sample;

• Description of the QA/QC procedures follo wed in preparing each distillation feed sample for analysis and perfor ming the required analysis; and

• The results of the analyses perfor med on each distillation feed sample.

Table 3. Distillation Feed Sample and Analysis ResultsSample DateUnit ID for Distillation ColumnHigher Heating Value (Btu/lb)Density (lb/ft3)API Gravity Concentrations (ppm)Unit IDs for Other DistillationColumn(s) with FeedRepresentativeIf the crude oil or intermediate slatebeing fed to the distillation columnduring the time of this sample issignificantly different than thecrude oil or intermediate slate usedduring 2010, briefly explainMercuryChlorineSulfurAntimonyArsenicBerylliumCadmiumChromiumCobaltLeadManganeseNickelSelenium